RU2817583C2 - New aerosol generating substrate - Google Patents

Abstract

FIELD: smoking accessories.

SUBSTANCE: invention relates to an aerosol-generating article. Article comprises an aerosol-generating substrate, wherein the aerosol-generating substrate comprises a homogenised plant material. Homogenised plant material contains at least 2.5 wt.% of eucalyptus particles in terms of dry weight, a substance for forming an aerosol and a binder. Aerosol-generating substrate contains at least 0.04 mg of eucalyptol per gram of substrate in terms of dry weight, at least 0.2 mg of eucalyptin per gram of substrate in terms of dry weight and at least 0.2 mg of 8-desmethyleucalyptin per gram of substrate in terms of dry weight.

EFFECT: invention makes it possible to create an aerosol-generating substrate for a heated aerosol-generating article, which provides an aerosol with an improved mouthfeel and a sense of fullness of the oral cavity, which makes the generating aerosol comparable to the sensations provided by a conventional combustible cigarette.

17 cl, 11 dwg, 4 tbl

Description

The present invention relates to aerosol-generating substrates that contain homogenized plant material formed from eucalyptus particles, and to aerosol-generating articles containing such an aerosol-generating substrate. The present invention further relates to an aerosol obtained from an aerosol generating substrate containing eucalyptus particles.

Aerosol-generating products in which an aerosol-generating substrate, such as a tobacco-containing substrate, is heated rather than burned are known in the art. Typically, in such products, the aerosol is generated by transfer of heat from the heat source to a physically separate aerosol-generating substrate or material that may be located in contact with, within, around, or downstream of the heat source. During use of an aerosol generating product, volatile compounds are released from the substrate through heat transfer from the heat source and are entrained in air drawn through the product. As the released compounds cool, they condense to form an aerosol.

Some aerosol-generating products contain a flavoring agent that is delivered to the consumer during use of the product to provide the consumer with a different sensation, for example, to improve the flavor of the aerosol. The flavoring agent may be used to deliver a gustatory sensation (taste), an olfactory sensation (smell), or both a gustatory and an olfactory sensation to the user inhaling the aerosol. It is known to provide heated aerosol generating products that contain flavoring agents.

It is also known to provide flavoring agents in conventional combustible cigarettes, in which smoking the end of the cigarette opposite the mouthpiece is ignited, causing the tobacco rod to burn to generate inhaled smoke. One or more flavoring agents are typically mixed with the tobacco in the tobacco rod to add additional flavor to the inhaled smoke when the tobacco is burned. Such flavoring agents may be provided, for example, in the form of an essential oil.

The aerosol from a regular cigarette, which contains many components that interact with receptors located in the mouth, provides a “mouth full” sensation, that is, a relatively strong sensation in the mouth. "Mouthfeel" as used herein refers to the physical sensation in the mouth caused by a food, beverage or aerosol and is distinct from taste. It is a fundamental sensory attribute that, along with taste and smell, determines the overall flavor of a food product or aerosol.

There are difficulties associated with replicating the consumer experience provided by conventional combustible cigarettes in aerosol-generating products in which the aerosol-generating substrate is heated rather than burned. This is partly due to the lower temperatures reached when such aerosol generating products are heated, resulting in a different profile of volatile compounds released.

It would be desirable to provide a new aerosol generating substrate for a heated aerosol generating article that provides an aerosol with improved mouthfeel and mouthfeel. It would be particularly desirable if such an aerosol generating substrate could provide an aerosol with a sensation comparable to that provided by a conventional combustible cigarette.

It would also be desirable to provide such an aerosol generating substrate that can be readily incorporated into an aerosol generating article and that can be manufactured using existing high speed methods and devices.

The present invention provides an aerosol generating article that contains an aerosol generating substrate, wherein the aerosol generating substrate comprises homogenized plant material containing eucalyptus particles. According to the present invention, the aerosol generating substrate contains: at least 0.04 mg of eucalyptol per gram of substrate on a dry weight basis; at least 0.2 mg of eucalyptin per gram of substrate on a dry weight basis; and at least 0.2 mg of 8-desmethyleucalyptin per gram of substrate on a dry weight basis.

The present invention further provides an aerosol generating article that contains an aerosol generating substrate, wherein the aerosol generating substrate comprises homogenized plant material containing eucalyptus particles. When the aerosol-generating substrate is heated in Test Method A as described below, an aerosol is generated containing: at least 10 micrograms of eucalyptol per gram of substrate on a dry weight basis; at least 10 micrograms of eucalyptin per gram of substrate on a dry weight basis; and at least 10 micrograms of 8-desmethyleucalyptin per gram of substrate on a dry weight basis. According to the present invention, the amount of eucalyptol per gram of substrate is not more than twice the amount of eucalyptin per gram of substrate, and the amount of eucalyptol per gram of substrate is not more than twice the amount of 8-desmethyleucalyptin per gram of substrate.

The present invention further provides an aerosol generating article comprising an aerosol generating substrate, wherein the aerosol generating substrate comprises homogenized plant material containing at least 2.5 percent by weight of eucalyptus particles on a dry weight basis.

The present invention further provides an aerosol-generating article that contains an aerosol-generating substrate, wherein the aerosol-generating substrate contains homogenized plant material, wherein when the aerosol-generating substrate is heated according to Test Method A, an aerosol generated from the aerosol-generating substrate contains : eucalyptol in an amount of at least 0.2 micrograms per puff of aerosol; eucalyptin in an amount of at least 0.2 micrograms per puff of aerosol; and 8-desmethyleucalyptine in an amount of at least 0.2 micrograms per aerosol puff, wherein the aerosol puff has a volume of 55 milliliters generated by the smoking machine. According to the present invention, the amount of eucalyptol per puff is no more than twice the amount of eucalyptin per puff, and the amount of eucalyptol per gram of homogenized plant material is no more than twice the amount of 8-desmethyleucalyptin per puff.

The present invention further provides an aerosol generating substrate that contains homogenized plant material containing eucalyptus particles. Heating the aerosol-generating substrate in Test Method A generates an aerosol containing: at least 10 micrograms of eucalyptol per gram of aerosol-generating substrate, on a dry weight basis; at least 10 micrograms of eucalyptin per gram of aerosol-generating substrate, based on dry weight; and at least 10 micrograms of 8-desmethyleucalyptin per gram of aerosol-generating substrate, on a dry weight basis. According to the present invention, the amount of eucalyptol per gram of aerosol-generating substrate is not more than twice the amount of eucalyptol per gram of aerosol-generating substrate, and the amount of eucalyptol per gram of aerosol-generating substrate is not more than twice the amount of 8-desmethyl-eucalyptin per gram of aerosol-generating substrate.

The present invention further provides a method for generating an aerosol, comprising providing an aerosol generating article according to the present invention as defined above, and heating an aerosol generating substrate, the aerosol generating article, to a temperature in the range of 150 degrees Celsius to 400 degrees Celsius.

The present invention further provides an aerosol produced by heating an aerosol-generating substrate, the aerosol containing: eucalyptol in an amount of at least 0.2 micrograms per puff of the aerosol; eucalyptin in an amount of at least 0.2 micrograms per puff of aerosol; and 8-desmethyleucalyptin in an amount of at least 0.2 micrograms per puff of aerosol, wherein the aerosol puff has a volume of 55 milliliters generated by the smoking machine in Test Method A. According to the present invention, the amount of eucalyptol per puff is no more than twice the amount of eucalyptin per puff, and the amount of eucalyptol per gram of homogenized plant material is no more than twice the amount of 8-desmethyleucalyptin per puff.

The present invention further provides a method for making an aerosol generating substrate, comprising: forming a pulp containing eucalyptus particles, optionally tobacco particles, water, a binder and an aerosol generating agent; casting or extruding pulp into sheet or filament form; and drying sheets or threads in the range of 80 to 160 degrees Celsius. Once a sheet of aerosol generating substrate is formed, the sheet may optionally be cut into threads or the sheet may be assembled to form a rod. The sheet may optionally be corrugated prior to the gathering step.

Any references below to aerosol generating substrates and aerosols of the present invention should be considered to apply to all aspects of the present invention unless otherwise indicated.

As used herein, the term “aerosol-generating article” refers to an aerosol-generating article, the article comprising an aerosol-generating substrate that is suitable and intended to be heated or burned to release volatile compounds that can form an aerosol. A regular cigarette is lit when the user brings a flame to one end of the cigarette and draws air through the other end. The localized heat provided by the flame and oxygen in the air drawn through the cigarette causes the end of the cigarette to ignite, and the resulting combustion generates inhaled smoke. In contrast, in "heated aerosol-generating products" the aerosol is generated by heating the aerosol-generating substrate rather than burning the aerosol-generating substrate. Known heated aerosol generating articles include, for example, electrically heated aerosol generating articles and aerosol generating articles in which aerosol is generated by heat transfer from a combustible fuel element or heat source to a physically separated aerosol generating substrate.

Also known are aerosol generating articles that are adapted for use in an aerosol generating system that supplies an aerosol generating agent to the aerosol generating articles. In such a system, the aerosol generating substrate in the aerosol generating articles contains substantially less aerosol generating agent relative to the aerosol generating substrate that contains and provides substantially all of the aerosol generating agent used in generating the aerosol during operation.

As used herein, the term “aerosol generating substrate” refers to a substrate capable of releasing volatile compounds when heated that can form an aerosol. Aerosol generated from aerosol-generating substrates may be visible or invisible to the human eye and may contain vapors (e.g., fine particles of substances that are gaseous and usually liquid or solid at room temperature), as well as gases and liquid droplets condensed vapors.

As used herein, the term “homogenized plant material” includes any plant material formed by agglomerating plant particles. For example, sheets or webs of homogenized plant material for aerosol generating substrates according to the present invention can be formed by agglomerating particles of plant material obtained by grinding, grinding or grinding eucalyptus plant material and optionally one or more of tobacco leaf blades and veins tobacco leaf. Homogenized plant material can be produced through casting, extrusion, papermaking processes, or any other suitable methods known in the art.

As used herein, the term "eucalyptus particles" covers particles derived from plants of the genus Eucalyptus, preferably particles derived from one or more of E. globulus, E. radiata, E. citriodora and E. smithii, most preferably particles derived from E. globulus, such as crushed or powdered eucalyptus leaf blades and crushed or powdered eucalyptus leaf stems. Eucalyptus leaf particles are made exclusively from the leaf of the eucalyptus plant. Eucalyptus stem particles are made exclusively from the leaf stem of the eucalyptus plant. The eucalyptus particles in the aerosol generating substrate of the present invention may comprise either eucalyptus leaf particles or eucalyptus stem particles, or both eucalyptus leaf particles and eucalyptus stem particles.

In contrast, eucalyptus essential oil is a distillate, and eucalyptol is a compound derived from eucalyptus. They are not considered eucalyptus particles and are not included in the percentage of particulate plant material.

The present invention provides an aerosol generating article that contains an aerosol generating substrate formed from homogenized plant material containing eucalyptus particles and an aerosol obtained from such an aerosol generating substrate. The inventors of the present invention have discovered that by incorporating eucalyptus particles into an aerosol-generating substrate, it is advantageously possible to obtain an aerosol that allows a new sensation to be experienced. This aerosol provides a unique flavor and can provide increased levels of fullness in the mouth.

In addition, the present inventors have discovered that it is advantageously possible to obtain an aerosol with improved eucalyptus aroma and flavor compared to an aerosol obtained by adding eucalyptus additives such as eucalyptus oil. Eucalyptus oil is distilled from the leaf of the eucalyptus plant and has a flavor composition that differs from eucalyptus particles, presumably due to the distillation process, which can selectively remove or retain certain flavors. Moreover, in some aerosol generating substrates provided herein, eucalyptus particles may be included at a sufficient level to impart the desired eucalyptus flavor while maintaining a sufficient amount of tobacco material to provide the desired level of nicotine to the consumer.

Additionally, it has surprisingly been found that the inclusion of eucalyptus particles in an aerosol generating substrate provides a significant reduction in certain undesirable aerosol compounds compared to an aerosol produced from an aerosol generating substrate containing 100 percent tobacco particles without eucalyptus particles.

The flavor emitted by eucalyptus is due to the presence of one or more volatile flavoring agents that evaporate and become aerosolized when heated. Eucalyptol (1-8-cineole, chemical formula: C ₁₀ H ₁₈ O, Chemical Abstracts number 470-82-6) typically makes up from about 62.4% to about 82.2% of the essential oil eucalyptus (number according to the abstract journal “Chemical Abstracts” 8000-48-4) by weight. In addition to eucalyptol, eucalyptus contains terpineol, sesquiterpene alcohols, various aliphatic aldehydes, isoamyl alcohol, ethanol and terpenes (Fenaroli's Handbook of Flavor Ingredients, 6th Ed. / George A. Burdock, 2010. ISBN 978-1-4200-9077-2).

The presence of eucalyptus in homogenized plant material (such as molded leaf) can be accurately determined using DNA barcoding. Methods for performing DNA barcoding based on the nuclear ITS2 gene, the rbcL and matK system, and the plastid intergenic spacer trnH-psbA are well known in the art and can be used (Chen S, Yao H, Han J, Liu C, Song J , et al. (2010) Validation of the ITS2 Region as a Novel DNA Barcode for Identifying Medicinal Plant Species. PLoSONE 5(1): e8613; Hollingsworth PM, Graham SW, Little DP (2011) Choosing and Using a Plant DNA Barcode. PLoS ONE 6(5): e19254).

The inventors of the present invention have conducted a sophisticated analysis and characterization of aerosols generated from the aerosol generating substrates of the present invention, which contain eucalyptus particles and a mixture of eucalyptus and tobacco particles, and comparing these aerosols with aerosols obtained from existing aerosol generating substrates formed from tobacco material without eucalyptus particles. Based on this, the present inventors were able to identify a group of “signature compounds” that are compounds present in aerosols and derived from eucalyptus particles. Thus, the detection of these characteristic compounds in an aerosol within a certain weight fraction range can be used to identify aerosols that are derived from an aerosol-generating substrate containing eucalyptus particles. These characteristic compounds are not present to a significant extent in aerosol generated from tobacco material. In addition, the proportion of characteristic compounds in the aerosol and the ratio of characteristic compounds to each other clearly indicate the use of eucalyptus plant material rather than eucalyptus oil. Likewise, the presence of these characteristic compounds in specific proportions in the aerosol-generating substrate indicates the inclusion of eucalyptus particles in the substrate.

Certain levels of characteristic compounds in the substrate and aerosol are specific to eucalyptus particles present in homogenized plant material. The level of each characteristic compound depends on the manner in which the eucalyptus particles were processed during the preparation of the homogenized plant material. The level also depends on the composition of the homogenized plant material and, in particular, will be affected by the level of other components in the homogenized plant material. The level of characteristic compounds in homogenized plant material will be different from the level of the same compound in the original eucalyptus material. It will also differ from the level of characteristic compounds in materials containing eucalyptus particles, but which do not comply with the present invention, as defined herein.

To characterize aerosols, the present inventors used complementary non-targeted differential screening (NTDS) using liquid chromatography coupled with high resolution mass spectrometry (LC-HRAM-MS) in parallel with two-dimensional gas chromatography coupled with time-of-flight mass. spectrometry (GCxGC-TOFMS).

Non-targeted screening (NTS) is a key technique for characterizing the chemical composition of complex matrices by matching unknown detected compound properties with spectral databases (putative screening analysis [SSA]) or, if preliminary data do not match, by elucidating the structure of the unknowns using, for example, information obtained from first-order fragmentation (MS/MS) compared with in silico predicted fragments from compound databases (non-targeted analysis [NTA]). It provides simultaneous measurement and the ability to semi-quantitate large numbers of small molecules in samples using an unbiased approach.

If the focus is on comparing two or more aerosol samples as described above, non-targeted differential screening (NTDS) can be performed to evaluate any significant differences in chemical composition between samples without controls, or if preliminary group-related data are available between groups of samples ). A complementary differential screening approach was applied using liquid chromatography coupled with high resolution mass spectrometry with accurate mass determination (LC-HRAM-MS) in parallel with two-dimensional gas chromatography coupled with time-of-flight mass spectrometry (GCxGC-TOFMS) to provide comprehensive analytical coverage to identify the most significant differences in aerosol composition between aerosols derived from articles containing 100% by weight eucalyptus as particulate plant material and aerosols obtained from articles containing 100% by weight tobacco as particulate plant material .

The aerosol was generated and collected using the device and methodology detailed below.

LC-HRAM-MS analysis was performed using a Thermo QExactive ^TM high-resolution mass spectrometer in both full scan and data-dependent modes. A total of three different methods were used to cover a wide range of substances with different ionization properties and compound classes. Samples were analyzed by RP chromatography with heated electrospray ionization (HESI) in both positive and negative modes and atmospheric pressure chemical ionization (APCI) in positive mode. The methods are described in the following documents: Arndt, D. et al, “Indepth characterization of chemical differences between heat-not-burn tobacco products and cigarettes using LC-HRAM-MS-based non-targeted differential screening” (DOI:10.13140/RG. 2.2.11752.16643); Wachsmuth, C. et al, “Comprehensive chemical characterization of complex matrices through integration of multiple analytical modes and databases for LC-HRAM-MS-based non-targeted screening” (DOI: 10.13140/RG.2.2.12701.61927); and “Buchholz, C. et al, “Increasing confidence for compound identification by fragmentation database and in silico fragmentation comparison with LC-HRAM-MS-based non-targeted screening of complex matrices” (DOI: 10.13140/RG.2.2.17944.49927) , all from the 66th ASMS Conference on Mass Spectrometry and Related Subjects, San Diego, USA (2018).

GCxGC-TOFMS analysis was performed using an Agilent GC model 6890A or 7890A equipped with an automatic liquid nebulizer (model 7683B) and a thermal modulator coupled to a LECO Pegasus 4D™ mass spectrometer in three different ways for nonpolar, polar, and highly volatile compounds in the aerosol. The methods are described in the following documents: Almstetter. et al, “Non-targeted screening using GC×GC-TOFMS for in-depth chemical characterization of aerosol from a heat-not-burn tobacco product” (DOI: 10.13140/RG.2.2.36010.31688/1); and Almstetter. et al, “Non-targeted differential screening of complex matrices using GC×GC-TOFMS for comprehensive characterization of the chemical composition and determination of significant differences” (DOI: 10.13140/RG.2.2.32692.55680), obtained from 66 and 64 1st ASMS Conference on Mass Spectrometry and Related Subjects, San Diego, USA, respectively.

The results of the analytical methods provided information on the main compounds responsible for the differences in aerosols generated by such products. The untargeted differential screening using both LC-HRAM-MS and GCxGC-TOFMS analytical platforms targeted compounds that were present at high levels in aerosols of a sample of the aerosol-generating substrate of the present invention containing 100 percent eucalyptus particles relative to a comparative sample of the aerosol-generating substrate containing 100 percent tobacco particles. The NTDS methodology is described in the documents listed above.

Based on this information, the present inventors were able to identify specific compounds in the aerosol that could be considered “signature compounds” derived from the eucalyptus particles in the substrate. Characteristic compounds unique to eucalyptus include, but are not limited to: eucalyptin, 8-desmethyleucalyptin and eucalyptol. For purposes of the present invention, targeted screening may be performed on a sample of the aerosol-generating substrate to identify the presence and amount of each of the characteristic compounds in the substrate. This targeted screening method is described below. As described, characteristic compounds can be detected and measured in both the aerosol-generating substrate and the aerosol derived from the aerosol-generating substrate.

As defined above, the aerosol generating article of the present invention contains an aerosol generating substrate formed from homogenized plant material containing eucalyptus particles. As a result of the inclusion of eucalyptus particles, the aerosol-generating substrate contains certain proportions of eucalyptus "signature compounds" as described above. Specifically, the aerosol generating substrate contains at least 0.04 mg of eucalyptol per gram of substrate, at least 0.2 mg of eucalyptin per gram of substrate, and at least 0.2 mg of 8-desmethyleucalyptin per gram of substrate on a dry basis. weight.

By defining the aerosol-generating substrate relative to the desired levels of signature compounds, consistency between products can be achieved despite potential differences in the levels of signature compounds in the starting materials. This advantageously allows for more effective control of the quality of the product.

Preferably, the aerosol generating substrate contains at least about 0.1 mg of eucalyptol per gram of substrate, more preferably about 0.5 mg of eucalyptol per gram of substrate on a dry weight basis. Alternatively or additionally, the aerosol generating substrate preferably contains no more than about 4 mg of eucalyptol per gram of substrate, more preferably no more than about 2 mg of eucalyptol per gram of substrate, and more preferably no more than about 1 mg of eucalyptol per gram of substrate. For example, the aerosol generating substrate may contain from about 0.04 mg to about 4 mg of eucalyptol per gram of substrate, or from about 0.1 mg to about 2 mg of eucalyptol per gram of substrate, or from about 0.5 mg to about 1 mg of eucalyptol per gram of substrate. mg of eucalyptol per gram of substrate on a dry weight basis.

Preferably, the aerosol generating substrate contains at least about 2 mg of eucalyptin per gram of substrate, more preferably about 4 mg of eucalyptin per gram of substrate on a dry weight basis. Alternatively or additionally, the aerosol generating substrate preferably contains no more than about 8 mg of eucalyptin per gram of substrate, more preferably no more than about 7 mg of eucalyptin per gram of substrate, and more preferably no more than about 6 mg of eucalyptin per gram of substrate. For example, the aerosol generating substrate may contain from about 0.2 mg to about 8 mg eucalyptin per gram of substrate, or from about 2 mg to about 7 mg eucalyptin per gram of substrate, or from about 4 mg to about 6 mg eucalyptin per gram substrate in terms of dry weight.

Preferably, the aerosol generating substrate contains at least about 2 mg of 8-desmethyl-eucalyptin per gram of substrate, more preferably at least about 4 mg of 8-desmethyl-eucalyptin per gram of substrate on a dry weight basis. Alternatively or additionally, the aerosol generating substrate preferably contains no more than about 8 mg of 8-desmethyl-eucalyptin per gram of substrate, more preferably no more than about 7 mg of 8-desmethyl-eucalyptin per gram of substrate, and more preferably no more than about 6 mg of 8-desmethyl-eucalyptin per gram of substrate. For example, the aerosol generating substrate may contain from about 0.2 mg to about 8 mg of 8-desmethyleucalyptin per gram of substrate, or from about 2 mg to about 7 mg of 8-desmethyleucalyptin per gram of substrate, or from about 4 mg to about 6 mg 8-desmethyleucalyptin per gram of substrate on a dry weight basis.

Preferably, the ratio of the characteristic compounds in the aerosol generating substrate is such that the amount of eucalyptin per gram of substrate is at least 3 times the amount of eucalyptol per gram of substrate, more preferably at least 4 times the amount of eucalyptol per gram of substrate on a dry basis weight. Alternatively or additionally, the amount of 8-desmethyleucalyptin per gram of substrate is at least 3 times the amount of eucalyptol per gram of substrate on a dry weight basis. The presence of eucalyptin and 8-desmethyleucalyptin at significantly higher levels than eucalyptol is characteristic of the inclusion of eucalyptus particles. In contrast, eucalyptus oil contains levels of eucalyptol that are significantly higher than the levels of eucalyptin and 8-desmethyleucalyptin.

As defined above, the present invention also provides an aerosol-generating article that contains an aerosol-generating substrate formed from homogenized plant material containing eucalyptus particles, wherein upon heating the aerosol-generating substrate, an aerosol is generated that contains "signature compounds" of eucalyptus.

For the purposes of the present invention, the aerosol generating substrate is heated according to "Test Method A". In Test Method A, an aerosol generating article that contains an aerosol generating substrate is heated in a Tobacco Heating System 2.2 holder (THS2.2 holder) according to a Health Canada approved machine smoking regime.

The tobacco heating system holder 2.2 (THS2.2 holder) corresponds to a commercially available iQOS device (Philip Morris Products SA, Switzerland), as described in Smith et al., 2016, Regul. Toxicol. Pharmacol. 81 (S2) S82-S92.

A Health Canada smoking regimen is a clearly defined and accepted smoking protocol as defined in Health Canada 2000 - Tobacco Products Information Regulations SOR/2000-273, Schedule 2; published by the Department of Justice of Canada. The test method is described in ISO/TR 19478-1:2014. In the Health Canada-approved smoking test, aerosol is collected from a sample of the aerosol-generating substrate for 12 puffs with a puff volume of 55 millimeters, puff duration of 2 seconds, and puff interval of 30 seconds, with all ventilation blocked if ventilation is present.

Thus, in the context of the present invention, the expression "when heating the aerosol-generating substrate according to Test Method A" means heating the aerosol-generating substrate in the THS2.2 holder according to the machine smoking regime approved by Health Canada, as defined in Health Canada 2000 - Tobacco Products Information Regulations SOR/2000-273, Schedule 2; published by Justice Canada, with the test method described in ISO/TR 19478-1:2014.

For analysis purposes, the aerosol generated by heating the aerosol-generating substrate is collected using a suitable device depending on the analysis method to be used.

In a suitable method for generating samples for LC-HRAM-MS analysis, the dispersed phase is captured using a standard 44 mm Cambridge glass fiber filter pad (according to ISO 3308) and a filter holder (according to ISO 4387 and ISO 3308). The remaining gas phase is collected downstream of the filter pad using two microimpingers (20 ml) in series, each containing methanol and an internal standard solution (ISTD) (10 ml), maintained at -60 degrees Celsius, using a mixture consisting of dry ice and isopropanol. The captured dispersed phase and gas phase are then recombined and extracted using methanol from the microimpinger by shaking the sample, vigorously stirring for 5 minutes and centrifuging (4500 g, 5 minutes, 10 degrees Celsius). The resulting extract is diluted with methanol and mixed in an Eppendorf thermal mixer (5 degrees Celsius, 2000 rpm). The test samples from the extract are analyzed by LC-HRAM-MS in a combination of full scan mode and fragmentation mode depending on the data to identify characteristic compounds. For the purposes of the present invention, LC-HRAM-MS analysis is suitable for the identification and quantification of eucalyptin and 8-desmethyleucalyptin.

Samples for GCxGC-TOFMS analysis can be generated in a similar manner, but for GCxGC-TOFMS analysis, different solvents are suitable for the extraction and analysis of polar compounds, non-polar compounds, and volatile compounds isolated from the entire aerosol.

For non-polar and polar compounds, all aerosol is collected using a standard 44mm Cambridge glass fiber filter pad (to ISO 3308) and a filter holder (to ISO 4387 and ISO 3308) and the two micro-impingers are connected and sealed in series. Each microimpinger (20 mL) contains 10 mL of dichloromethane/methanol (80:20 v/v) containing internal standard (ISTD) and retention index marker (RIM) compounds. Microimpingers are maintained at -80 degrees Celsius using a mixture of dry ice and isopropanol. For the analysis of non-polar compounds, the dispersed phase of the entire aerosol is extracted from a glass fiber filter pad using the contents of microimpingers. Water is added to an aliquot (10 ml) of the resulting extract, and the sample is vortexed and centrifuged as described above. The dichloromethane layer is separated, dried with sodium sulfate and analyzed by GCxGC-TOFMS in full scan mode. To analyze polar compounds, use the layer of water remaining from the preparation of the non-polar sample described above. ISTD and RIM compounds are added to the water layer, which is then directly analyzed by GCxGC-TOFMS in full scan mode.

For volatile compounds, the entire aerosol is collected using two series-connected and sealed microimpingers (20 mL), each filled with 10 mL of N,N-dimethylformamide (DMF) containing ISTD and RIM compounds. Microimpingers are maintained at -50 to -60 degrees Celsius using a mixture of dry ice and isopropanol. After collection, the contents of the two microimpingers are combined and analyzed by GCxGC-TOFMS in full scan mode.

For the purposes of the present invention, the GCxGC-TOFMS analysis is suitable for the identification and quantification of eucalyptol.

The aerosol generated by heating the aerosol generating substrate of the present invention according to Test Method A is characterized by the amounts and ratios of the representative compounds, eucalyptol, eucalyptin and 8-desmethyleucalyptin, as defined above.

According to the present invention, the aerosol contains at least 10 milligrams of eucalyptol per gram of aerosol-generating substrate, at least 10 milligrams of eucalyptin per gram of aerosol-generating substrate, and at least 10 milligrams of eucalyptin per gram of aerosol-generating substrate, based on dry weight .

The ranges define the amount of each of the characteristic compounds in the generated aerosol per gram of aerosol-generating substrate (also referred to herein as “substrate”). This equals the total amount of the characteristic compound measured in the aerosol collected during Test Method A divided by the dry weight of the aerosol-generating substrate before heating.

Preferably, the aerosol generated from the aerosol generating substrate of the present invention contains at least about 50 micrograms of eucalyptol per gram of substrate, more preferably at least about 200 micrograms of eucalyptol per gram of substrate. Alternatively or additionally, the aerosol generated from the aerosol generating substrate contains up to about 750 micrograms of eucalyptol per gram of substrate, preferably up to about 600 micrograms of eucalyptol per gram of substrate, and more preferably up to about 450 micrograms of eucalyptol per gram of substrate. For example, the aerosol generated from the aerosol generating substrate may contain from about 10 micrograms to about 750 micrograms of eucalyptol per gram of substrate, or from about 50 micrograms to about 600 micrograms of eucalyptol per gram of substrate, or from about 200 micrograms to about 450 micrograms of eucalyptol per gram of substrate.

Preferably, the aerosol generated from the aerosol generating substrate of the present invention contains at least about 50 micrograms of eucalyptin per gram of substrate, more preferably at least about 200 micrograms of eucalyptin per gram of substrate. Alternatively or additionally, the aerosol generated from the aerosol generating substrate contains up to about 750 micrograms of eucalyptin per gram of substrate, preferably up to about 600 micrograms of eucalyptin per gram of substrate, and more preferably up to about 450 micrograms of eucalyptin per gram of substrate. For example, the aerosol generated from the aerosol generating substrate may contain from about 10 micrograms to about 750 micrograms of eucalyptin per gram of substrate, or from about 50 micrograms to about 600 micrograms of eucalyptin per gram of substrate, or from about 200 micrograms to about 450 micrograms of eucalyptin per gram of substrate.

Preferably, the aerosol generated from the aerosol generating substrate of the present invention contains at least about 50 micrograms of 8-desmethyleucalyptin per gram of substrate, more preferably at least about 200 micrograms of 8-desmethyleucalyptin per gram of substrate. Alternatively or additionally, the aerosol generated from the aerosol generating substrate contains up to about 750 micrograms of 8-desmethyleucalyptin per gram of substrate, preferably up to about 600 micrograms of 8-desmethyleucalyptin per gram of substrate, and more preferably up to about 450 micrograms of 8-desmethyleucalyptin per gram of substrate. For example, an aerosol generated from an aerosol generating substrate may contain from about 10 micrograms to about 750 micrograms of 8-desmethyleucalyptin per gram of substrate, or from about 50 micrograms to about 600 micrograms of 8-desmethyleucalyptin per gram of substrate, or about 200 micrograms to about 450 micrograms of 8-desmethyleucalyptin per gram of substrate.

According to the present invention, the aerosol generated from the aerosol generating substrate during Test Method A has an amount of eucalyptol per gram of substrate that is no more than twice the amount of eucalyptin per gram of substrate. Therefore, the ratio of eucalyptol to eucalyptin is no more than 2:1.

Preferably, the amount of eucalyptol per gram of substrate is no more than 1.5 times the amount of eucalyptin per gram of substrate, resulting in a eucalyptol to eucalyptin ratio of no more than 1.5:1. More preferably, the amount of eucalyptol per gram of substrate is no more than 1.2 times the amount of eucalyptin per gram of substrate, resulting in a eucalyptol to eucalyptin ratio of no more than 1.2:1. More preferably, the amount of eucalyptol per gram of substrate is less than or equal to the amount of eucalyptol per gram of substrate, such that the ratio of eucalyptol to eucalyptin is no more than 1:1.

According to the present invention, the aerosol generated from the aerosol generating substrate during Test Method A has an amount of eucalyptol per gram of substrate that is no more than twice the amount of 8-desmethyleucalyptin per gram of substrate. Therefore, the amount of eucalyptol to 8-desmethyleucalyptin is no more than 2:1.

Preferably, the amount of eucalyptol per gram of substrate is no more than 1.5 times the amount of 8-desmethyleucalyptin per gram of substrate, resulting in a ratio of eucalyptol to 8-desmethyleucalyptin of no more than 1.5:1. More preferably, the amount of eucalyptol per gram of substrate is no more than 1.2 times the amount of eucalyptol per gram of substrate, resulting in a ratio of eucalyptol to 8-desmethyleucalyptin of no more than 1.2:1. More preferably, the amount of eucalyptol per gram of substrate is less than or equal to the amount of 8-desmethyleucalyptin per gram of substrate, such that the ratio of eucalyptol to 8-desmethyleucalyptin is no more than 1:1.

Preferably, the ratio of eucalyptin to 8-desmethyleucalyptin in the aerosol is from about 1.2:1 to 1:1.

Certain ratios of eucalyptol to eucalyptin and 8-desmethyleucalyptin characterize the aerosol that is obtained from eucalyptus particles. In contrast, in an aerosol derived from eucalyptus oil, the ratio of eucalyptol to eucalyptin and the ratio of eucalyptol to 8-desmethyleucalyptin will be significantly greater than 2:1. This is due to the relatively high proportion of eucalyptol in eucalyptus oil compared to eucalyptus plant material.

The aerosol produced from the aerosol-generating substrate of the present invention during Test Method A may further contain at least about 5 milligrams of aerosol-forming agent per gram of aerosol-generating substrate, or at least about 10 milligrams of aerosol per gram of substrate, or at least approximately 15 milligrams of aerosol-forming agent per gram of substrate. Alternatively or additionally, the aerosol may contain up to about 30 milligrams of an aerosolizing agent per gram of substrate, or up to about 25 milligrams of an aerosolizing agent per gram of substrate, or up to about 20 milligrams of an aerosolizing agent per gram of substrate. For example, an aerosol may contain from about 5 milligrams to about 30 milligrams of an aerosol-forming agent per gram of substrate, or from about 10 milligrams to about 25 milligrams of an aerosol-forming agent per gram of substrate, or from about 15 milligrams to about 20 milligrams of an aerosol-forming agent per gram of substrate. aerosol per gram of substrate. In alternative embodiments, the aerosol may contain less than 5 milligrams of aerosol-forming agent per gram of substrate. This may be suitable, for example, if the aerosol generating substance is provided separately within the aerosol generating article or aerosol generating device.

Aerosol-forming agents suitable for use in the present invention are presented below.

Various methods known in the art can be used to measure the amount of aerosol-forming agent in an aerosol.

Preferably, the aerosol produced from the aerosol generating substrate of the present invention during Test Method A further contains at least about 0.1 microgram of nicotine per gram of substrate, more preferably at least about 1 microgram of nicotine per gram of substrate, more preferably at least at least approximately 2 micrograms of nicotine per gram of substrate. Preferably, the aerosol contains up to about 10 micrograms of nicotine per gram of substrate, more preferably up to about 7.5 micrograms of nicotine per gram of substrate, more preferably up to about 4 micrograms of nicotine per gram of substrate. For example, an aerosol may contain from about 0.1 microgram to about 10 micrograms of nicotine per gram of substrate, or from about 1 microgram to about 7.5 micrograms of nicotine per gram of substrate, or from about 2 micrograms to about 4 micrograms of nicotine per gram of substrate. In some embodiments of the present invention, the aerosol may contain zero micrograms of nicotine.

Various methods known in the art can be used to measure the amount of nicotine in an aerosol.

Alternatively or additionally, the aerosol produced from the aerosol generating substrate of the present invention during Test Method A may optionally further contain at least about 20 milligrams of a cannabinoid compound per gram of substrate, more preferably at least about 50 milligrams of a cannabinoid compound per gram of substrate. more preferably at least about 100 milligrams of cannabinoid compound per gram of substrate. Preferably, the aerosol contains up to about 250 milligrams of a cannabinoid compound per gram of substrate, more preferably up to about 200 milligrams of a cannabinoid compound per gram of substrate, more preferably up to about 150 milligrams of a cannabinoid compound per gram of substrate. For example, an aerosol may contain from about 20 milligrams to about 250 milligrams of a cannabinoid compound per gram of substrate, or from about 50 milligrams to about 200 milligrams of a cannabinoid compound per gram of substrate, or from about 100 milligrams to about 150 milligrams of a cannabinoid compound per gram of substrate. In some embodiments of the present invention, the aerosol may contain zero micrograms of a cannabinoid compound.

Preferably the cannabinoid compound is selected from CBD and THC. More preferably, the cannabinoid compound is CBD.

Various methods known in the art can be used to measure the amount of cannabinoid compound in an aerosol.

Carbon monoxide may also be present in the aerosol generated from the aerosol generating substrate of the present invention during Test Method A and can be measured and used to further characterize the aerosol. Oxides of nitrogen, such as nitric oxide and nitrogen dioxide, may also be present in the aerosol and can be measured and used to further characterize the aerosol.

As described above, the presence of characteristic compounds in the aerosol in certain quantities and ratios indicates the inclusion of eucalyptus particles in the homogenized plant material forming the aerosol-generating substrate.

Preferably, the aerosol generating substrate of the present invention comprises homogenized plant material containing at least about 2.5 percent by weight of eucalyptus particles on a dry weight basis. Preferably, the particulate plant material comprises at least about 5 percent by weight of eucalyptus particles, more preferably at least about 10 percent by weight of eucalyptus particles, more preferably at least about 15 percent by weight of eucalyptus particles, more preferably at least about 20 percent by weight of eucalyptus particles, more preferably at least about 30 percent by weight of eucalyptus particles on a dry weight basis.

In certain embodiments of the present invention, the plant particles forming the homogenized plant material may comprise at least 98 percent by weight of eucalyptus particles, or at least 95 percent by weight of eucalyptus particles, or at least 90 percent by weight of eucalyptus particles based on dry weight of plant particles. Thus, in such embodiments, the aerosol generating substrate comprises eucalyptus particles substantially free of other plant particles.

In alternative embodiments of the present invention, the homogenized plant material may contain eucalyptus particles in combination with at least one of tobacco particles or hemp particles, as described below.

In the following description of the present invention, the term “particulate plant material” is used to refer collectively to the particles of plant material that are used to form homogenized plant material. The particulate plant material may consist essentially of eucalyptus particles or may be a mixture of eucalyptus particles with tobacco particles, hemp particles, or both tobacco particles and hemp particles.

The homogenized plant material may contain up to approximately 95 percent by weight of eucalyptus particles on a dry weight basis. Preferably, the homogenized plant material contains up to about 90 percent by weight of eucalyptus particles, more preferably up to about 80 percent by weight of eucalyptus particles, more preferably up to about 70 percent by weight of eucalyptus particles, more preferably up to about 60 percent by weight of eucalyptus particles, more preferably up to approximately 50 percent by weight of eucalyptus particles on a dry weight basis.

For example, the homogenized plant material may contain from about 2.5 percent to about 95 percent by weight of eucalyptus particles, or from about 5 percent to about 90 percent by weight of eucalyptus particles, or from about 10 percent to about 80 percent by weight of eucalyptus particles, or from about 15 percent to about 70 percent by weight of eucalyptus particles, or from about 20 percent to about 60 percent by weight of eucalyptus particles, or from about 30 percent to about 50 percent by weight of eucalyptus particles on a dry weight basis.

As described above, the present inventors have identified a number of "signature compounds" which are compounds characteristic of the eucalyptus plant and thus indicative of the inclusion of eucalyptus plant particles in the aerosol-generating substrate.

The amounts of characteristic compounds present in pure eucalyptus particles are expected to differ from those present in the aerosol-generating substrate. The substrate manufacturing process, which includes hydration in a slurry or slurry and drying at elevated temperatures, as well as the presence of other ingredients, including an aerosolizing agent and a binder, will vary the amounts of each of the characteristic compounds differently. The integrity of the eucalyptus particles and the stability of the compound under temperature and manipulation during production will also influence the final amount of the characteristic compound that is present in the substrate. It is therefore expected that the ratio of the characteristic compounds to each other will be different after the inclusion of eucalyptus particles in the substrate in different physical forms, for example in the form of sheets, threads and granules.

The presence of eucalyptus in the aerosol-generating substrate and the proportion of eucalyptus provided in the aerosol-generating substrate can be determined by measuring the amount of signature compounds in the substrate and comparing it with the corresponding amount of signature compounds in pure eucalyptus material. The presence and amount of characteristic compounds can be determined using any suitable techniques known to one skilled in the art.

In a suitable procedure, a sample of 250 milligrams of aerosol-generating substrate is mixed with 5 milliliters of methanol and extracted by vortexing, vigorous stirring for 5 minutes, and centrifugation (4500 g, 5 minutes, 10 degrees Celsius). Aliquots (300 microliters) of the extract are transferred to a silanized chromatography vial and diluted with methanol (600 microliters) and internal standard solution (ISTD) (100 microliters). The bottles are closed and their contents are mixed for 5 minutes using an Eppendorf thermal mixer (5 degrees Celsius; 2000 rpm). Test samples from the resulting extract are analyzed by LC-HRAM-MS in a combination of full scan mode and fragmentation mode depending on the data to identify representative compounds.

Preferably, the homogenized plant material further contains up to about 92 percent by weight of tobacco particles on a dry weight basis.

For example, the homogenized plant material preferably contains from about 10 percent to about 92 percent by weight of tobacco particles, more preferably from about 20 percent to about 90 percent by weight of tobacco particles, more preferably from about 30 percent to about 85 percent by weight of tobacco particles, more preferably from about 40 percent to about 80 percent by weight of tobacco particles, more preferably from about 50 percent to about 70 percent by weight of tobacco particles on a dry weight basis.

The weight ratio of eucalyptus particles to tobacco particles in the particulate plant material forming the homogenized plant material may vary depending on the desired flavor characteristics and aerosol composition.

Preferably, the ratio of eucalyptus particles to tobacco particles is no more than about 1:4, more preferably no more than about 1:5, more preferably no more than about 1:6, more preferably no more than about 1:7, and more preferably no more than approximately 1:8. In one particularly preferred embodiment, the homogenized plant material comprises a 1:4 weight ratio of eucalyptus particles to tobacco particles, which corresponds to a particulate plant material consisting of approximately 20 percent by weight eucalyptus particles and approximately 80 percent by weight tobacco particles. For a homogenized plant material formed from approximately 75 percent by weight of particulate plant material, this corresponds to approximately 15 percent by weight of eucalyptus particles and approximately 60 percent by weight of tobacco particles in the homogenized plant material on a dry weight basis.

In another embodiment, the homogenized plant material comprises a 1:9 weight ratio of eucalyptus particles to tobacco particles. In yet another embodiment, the homogenized plant material comprises a 1:30 weight ratio of eucalyptus particles to tobacco particles.

For purposes of the present invention, the term "tobacco particles" describes particles of any plant belonging to the genus Nicotiana . The term “tobacco particles” includes shredded or powdered tobacco leaf blades, shredded or powdered tobacco leaf stems, tobacco dust, tobacco fines, and other particulate tobacco by-products generated during tobacco processing, handling, and shipping. In a preferred embodiment, the tobacco particles are substantially all derived from tobacco leaf blades. In contrast, separated nicotine and nicotine salts are compounds derived from tobacco, but are not considered tobacco particles for purposes of the present invention and are not included in the percentage of particulate plant material.

Tobacco particles can be obtained from one or more varieties of tobacco plants. Any type of tobacco can be used in the mixture. Examples of the types of tobacco that may be used include, but are not limited to, sun-cured tobacco, fire-cured tobacco, Burley tobacco, Maryland tobacco, Eastern tobacco, Virginia tobacco, and other specialty tobaccos.

Fire drying is a method of drying tobacco that is especially widely used with Virginia tobaccos. During the flue drying process, heated air is circulated through the tightly packed tobacco. During the first stage, tobacco leaves turn yellow and wither. During the second stage, the leaf blades dry out completely. During the third stage, the leaf stems dry out completely.

Burley tobacco plays an important role in many tobacco blends. Burley tobacco has a distinctive flavor and aroma, and also has the ability to absorb large quantities of sauce.

Oriental tobacco has small leaves and pronounced aromatic qualities. However, oriental tobacco has a milder flavor than, for example, Burley tobacco. Consequently, in general, oriental tobacco is used in relatively small proportions in tobacco blends.

Kasturi, Maduro and Yatim are the subtypes of sun-cured tobacco that can be used. Preferably, Kasturi tobacco and fire-cured tobacco may be used in a mixture to produce tobacco particles. Accordingly, the tobacco particles in the particulate plant material may comprise a mixture of Kasturi tobacco and fire-cured tobacco.

The tobacco particles may have a nicotine content of at least about 2.5 percent by weight on a dry weight basis. More preferably, the tobacco particles may have a nicotine content of at least about 3 percent, even more preferably at least about 3.2 percent, even more preferably at least about 3.5 percent, most preferably at least about 4 percent by weight in in terms of dry weight. When the aerosol generating substrate contains tobacco particles in combination with eucalyptus particles, types of tobacco having a higher nicotine content are preferred to maintain similar nicotine levels compared to conventional aerosol generating substrates without eucalyptus particles as the total amount of nicotine would otherwise be would be reduced by replacing tobacco particles with eucalyptus particles.

Nicotine may optionally be included in the aerosol generating substrate, although it is considered a non-tobacco material for purposes of the present invention. Nicotine may contain one or more nicotine salts selected from the list consisting of nicotine lactate, nicotine citrate, nicotine pyruvate, nicotine bitartrate, nicotine benzoate, nicotine pectate, nicotine alginate and nicotine salicylate. Nicotine may be included in addition to low nicotine tobacco, or nicotine may be included in an aerosol generating substrate that has reduced or no tobacco content.

Alternatively or in addition to including tobacco particles in the homogenized plant material of the aerosol generating substrate of the present invention, the homogenized plant material may contain up to 92 percent by weight of hemp particles on a dry weight basis. The term "cannabis particles" refers to particles of the hemp plant, such as the species Cannabis sativa, Cannabis indica , and Cannabis ruderalis .

For example, the particulate plant material may comprise from about 10 percent to about 92 percent by weight hemp particles, more preferably from about 20 percent to about 90 percent by weight tobacco particles, more preferably from about 30 percent to about 85 percent by weight particles tobacco, more preferably from about 40 percent to about 80 percent by weight of tobacco particles, more preferably from about 50 percent to about 70 percent by weight of tobacco particles on a dry weight basis.

One or more cannabinoid compounds may optionally be included in the aerosol generating substrate, although it is considered a non-hemp material for purposes of the present invention. As used herein with respect to the present invention, the term “cannabinoid compound” describes any of a class of naturally occurring compounds that are found in parts of the cannabis plant, namely Cannabis sativa , Cannabis indica and Cannabis ruderalis species. The cannabinoid compounds are particularly concentrated in the female flower heads and are commonly sold as hemp oil. The cannabinoid compounds found naturally in the hemp plant include tetrahydrocannabinol (THC) and cannabidiol (CBD). In the context of the present invention, the term “cannabinoid compounds” is used to describe both naturally occurring cannabinoid compounds and synthetically manufactured cannabinoid compounds.

For example, the aerosol generating substrate may contain a cannabinoid compound selected from the group consisting of: tetrahydrocannabinol (THC), tetrahydrocannabinolic acid (THCA), cannabidiol (CBD), cannabidiolic acid (CBDA), cannabinol (CBN), cannabigerol (CBG) , cannabigerol monomethyl ester (CBGM), cannabivarin (CBV), cannabidivarin (CBDV), tetrahydrocannabivarin (THCV), cannabichromene (CBC), cannabicyclol (CBL), cannabichromevarin (CBCV), cannabigerovarin (CBGV), cannabielsoin (CBE), cannabicitran ( CBT) and their combinations.

The homogenized plant material may further comprise a proportion of other flavoring particles in addition to the eucalyptus particles, or a combination of eucalyptus particles with at least one of tobacco particles and hemp particles (“particulate plant material”).

For purposes of the present invention, the term “other flavoring particles” refers to particles of plant material other than eucalyptus, tobacco and hemp that are capable of generating one or more flavoring agents when heated. This term should be considered to exclude particles of neutral plant material, such as cellulose, which do not contribute to the perceived effect of the aerosol-generating substrate. The particles can be obtained from crushed or powdered leaf blades, fruits, petioles, stems, roots, seeds, buds or bark from other plants. Flavor particles from plants suitable for inclusion in the aerosol generating substrate of the present invention are known to one skilled in the art and include, but are not limited to, clove particles and tea particles.

The composition of the homogenized plant material can advantageously be adjusted by mixing the desired amounts and types of particles from different plants. This allows the aerosol generating substrate to be formed from a single homogenized plant material, if desired, without the need for combining or mixing different mixtures, as is the case, for example, in the manufacture of conventional cut litter. Therefore, the fabrication of the aerosol generating substrate could potentially be simplified.

The particulate plant material used in the aerosol generating substrates of the present invention can be tailored to provide a desired particle size distribution. Particle size distributions are referred to herein as D values, wherein the D value refers to the percentage by number of particles that have a diameter less than or equal to the specified D value. For example, in a D95 particle size distribution, 95 percent by number of particles have diameter less than or equal to the specified D95 value, and 5 percent by number of particles have a diameter that is greater than the specified D95 value.

The particulate plant material may have a D95 value of greater than or equal to 20 microns to a D95 value of less than or equal to 300 microns. By this it is meant that the particulate plant material may have a distribution represented by any D95 value within the specified range, that is, the D95 may be 20 microns, or the D95 may be 25 microns, etc. , up to and including D95 can be equal to 300 microns. By providing a D95 value in this range, the inclusion of relatively large plant particles in the homogenized plant material is avoided. This is desirable since generating aerosol from such large plant particles is likely to be relatively inefficient. Additionally, the inclusion of large plant particles in homogenized plant material may adversely affect the consistency of the material.

Preferably, the particulate plant material may have a D95 value of greater than or equal to about 30 microns to a D95 value of less than or equal to about 120 microns, more preferably a D95 value of greater than or equal to about 40 microns to a D95 value of less than or equal to about 80 micron. Both the particulate eucalyptus material and the particulate tobacco material may have D95 values from greater than or equal to about 20 microns to D95 values less than or equal to about 300 microns, preferably D95 values from greater than or equal to 30 microns to D95 values less than or equal to about 120 microns, more preferably D95 values from greater than or equal to about 40 microns to D95 values less than or equal to about 80 microns.

In some embodiments, the particulate plant material may be specifically ground to form particles having a desired particle size distribution. Therefore, the use of specially ground plant material advantageously improves the uniformity of the particulate plant material and the consistency of the homogenized plant material.

The diameter of 100 percent of the particulate plant material may be less than or equal to about 350 microns, more preferably less than or equal to about 400 microns. The diameter of 100 percent eucalyptus particulate material and 100 percent tobacco particulate material may be less than or equal to about 400 microns, more preferably less than or equal to about 200 microns. The range of eucalyptus particle sizes allows eucalyptus particles to be combined with tobacco particles in existing sheet forming processes.

The homogenized plant material preferably contains at least about 55 percent by weight of particulate plant material containing eucalyptus particles as described above, more preferably at least about 60 percent by weight of particulate plant material, and more preferably at least about 65 percent by weight of particulate plant material on a dry weight basis. The homogenized plant material preferably contains no more than about 95 weight percent particulate plant material, more preferably no more than about 90 weight percent particulate plant material, and more preferably no more than about 85 weight percent particulate plant material in terms of dry weight. For example, the homogenized plant material may contain from about 55 percent to about 95 percent by weight particulate plant material, or from about 60 percent to about 90 percent by weight particulate plant material, or from about 65 percent to about 85 percent by weight particulate plant material on a dry weight basis. In one particularly preferred embodiment, the homogenized plant material contains approximately 75 percent by weight of particulate plant material on a dry weight basis.

Thus, the particulate plant material is typically combined with one or more other components to form a homogenized plant material.

The homogenized plant material may further comprise a binder to modify the mechanical properties of the particulate plant material, the binder being incorporated into the homogenized plant material during manufacture as described herein. Suitable exogenous binders are known to one skilled in the art and include, without limitation: gums such as, for example, guar gum, xanthan gum, acacia and locust bean gum; cellulose binders such as, for example, hydroxypropylcellulose, carboxymethylcellulose, hydroxyethylcellulose, methylcellulose and ethylcellulose; polysaccharides, such as, for example, starches, organic acids, such as alginic acid, salts of bases conjugate with organic acids, such as sodium alginate, agar and pectins; and their combinations. Preferably the binder contains guar gum.

The binder may be present in an amount from about 1 percent to about 10 percent by weight based on the dry weight of the homogenized plant material, preferably in an amount from about 2 percent to about 5 percent by weight based on the dry weight of the homogenized plant material.

Alternatively or additionally, the homogenized plant material may further comprise one or more lipids that promote the diffusivity of volatile components (eg, aerosol formers, eucalyptol, and nicotine), the lipid being incorporated into the homogenized plant material during manufacture as described herein. Lipids suitable for inclusion in the homogenized plant material include, but are not limited to: medium chain triglycerides, cocoa butter, palm oil, palm kernel oil, mango butter, shea butter seed oil, soybean oil, cottonseed oil, coconut oil, hydrogenated coconut oil, candelilla wax, carnauba wax, shellac, sunflower wax, rice bran wax and Revel A; and their combinations.

Alternatively or additionally, the homogenized plant material may further contain a pH modifier.

Alternatively or additionally, the homogenized plant material may further comprise fibers to modify the mechanical properties of the homogenized plant material, the fibers being incorporated into the homogenized plant material during manufacture as described herein. Exogenous fibers suitable for inclusion in homogenized plant material are known in the art and include fibers formed from non-tobacco material and non-eucalyptus material, including, but not limited to: cellulose fibers; softwood fibers; hardwood fibers; jute fibers and their combinations. Exogenous fibers derived from tobacco and/or eucalyptus may also be added. Any fibers added to homogenized plant material are not considered to form part of the “particulate plant material” as defined above. Before inclusion in the homogenized plant material, the fibers can be processed by suitable methods known in the art, including, without limitation: mechanical pulping; cleaning; chemical transformation into fibrous mass; whitening; sulfate transformation into fibrous mass; and their combinations. The fiber usually has a length greater than its width.

Suitable fibers typically have lengths greater than 400 micrometers and less than or equal to 4 mm, preferably in the range of 0.7 mm to 4 mm. Preferably, the fibers are present in an amount of from about 2 percent to about 15 percent by weight, most preferably at about 4 percent by weight, based on the dry weight of the substrate.

Alternatively or additionally, the homogenized plant material may further contain one or more aerosol-forming agents. Once evaporated, the aerosol-forming agent can carry other vaporized compounds released from the aerosol-generating substrate when heated, such as nicotine and flavoring agents, into the aerosol. The formation of an aerosol of specific compounds from the aerosol-generating substrate is determined not only by its boiling point. The amount of compound aerosolized may be influenced by the physical form of the substrate, as well as other components that are also present in the substrate. The stability of the compound under the influence of temperature and the time interval of aerosol generation will also affect the amount of compound that is present in the aerosol.

Aerosol-forming agents suitable for inclusion in homogenized plant material are known in the art and include, but are not limited to: polyhydric alcohols such as triethylene glycol, propylene glycol, 1,3-butanediol and glycerol; polyhydric alcohol esters such as glycerol mono-, di- or triacetate; and aliphatic esters of mono-, di- or polycarboxylic acids, such as dimethyl dodecanedioate and dimethyl tetradecanedioate.

The homogenized plant material may have an aerosol forming agent content of from about 5 percent to about 30 percent by weight on a dry weight basis, such as from about 10 percent to about 25 percent by weight on a dry weight basis, or from about 15 percent to about 20 percent by weight on a dry weight basis.

For example, if the substrate is to be used in an aerosol generating article for an electrical aerosol generating system having a heating element, it may preferably contain an aerosol generating agent content of from about 5 percent to about 30 percent by weight on a dry weight basis. If the substrate is to be used in an aerosol generating article for an electrical aerosol generating system having a heating element, the aerosol generating substance is preferably glycerol.

In other embodiments, the homogenized plant material may have an aerosol-forming agent content of from about 1 percent to about 5 percent by weight on a dry weight basis. For example, if the substrate is for use in an aerosol-generating article in which the aerosol-forming agent is held in a reservoir separate from the substrate, the substrate may have an aerosol-forming agent content of greater than 1 percent and less than about 5 percent. In such embodiments, the aerosol-forming agent is vaporized by heating and a stream of the aerosol-forming agent is contacted with the aerosol-generating substrate to capture flavoring agents from the aerosol-generating substrate in the aerosol.

The aerosol generating agent may act as a humectant in the aerosol generating substrate.

The homogenized plant material of the aerosol generating substrate according to the present invention may contain one type of homogenized plant material or two or more types of homogenized plant material having compositions or forms different from each other. For example, in one embodiment, the aerosol generating substrate comprises eucalyptus particles and tobacco particles or hemp particles contained in the same sheet of homogenized plant material. However, in other embodiments, the aerosol generating substrate may contain tobacco particles or hemp particles and eucalyptus particles in leaves that are different from each other.

The homogenized plant material may be provided in any suitable form. For example, the homogenized plant material may be in the form of one or more sheets. As used herein with reference to the present invention, the term "sheet" describes a layered element having a width and a length that is substantially greater than its thickness.

Alternatively or additionally, the homogenized plant material may be in the form of a plurality of beads or granules.

Alternatively or additionally, the homogenized plant material may be in a form that can fill a hookah cartridge or consumable, or that can be used in a hookah device. The present invention provides a cartridge or hookah device that contains homogenized plant material.

Alternatively or additionally, the homogenized plant material may be in the form of multiple strands, strips or pieces. As used herein, the term "thread" describes an elongated piece of material whose length is substantially greater than its width and thickness. The term "thread" should be considered to include strips, pieces and any other homogenized plant material having a similar shape. The strands of homogenized plant material may be formed by cutting or piecing a sheet of homogenized plant material or by other methods, such as an extrusion method.

In some embodiments, the filaments may be formed in situ in the aerosol-generating substrate as a result of separation or splitting of a sheet of homogenized plant material during formation of the aerosol-generating substrate, for example, as a result of crimping. The strands of homogenized plant material in the aerosol-generating substrate can be separated from each other. Alternatively, each strand of homogenized plant material in the aerosol generating substrate may be at least partially connected to an adjacent strand or strands along the length of the strands. For example, adjacent threads may be connected by one or more fibers. This may occur, for example, if the filaments were formed by splitting a sheet of homogenized plant material during the preparation of the aerosol generating substrate as described above.

Preferably, the aerosol generating substrate is provided in the form of one or more sheets of homogenized plant material. In various embodiments of the present invention, one or more sheets of homogenized plant material can be obtained from a casting process. In various embodiments of the present invention, one or more sheets of homogenized plant material can be obtained from a papermaking process. Each of the one or more sheets as described herein may individually have a thickness of from about 100 micrometers to 600 micrometers, preferably from 150 micrometers to 300 micrometers, and most preferably from 200 micrometers to 250 micrometers. Individual thickness refers to the thickness of an individual sheet, while cumulative thickness refers to the total thickness of all sheets that make up the aerosol generating substrate. For example, if the aerosol generating substrate is formed from two separate sheets, then the combined thickness is the sum of the thicknesses of the two individual sheets or the measured thickness of the two sheets when the two sheets are stacked on top of each other in the aerosol generating substrate.

Each of the one or more sheets as described herein may individually have a grammage of from about 100 ^gsm to about 300 ^gsm .

Each of the one or more sheets as described herein may individually have a density of from about 0.3 gsm³ up to approximately 1.3 g/cm³, and preferably from about 0.7 g/cm³ up to approximately 1.0 g/cm³.

The term "tensile strength" is used throughout this specification to indicate a measure of the force required to stretch a sheet of homogenized plant material until it breaks. More specifically, tensile strength is the maximum tensile force per unit width that the sheet material will withstand before breaking, and is measured in the machine direction or cross direction of the sheet material. It is expressed in units of newtons per meter of material (N/m). Tests for measuring the tensile strength of sheet material are well known. A suitable test is published in the 2014 publication of International Standard ISO 1924-2 entitled “Paper and paperboard. Determination of tensile strength. Part 2: Constant Rate Stretching Method.”

Materials and equipment required for testing according to ISO 1924-2: universal tensile/compression testing machine, Instron 5566, or equivalent; 100 Newton tension cell, Instron, or equivalent; two pneumatic grippers; steel measuring block 180 ± 0.25 millimeters long (width: approximately 10 millimeters, thickness: approximately 3 millimeters); strip cutter with two cutting edges, size 15 ± 0.05 x approximately 250 millimeters, Adamel Lhomargy, or equivalent; scalpel; PC-based data acquisition software, Merlin, or equivalent; and compressed air.

The sample is prepared as follows: first, incubate a sheet of homogenized plant material for at least 24 hours at a temperature of 22 ± 2 degrees Celsius and a relative humidity of 60 ± 5% before testing. The sample in the machine direction or cross direction is then cut to a size of approximately 250 x 15 ± 0.1 millimeters using a strip cutter with two cutting edges. The edges of the test samples must be trimmed carefully, so no more than three test samples are cut at a time.

The tensile/compression test apparatus is set up by installing a 100 Newton tensile force cell, turning on the universal tensile/compression testing machine and computer, and selecting the measurement method specified in the software, with the test speed set to 8 millimeters per hour. minute. Then the tensile force element is calibrated and pneumatic grippers are installed. The test distance between the pneumatic grips is adjusted to 180 ± 0.5 millimeters using a steel measuring block, the distance and force being set to zero.

The test sample is then placed directly and centrally between the grips, avoiding fingers touching the area to be tested. The upper grip is closed, with the paper strip hanging in the open lower grip. The force is set to zero. The paper strip is then pulled down slightly and closes the lower grip; the initial force should be between 0.05 and 0.20 newton. As the upper grip moves upward, gradually increasing force is applied until the test piece breaks. The same procedure is repeated with the remaining test samples. The result is valid when the test sample breaks when the clamps are separated to a distance of more than 10 millimeters. If this is not the case, the result is discarded and an additional measurement is performed.

Each of the one or more sheets of homogenized plant material as described herein may individually have a peak transverse tensile strength of from 50 N/m to 400 N/m, or preferably from 150 N/m to 350 N/m m. Given that sheet thickness affects tensile strength, and if thickness varies across a batch of sheets, it may be desirable to normalize the value to a specific sheet thickness.

Each of the one or more sheets as described herein may individually have a peak machine direction tensile strength of 100 N/m to 800 N/m, or preferably 280 N/m to 620 N/m, normalized relative to sheet thickness 215 microns. Machine direction refers to the direction in which the sheet material is wound onto or unwinded from a reel and fed into the machine, with the cross direction being perpendicular to the machine direction. These tensile strength values make the sheets and methods described herein particularly suitable for subsequent operations involving mechanical loads.

Providing a sheet having levels of thickness, grammage, and tensile strength as defined above advantageously optimizes the processability of the sheet to form an aerosol-generating substrate and ensures that damage, such as sheet tearing, is prevented during high-speed processing of the sheet.

In embodiments of the present invention in which the aerosol generating substrate comprises one or more sheets of homogenized plant material, the sheets are preferably in the form of one or more assembled sheets. As used herein, the term "assembled" is used to describe a sheet of homogenized plant material that is rolled, folded, or otherwise compressed or tapered in a direction substantially transverse to the cylindrical axis of the rod or rod. As used herein, the term “longitudinal” refers to the direction corresponding to the major longitudinal axis of the aerosol generating article that extends between the upstream and downstream ends of the aerosol generating article. During use, air is drawn longitudinally through the aerosol-generating product. The term "transverse" refers to a direction that is perpendicular to the longitudinal axis. As used herein, the term “length” refers to the dimension of a component in the longitudinal direction, and the term “width” refers to the dimension of the component in the transverse direction. For example, in the case of a rod or rod having a circular cross-section, the maximum width corresponds to the diameter of the circle.

As used herein, the term “rod” refers to a generally cylindrical element with a generally polygonal, circular, oval or elliptical cross-section. As used herein, the term “rod” refers to a generally cylindrical member with a substantially polygonal cross-section and preferably a circular, oval or elliptical cross-section. The rod may have a length that is greater than or equal to the length of the rod. As a rule, the rod has a length that is greater than the length of the rod. The rod may comprise one or more rods, preferably aligned in the longitudinal direction.

As used herein, the terms “upstream” and “downstream” describe the relative positions of elements or portions of elements of an aerosol generating article with respect to the direction in which the aerosol is transported during use through the aerosol generating article. The downstream end of the air flow path is the end through which the aerosol is delivered to the user of the product.

One or more sheets of homogenized plant material may be collected transversely to its longitudinal axis and surrounded by a wrapper to form a continuous rod or rod. A continuous rod can be divided into a number of individual rods or rods. The wrapper may be a paper wrapper or a non-paper wrapper. Paper wrappers suitable for use in particular embodiments of the present invention are known in the art and include, but are not limited to: types of cigarette papers; and filter ficells. Non-paper wrappers suitable for use in particular embodiments of the present invention are known in the art and include, without limitation, sheets of homogenized tobacco materials. Homogenized tobacco wrappers are particularly suitable for use in embodiments in which the aerosol generating substrate comprises one or more sheets of homogenized plant material formed from particulate plant material, wherein the particulate plant material comprises eucalyptus particles in combination with low percentage by weight of tobacco particles, for example, from 20 percent to 0 percent by weight of tobacco particles on a dry weight basis.

Alternatively, one or more sheets of homogenized plant material may be cut into threads as mentioned above. In such embodiments, the aerosol generating substrate comprises multiple strands of homogenized plant material. Threads can be used to form a rod. Typically, the width of such threads is about 5 mm, or about 4 mm, or about 3 mm, or about 2 mm or less. The length of the threads may be greater than about 5 mm, from about 5 mm to about 15 mm, from about 8 mm to about 12 mm, or about 12 mm. The length of the threads can be determined by a manufacturing process in which the rod is cut into shorter rods and the length of the threads corresponds to the length of the rod. Threads can be fragile, which can lead to breakage, especially during movement. In such cases, the length of some threads may be less than the length of the rod.

One or more sheets of homogenized plant material may be textured by crimping, embossing, or perforating. One or more sheets may be textured before being assembled or before being cut into threads. Preferably, one or more sheets of the homogenized plant material are corrugated prior to collection, whereby the homogenized plant material may be in the form of a corrugated sheet, more preferably in the form of a collected corrugated sheet. As used herein, the term “corrugated sheet” means a sheet having a plurality of substantially parallel folds or corrugations, generally aligned with the longitudinal axis of the product.

In one embodiment, the aerosol generating substrate may be in the form of a single rod of aerosol generating substrate. Preferably, the aerosol generating substrate rod may comprise multiple strands of homogenized plant material. Most preferably, the aerosol generating substrate rod may contain one or more sheets of homogenized plant material. Preferably, one or more sheets of homogenized plant material may be corrugated such that they have a plurality of folds or corrugations substantially parallel to the cylindrical axis of the rod. This treatment advantageously facilitates the collection of the corrugated sheet of homogenized plant material to form an extrusion. Preferably, one or more sheets of homogenized plant material may be collected. It should be understood that the corrugated sheets of homogenized plant material may alternatively or additionally have a plurality of substantially parallel folds or corrugations located at an acute or obtuse angle to the cylindrical axis of the rod. The sheet may be corrugated to such an extent that the integrity of the sheet is broken into multiple parallel folds or corrugations, causing the material to separate and resulting in pieces, strands or strips of homogenized plant material.

In another embodiment of the aerosol generating substrate, the homogenized plant material comprises a first rod containing the first homogenized plant material and a second rod containing the second homogenized plant material, wherein the first homogenized plant material contains from about 50 percent to about 95 percent by weight of eucalyptus particles in terms of dry weight; in terms of dry weight; and wherein the second homogenized plant material contains from about 50 percent to about 95 percent by weight of tobacco particles on a dry weight basis. In general, in accordance with the present invention, the homogenized plant materials in the aerosol generating substrate contain at least 2.5 percent by weight of eucalyptus particles and up to 95 percent by weight of tobacco particles on a dry weight basis.

Optionally, the first homogenized plant material may comprise at least 60 percent by weight of eucalyptus particles, and the second homogenized plant material may comprise at least 60 percent by weight of tobacco particles. Optionally, the first homogenized plant material may comprise at least about 90 percent by weight of a eucalyptus portion, and the second homogenized plant material may contain at least about 90 percent by weight of tobacco particles.

In such arrangements, the first homogenized plant material comprises a first particulate plant material with a major proportion of eucalyptus particles, and the second homogenized plant material comprises a second particulate plant material with a major proportion of tobacco particles.

Preferably, the first homogenized plant material may be in the form of one or more sheets, and the second homogenized plant material may be in the form of one or more sheets.

Optionally, the aerosol generating substrate may comprise one or more rods. Preferably, the substrate may comprise a first rod and a second rod, wherein a first homogenized plant material can be located in the first rod and a second homogenized plant material can be located in the second rod.

Two or more rods may be combined so that they are end to end and extend to form a rod. Two rods can be arranged in the longitudinal direction with a gap between them, as a result of which a cavity is created in the rod. The rods may be arranged in any suitable manner within the rod.

For example, in a preferred arrangement, a downstream rod containing a majority of eucalyptus particles may be adjacent to an upstream rod containing a majority of tobacco particles to form a rod. An alternative configuration is also provided in which the upstream and downstream positions of the respective rods are varied relative to each other. Alternative configurations are also provided in which the third homogenized plant material contains either a major proportion of eucalyptus particles or a major proportion of tobacco particles, and forming a third rod. For example, a rod containing the majority of eucalyptus particles by weight may be located between two rods, each of which contains a major proportion of tobacco particles by weight, or a rod containing the majority of tobacco particles by weight may be located between two rods, each of which which contains the bulk of eucalyptus particles by weight. Additional configurations may be contemplated by one skilled in the art. If two or more extensions are provided, the homogenized plant material may be provided in the same form in each extension or in different forms in each extension, that is, it can be collected or divided into pieces. One or more rods may optionally be wrapped individually or together in metal foil, such as aluminum foil or metallized paper. Metal foil or metallized paper serves the purpose of quickly conducting heat through the aerosol-generating substrate. Metal foil or metallized paper may contain metal particles, such as iron particles.

The first rod may contain one or more sheets of the first homogenized plant material, and the second rod may contain one or more sheets of the second homogenized plant material. The sum of the rod lengths may range from about 10 mm to about 40 mm, preferably from about 10 to about 15 mm, more preferably about 12 mm. The first rod and the second rod may have the same length or may have different lengths. If the first rod and the second rod have the same lengths, the length of each rod may preferably be from about 6 mm to about 20 mm. Preferably, the second rod may be longer than the first rod to provide the desired ratio of tobacco particles to eucalyptus particles in the substrate. In general, preferably the substrate contains from 0 to 72.5 percent by weight of tobacco particles and from 75 to 2.5 percent by weight of eucalyptus particles on a dry weight basis. Preferably, the second rod is at least 40 percent to 50 percent longer than the first rod.

If the first homogenized plant material and the second homogenized plant material are in the form of one or more sheets, preferably the one or more sheets of the first homogenized plant material and the second homogenized plant material may be assembled sheets. Preferably, one or more sheets of the first homogenized plant material and the second homogenized plant material may be corrugated sheets. It should be understood that all other physical properties described with reference to an embodiment in which one homogenized plant material is present apply equally to the embodiment in which a first homogenized plant material and a second homogenized plant material are present. In addition, it should be understood that the description of additives (such as binders, lipids, fibers, aerosol formers, humectants, plasticizers, flavoring agents, fillers, aqueous and non-aqueous solvents, and combinations thereof) with reference to an embodiment in which one homogenized plant material is equally applicable to an embodiment in which a first homogenized plant material and a second homogenized plant material are present.

In yet another embodiment of the aerosol generating substrate, the first homogenized plant material is in the form of a first leaf, the second homogenized plant material is in the form of a second leaf, and the second leaf at least partially overlaps the first leaf.

The first sheet may be a textured sheet and the second sheet may be non-textured.

Both the first and second sheets may be textured sheets.

The first sheet may be a textured sheet that is textured differently from the second sheet. For example, the first sheet may be corrugated and the second sheet may be perforated. Alternatively, the first sheet may be perforated and the second sheet may be corrugated.

Both the first and second sheets may be corrugated sheets that are morphologically different from each other. For example, the second sheet may be corrugated with a different number of corrugations per unit sheet width than the first sheet.

The sheets can be collected to form a rod. The sheets that are assembled together to form a rod can have different physical dimensions. The width and thickness of the sheets may vary.

It may be desirable to assemble two sheets together, each of which has a different thickness, or each of which has a different width. This can change the physical properties of the rod. This may facilitate the formation of a mixture of aerosol-generating substrate from sheets with different chemical compositions.

The first sheet may have a first thickness, and the second sheet may have a second thickness that is a multiple of the first thickness, for example, the second sheet may have a thickness that is two or three times the first thickness.

The first sheet may have a first width and the second sheet may have a second width that is different from the first width.

The first sheet and the second sheet may be arranged in an overlapping manner before or as they are assembled with each other. Sheets can have the same width and thickness. Sheets can have different thicknesses. Sheets can have different widths. Sheets can be textured in different ways.

If it is desired that both the first sheet and the second sheet are textured, the sheets may be textured simultaneously before gathering. For example, the sheets may be arranged in an overlapping manner and passed through texturing means such as a pair of corrugating rollers. An apparatus and method suitable for simultaneous corrugation are described with reference to FIGS. 2 documents WO-A-2013/178766. In a preferred embodiment, a second sheet of the second homogenized plant material overlaps the first sheet of the first homogenized plant material, and the combined sheets are collected to form an aerosol-generating substrate rod. Optionally, the sheets may be corrugated together before gathering to facilitate assembly.

Alternatively, each sheet can be textured individually and then they can be brought together to form an extruder. For example, if two sheets have different thicknesses, it may be desirable to corrugate the first sheet differently relative to the second sheet.

It should be understood that all other physical properties described with reference to an embodiment in which one homogenized plant material is present apply equally to the embodiment in which a first homogenized plant material and a second homogenized plant material are present. In addition, it should be understood that the description of additives (such as binders, lipids, fibers, aerosol formers, humectants, plasticizers, flavoring agents, fillers, aqueous and non-aqueous solvents, and combinations thereof) with reference to an embodiment in which one homogenized plant material is equally applicable to an embodiment in which a first homogenized plant material and a second homogenized plant material are present.

The homogenized plant material used in the aerosol generating substrates of the present invention can be produced through a variety of processes, including papermaking, casting, reconstitution, extrusion, or any other suitable process.

In certain embodiments, a casting process is used to produce the "molded sheet". The term "molded sheet" is used herein to mean a sheet product made by a casting process that is based on the casting of a pulp containing plant particles (for example, eucalyptus particles, or tobacco particles and eucalyptus particles in a mixture) and a binder (for example, guar gum ), onto a support surface such as a conveyor belt, drying the pulp and removing the dried sheet from the support surface. An example of a casting or sheet forming process is described, for example, in US Pat. No. 5,724,998 for the production of tobacco in the form of molded leaves. During the sheet forming process, particulate plant materials are mixed with a liquid component, usually water, to form a pulp. Other added components in the pulp may include fibers, binder and aerosolizing agent. Particulate plant materials can agglomerate in the presence of a binder. The pulp is poured onto a supporting surface and dried to form a sheet of homogenized plant material.

In certain preferred embodiments, the homogenized plant material used in the articles of the present invention is produced by casting. Homogenized plant material produced through a casting process typically contains agglomerated plant material in particulate form.

During the sheet forming process, since substantially all of the soluble fraction is retained in the plant material, predominantly the majority of the flavor compounds are retained. Additionally, energy-intensive papermaking steps are eliminated.

In one preferred embodiment of the present invention, to form homogenized plant material, a mixture is formed containing particulate plant material, water, a binder and an aerosol forming agent. Both the particulate plant material and the aerosol forming agent are as described above with reference to the first aspect of the present invention. A leaf is formed from the mixture, and then the leaf is dried. Preferably the mixture is an aqueous mixture. As used herein, the term “dry weight” refers to the weight of a particular non-aqueous component relative to the sum of the weights of all non-aqueous components in the mixture, expressed as a percentage. The composition of aqueous mixtures can be considered as "percent dry weight". This refers to the weight of the non-aqueous components relative to the weight of the total aqueous mixture, expressed as a percentage.

The mixture may be a pulp. As used herein, the term "pulp" refers to a homogenized aqueous mixture of relatively low dry weight. The pulp used in the method herein may preferably have a dry weight of from about 5 percent to 60 percent.

Alternatively, the mixture may be a dough-like mass. As used herein, the term “dough mass” refers to an aqueous mixture with a relatively high dry weight. The dough mass used in the method herein may preferably have a dry weight of at least 60 percent, more preferably at least 70 percent.

Suspensions having a dry weight greater than 30 percent and dough-like masses may be preferred in certain embodiments of this method.

The step of mixing the particulate plant material, water and other optional components can be accomplished by any suitable means. For mixtures with low viscosity, i.e. some suspensions, it is preferable that mixing is carried out using a high intensity mixer or a high shear mixer. With this mixing, destruction and uniform distribution of the various phases of the mixture occur. For mixtures with higher viscosity, i.e. some dough-like masses, a kneading process can be used to distribute the different phases of the mixture evenly.

The methods of the present invention may further include the step of vibrating the mixture to distribute the various components. Vibrating the mixture, that is, for example, vibrating a container or intermediate bin in which the homogenized mixture is located, can help homogenize the mixture, in particular when the mixture is a mixture with low viscosity, ie some suspensions. Less mixing time may be required to homogenize the mixture to the target value for optimal casting if vibration is also applied along with mixing.

If the mixture is a pulp, a web of homogenized plant material is preferably formed through a casting process involving casting the pulp onto a support surface, such as a conveyor belt. A method for producing homogenized plant material includes the step of drying said molded web to form a sheet. The molded web can be dried at room temperature or at an ambient temperature of 80 to 160 degrees Celsius for a suitable period of time. Preferably, the moisture content of the sheet after drying is from about 5 percent to about 15 percent, based on the total weight of the sheet. After drying, the sheet can be removed from the supporting surface. The molded sheet has such tensile strength that it can be moved by mechanical means and spooled onto or unwound from a reel without tearing or deformation.

If the mixture is a doughy mass, the doughy mass may be extruded into sheet, thread or strip form before the step of drying the extruded mixture. Preferably, the dough-like mass can be extruded in sheet form. The extruded mixture can be dried at room temperature or at a temperature of 80 to 160 degrees Celsius for a suitable period of time. Preferably, the moisture content of the extruded mixture after drying is from about 5 percent to about 15 percent, based on the total weight of the sheet. A sheet formed from a pasty mass requires less drying time and/or lower drying temperatures due to the substantially lower water content relative to a sheet formed from a pulp.

After drying the sheet, the method may optionally include the step of applying a nicotine salt, preferably together with an aerosol forming agent, to the sheet, as described in the disclosure of document WO-A-2015/082652.

After drying the sheet, the methods of the present invention may optionally include the step of cutting the sheet into threads, pieces or strips to form an aerosol generating substrate, as described above. The threads, pieces or strips can be brought together to form a rod of aerosol generating substrate using a suitable means. In the formed aerosol generating substrate rod, the threads, pieces or strips may be substantially aligned, for example, in the longitudinal direction of the rod. Alternatively, the threads, pieces or strips may be randomly oriented in the rod.

In certain preferred embodiments, the method further includes the step of corrugating the sheet. This may make it easier to gather the sheet to form a rod, as described below. The "corrugation" stage produces a sheet having many folds or corrugations.

In certain preferred embodiments, the method further includes the step of gathering the sheet to form a rod. The term "assembled" means a sheet that is folded, folded, or otherwise compressed or tapered in a direction substantially transverse to the longitudinal axis of the aerosol generating substrate. The step of "gathering" the sheet can be carried out using any suitable means that provides the necessary lateral compression of the sheet.

The methods of the present invention may optionally further include the step of winding the sheet onto a reel after the drying step.

The present invention further provides an alternative papermaking process for producing sheets of homogenized plant material. The method includes a first step of mixing plant material and water to form a dilute suspension. The diluted suspension contains mainly separated cellulose fibers. The slurry has a lower viscosity and higher water content than the slurry produced by the casting process. This first step may involve soaking, optionally in the presence of an alkali such as sodium hydroxide, and optionally applying heat.

The method further includes a second step of separating the suspension into an insoluble portion containing insoluble fibrous plant material and a liquid or aqueous portion containing soluble plant matter. The water remaining in the insoluble fibrous plant material can be drained through a mesh that acts as a sieve, whereby a web of randomly interwoven fibers can be laid down. Water can be further removed from this web by compression by rollers, sometimes by suction or vacuum.

After removing the aqueous part and water, a sheet is formed from the insoluble part. Preferably, a generally flat, uniform sheet of plant fibers is formed.

Preferably, the method further includes the steps of concentrating the soluble plant matter that has been removed from the leaf and adding the concentrated plant matter to a sheet of insoluble fibrous plant material to form a sheet of homogenized plant material. Alternatively or additionally, soluble plant matter or concentrated plant matter from another process may be added to the leaf. The soluble plant matter or concentrated plant matter may be obtained from a different variety of the same plant species, or from other plant species.

This process, as described in US-A-3,860,012, has been used with tobacco to make reconstituted tobacco products, also known as tobacco paper. The same process can also be used with one or more plants to produce a paper-type sheet material, such as a sheet of eucalyptus paper.

In certain preferred embodiments, the homogenized plant material used in the articles of the present invention is obtained through a papermaking process as defined above. Homogenized tobacco material or homogenized eucalyptus material obtained through such a process is called tobacco paper or eucalyptus paper. Homogenized plant material made through the papermaking process can be identified by the presence of many fibers throughout the material, visible to the naked eye or under a light microscope, especially when the paper is wetted with water. In contrast, homogenized plant material made through the casting process contains fewer fibers than paper and tends to dissociate into pulp when it is wetted. Tobacco-eucalyptus blend paper refers to homogenized plant material obtained through such a process using a mixture of tobacco material and eucalyptus material.

In embodiments in which the aerosol-generating substrate contains a combination of eucalyptus particles and tobacco particles, the aerosol-generating substrate may comprise one or more sheets of eucalyptus paper and one or more sheets of tobacco paper. Sheets of eucalyptus and tobacco paper can be arranged alternately with each other or stacked on top of each other before being gathered to form a core. Optionally, the sheets can be corrugated. Alternatively, sheets of eucalyptus and tobacco paper can be cut into threads, strips or pieces and then combined to form a rod. The relative amounts of tobacco and eucalyptus in the aerosol generating substrate can be adjusted by varying the corresponding number of tobacco and eucalyptus sheets or the relative amounts of eucalyptus and tobacco threads, strips or pieces in the rod.

Other known processes that can be used to obtain homogenized plant materials are reconstitution processes of the type described, for example, in US Pat. No. 3,894,544; and extrusion processes of the type described, for example, in document GB-A-983,928. Generally, the densities of homogenized plant materials produced by extrusion processes and reconstitution processes are higher than the densities of homogenized plant materials produced by casting processes.

The aerosol generating articles of the present invention comprise an aerosol generating substrate as described above and may optionally further comprise a mouthpiece. The mouthpiece may include one or more filter segments, which are combined during manufacture of the article. The aerosol generating article may comprise a rod, in turn, containing a substrate in one or more rods. When the rod contains optional filter segments, it may have a rod length of from about 5 mm to about 130 mm. When the rod does not include optional filter segments, it may have a length of from about 5 mm to about 120 mm. The rod may contain one or more aerosol-generating substrate rods. When one rod of the aerosol generating substrate forms a rod, both rod and rod preferably have a length of from about 10 mm to about 40 mm, more preferably from about 10 mm to 15 mm, most preferably about 12 mm. The rods can have a diameter from about 5 mm to about 10 mm depending on their intended purpose.

The aerosol generating products of the present invention also include, but are not limited to, a hookah cartridge or consumable.

The aerosol generating articles of the present invention may optionally comprise at least one hollow tube located immediately downstream of the aerosol generating substrate. One of the functions of the tube is to place the aerosol generating substrate towards the distal end of the aerosol generating article so that it can come into contact with the heating element. The tube is designed to prevent the aerosol generating substrate from moving along the aerosol generating article towards other downstream elements when the heating element is inserted into the aerosol generating substrate. The tube also acts as a separation element to separate downstream elements from the aerosol-generating substrate. The tube can be made of any material such as cellulose acetate, polymer, cardboard or paper.

The aerosol generating articles of the present invention optionally include one or more of a separator or aerosol cooling element downstream of the aerosol generating substrate and immediately downstream of the hollow tube. In use, the aerosol formed by volatile compounds released from the aerosol-generating substrate is passed over and cooled by the aerosol cooling element before being inhaled by the user. The lower temperature allows the vapor to condense to form an aerosol. The separator or aerosol cooling element may be a hollow tube, such as a hollow cellulose acetate tube or cardboard tube, which may be similar to a tube immediately downstream of the aerosol generating substrate. The separator may be a hollow tube that has the same outer diameter but a smaller or larger inner diameter than the hollow cellulose acetate tube. In one embodiment, the paper-wrapped aerosol cooling element comprises one or more longitudinal channels made of any suitable material, such as metal foil, foil laminated paper, polymer sheet, preferably made of a synthetic polymer, and substantially non-porous paper or cardboard. In some embodiments, the paper-wrapped cooling aerosol element may comprise one or more sheets made of a material selected from the group consisting of polyethylene (PE), polypropylene (PP), polyvinyl chloride (PVC), polyethylene terephthalate (PET), polylactic acid (PLA), cellulose acetate (CA) and aluminum foil. Alternatively, the aerosol cooling element may be made of woven or non-woven filaments of a material selected from the group consisting of polyethylene (PE), polypropylene (PP), polyvinyl chloride (PVC), polyethylene terephthalate (PET), polylactic acid (PLA) and cellulose acetate (CA). In a preferred embodiment, the aerosol cooling element is a corrugated and assembled polylactic acid sheet wrapped in filter paper. In another preferred embodiment, the aerosol cooling element comprises a longitudinal channel and is made of woven synthetic polymer filaments, such as polylactic acid filaments, which are wrapped in paper.

The aerosol generating articles of the present invention may further comprise a filter or mouthpiece downstream of the aerosol generating substrate and a hollow acetate tube, separator or aerosol cooling element. The filter may contain one or more filter materials to remove particulate components, gaseous components, or a combination thereof. Suitable filter materials are known in the art and include, but are not limited to: fibrous filter materials such as, for example, cellulose acetate tow and paper; adsorbents such as, for example, activated alumina, zeolites, molecular sieves and silica gel; biodegradable polymers including, for example, polylactic acid (PLA), Mater-Bi®, hydrophobic rayon fibers and bioplastics; and their combinations. The filter may be located at the downstream end of the aerosol generating article. The filter may be a cellulose acetate filter rod. The filter in one embodiment has a length of approximately 7 mm, but can have a length of from about 5 mm to about 10 mm.

In one embodiment, the aerosol generating article has an overall length of approximately 45 mm. The aerosol generating article may have an outer diameter of 7 mm to 8 mm, preferably approximately 7.3 mm.

The aerosol generating articles of the present invention may further comprise one or more aerosol modifying elements. The aerosol modifying element may include an aerosol modifying agent. As used herein, the term aerosol modifying agent is used to describe any agent that, when used, modifies one or more attributes or properties of the aerosol passing through the filter. Suitable aerosol modifying agents include, but are not limited to, agents that, when used, impart a flavor or aroma to the aerosol passing through the filter.

The aerosol modifying agent may be one or more of a moisture or a liquid flavoring agent. Water or moisture may modify the sensation experienced by the user, for example, by wetting the generated aerosol, which may have a cooling effect on the aerosol and may reduce the perceived astringency experienced by the user. The aerosol modifying element may be in the form of a flavor delivery element for delivering one or more liquid flavoring agents.

The one or more liquid flavoring agents may contain any flavoring compound or plant extract suitable for release in liquid form in a flavoring element to improve the flavor of the aerosol produced during use of the aerosol generating article. Flavoring agents, liquid or solid, may also be located directly in the material that forms the filter, such as cellulose acetate tow. Suitable flavoring agents or aroma agents include, but are not limited to, menthol, mints such as peppermint and spearmint, chocolate, licorice, citrus and other fruit flavoring agents, gamma-octalactone, vanillin, ethyl vanillin, flavoring agents for fresh breath, spicy flavoring agents such as cinnamon, methyl salicylate, linalool, eugenol, bergamot oil, geranium oil, lemon oil, hemp oil and tobacco flavoring agent. Other suitable flavoring agents may include flavoring compounds selected from the group consisting of acid, alcohol, ester, aldehyde, ketone, pyrazine, combinations or mixtures thereof, and the like.

One or more aerosol modifying elements may be located downstream of the aerosol generating substrate or within the aerosol generating substrate. The aerosol generating substrate may comprise homogenized plant material and an aerosol modifying element. In various embodiments, the aerosol modifying element may be located adjacent to or incorporated into the homogenized plant material. Typically, the aerosol modifying elements may be located downstream of the aerosol generating substrate, most commonly within the aerosol cooling element, within the filter of the aerosol generating article, for example, within a filter rod or within a cavity between the filter rods. The one or more aerosol modifying elements may be in the form of one or more of a filament, capsule, microcapsule, bead or polymer matrix material, or a combination thereof.

If the aerosol modifying element is in the form of a thread, as described in WO-A-2011/060961, the thread may be formed from paper such as filter ficella, and the thread may be filled with at least one aerosol modifying agent, and located inside the main part of the filter. Other materials that can be used to form the thread include cellulose acetate and cotton.

If the aerosol modifying element is in the form of a capsule, as described in WO-A-2007/010407, WO-A-2013/068100 and WO-A-2014/154887, the capsule may be a frangible capsule located inside the filter, wherein the inner core of the capsule contains an aerosol modifying agent that can be released upon destruction of the outer shell of the capsule when the filter is subjected to external force. The capsule can be located inside the filter rod or inside the cavity between the filter rods.

If the aerosol modifying element is in the form of a polymer matrix material, the polymer matrix material releases the flavor additive when the aerosol generating article is heated, for example, when the polymer matrix is heated above the melting point of the polymer matrix material, as described in WO-A-2013/034488 . Typically, such a polymer matrix material may be located within a bead within an aerosol-generating substrate. Alternatively or additionally, the flavor additive may be contained within domains of the polymer matrix material and may be released from the polymer matrix material upon compression of the polymer matrix material. Such flavor modifying elements may provide sustained release of the liquid flavor over a force range of at least 5 Newtons, for example 5 N to 20 N, as described in WO2013/068304. Typically, such a polymer matrix material may be located within a ball within the filter.

The aerosol generating article may comprise a combustible heat source and an aerosol generating substrate located downstream of the combustible heat source, the aerosol generating substrate being as described above with respect to the first aspect of the present invention.

For example, the substrates described herein can be used in the types of heated aerosol-generating articles described in WO-A-2009/022232, which contain a combustible carbon-based heat source, the aerosol-generating substrate located downstream relative to a combustible heat source, and a thermal conductive element surrounding and in contact with a rear portion of the carbon-based combustible heat source and an adjacent front portion of the aerosol generating substrate. However, it should be understood that the substrates described herein may also be used in heated aerosol generating articles containing combustible heat sources of other designs.

The present invention provides an aerosol generating system that includes an aerosol generating device that includes a heating element, and an aerosol generating article for use with the aerosol generating device, wherein the aerosol generating article contains an aerosol generating substrate as described above .

In a preferred embodiment, the aerosol generating substrates described herein can be used in heated aerosol generating articles for use in electrical aerosol generating systems in which the aerosol generating substrate of the heated aerosol generating article is heated by an electrical source heat.

For example, the aerosol generating substrates described herein can be used in heated aerosol generating articles of the type described in EP-A-0 822 760.

The heating element of such aerosol generating devices may be of any suitable shape for conducting heat. Heating of the aerosol-generating substrate can be achieved from the inside, the outside, or both. The heating element may preferably be a heating plate or pin adapted to be inserted into the substrate, thereby heating the substrate internally. Alternatively, the heating element may partially or completely surround the substrate and heat the substrate circumferentially from the outside.

The aerosol generating system may be an electrical aerosol generating system comprising an induction heating device. Induction heating devices typically include an induction source configured to be connected to a current collector. The induction source generates an alternating electromagnetic field, which induces magnetization or eddy currents in the pantograph. The pantograph may become hot as a result of hysteresis losses or induced eddy currents that heat the pantograph through ohmic or resistive heating.

Electrical aerosol generating systems that include an induction heating device may also include an aerosol generating article that contains an aerosol generating substrate and a current collector in thermal proximity to the aerosol generating substrate. Typically, the pantograph is in direct contact with the aerosol-generating substrate, and heat is transferred from the pantograph to the aerosol-generating substrate primarily by conduction. Examples of electrical aerosol generating systems containing induction heating devices and aerosol generating products containing current collectors are described in WO-A1-95/27411 and WO-A1-2015/177255.

The susceptor may be a plurality of susceptor particles that may be deposited on or embedded in the aerosol-generating substrate. When the aerosol generating substrate is in the form of one or more sheets, a plurality of current collecting particles may be deposited on or contained within the one or more sheets. The current-receiving particles are immobilized by the substrate, for example in the form of a sheet, and remain in their original position. Preferably, the susceptor particles may be uniformly distributed in the homogenized plant material of the aerosol-generating substrate. Due to the fact that the susceptor is in the form of particles, heat is produced according to the distribution of particles in the sheet of homogenized plant substrate material. Alternatively, a susceptor in the form of one or more sheets, strips, pieces or rods may also be positioned adjacent to or embedded within the homogenized plant material. In one embodiment, the aerosol-forming substrate comprises one or more current collection strips. In another embodiment, the pantograph is located in the aerosol generating device.

The current collector may have a heat loss of more than 0.05 J/kg, preferably a heat loss of more than 0.1 J/kg. Heat loss is the ability of a pantograph to transfer heat to the surrounding material. Since the susceptor particles are preferably uniformly distributed in the aerosol-generating substrate, uniform heat loss from the susceptor particles can be achieved, which ensures uniform heat distribution in the aerosol-generating substrate and results in uniform temperature distribution in the aerosol-generating article. It has been found that a specific minimum heat loss of 0.05 J/kg in the current collector particles allows the aerosol generating substrate to be heated to a substantially uniform temperature allowing aerosol generation. Preferably, the average temperatures achieved within the aerosol generating substrate in such embodiments are from about 200 degrees Celsius to about 240 degrees Celsius.

Reducing the risk of overheating of the aerosol-generating substrate can be supported by the use of current collector materials having a Curie temperature, which ensures the heating process due to hysteresis losses only up to a certain maximum temperature. The current collector may have a Curie temperature of from about 200 degrees Celsius to about 450 degrees Celsius, preferably from about 240 degrees Celsius to about 400 degrees Celsius, such as about 280 degrees Celsius. When the susceptor material reaches its Curie temperature, the magnetic properties change. At the Curie temperature, the current collector material transitions from the ferromagnetic phase to the paramagnetic phase. At this point, heating, based on energy losses due to the orientation of the ferromagnetic domains, stops. Further heating is then mainly based on the formation of eddy current, so that the heating process is automatically reduced when the Curie temperature of the current collector material is reached. Preferably, the receiver material and its Curie temperature are tailored to the composition of the aerosol generating substrate to achieve optimal temperatures and temperature distribution in the aerosol generating substrate for optimal aerosol generation.

In some preferred embodiments, the aerosol generating article of the present invention is made of ferrite. Ferrite is a ferromagnetic material with high magnetic permeability and is particularly suitable as a current collector material. The main component of ferrite is iron. Other metallic components, such as zinc, nickel, manganese, or non-metallic components, such as silicon, may be present in varying amounts. Ferrite is a relatively inexpensive material available on the market. Ferrite is available in particle form in the particle size ranges used in the particulate plant material forming the homogenized plant material of the present invention. Preferably the particles are fully sintered ferrite powder, such as FP160, FP215, FP350, available from PPT, Indiana, USA.

In certain embodiments of the present invention, an aerosol generating system comprises an aerosol generating article that contains an aerosol generating substrate as defined above, a source of aerosol generating agent, and a means for vaporizing the aerosol generating agent, preferably a heating element, as described above. The source of the aerosol generating agent may be a reservoir, which may be refillable or replaceable, located on the aerosol generating device. Although the reservoir is physically separate from the aerosol generating article, the generated vapor is directed through the aerosol generating article. The steam comes into contact with an aerosol-generating substrate, which releases volatile compounds such as nicotine and flavoring agents in the particulate plant material to form an aerosol. Optionally, to avoid vaporization of compounds in the aerosol-generating substrate, the aerosol-generating system may further comprise a heating element for heating the aerosol-generating substrate, preferably in a manner coordinated with the aerosol-generating substance. However, in certain embodiments, the heating element used to heat the aerosol-generating article is separate from the heater that heats the aerosol-generating substance.

As defined above, the present invention further provides an aerosol produced by heating an aerosol generating substrate, the aerosol comprising specific amounts and ratios of characteristic compounds derived from eucalyptus particles as defined above.

According to the present invention, the aerosol contains eucalyptol in an amount of at least 0.2 micrograms per puff of the aerosol; eucalyptin in an amount of at least 0.2 micrograms per puff of aerosol; and 8-desmethyleucalyptin in an amount of at least 0.2 micrograms per puff of aerosol. For purposes of the present invention, a "puff" is defined as the volume of aerosol released from the aerosol-generating substrate when heated and collected for analysis, the aerosol puff having a puff volume of 55 milliliters generated by the smoking machine. Accordingly, any reference to a “puff” of an aerosol should be understood to mean a 55-milliliter puff unless otherwise noted.

The ranges shown indicate the total amount of each component measured in a 55-milliliter puff of aerosol. An aerosol can be generated from an aerosol-generating substrate using any suitable means and can be captured and analyzed as described above to identify characteristic compounds in the aerosol and measure their quantities. For example, “puff” may correspond to a 55 milliliter puff taken on a smoking machine, such as the machine used in the Health Canada approved test method described herein.

Preferably, the aerosol of the present invention contains at least about 0.5 micrograms of eucalyptol per aerosol puff, more preferably at least about 2 micrograms of eucalyptol per aerosol puff, more preferably at least about 5 micrograms of eucalyptol per aerosol puff. Alternatively or additionally, the aerosol generated from the aerosol generating substrate contains up to about 25 micrograms of eucalyptol per aerosol puff, preferably up to about 15 micrograms of eucalyptol per aerosol puff, and more preferably up to about 10 micrograms of eucalyptol per aerosol puff. For example, an aerosol generated from an aerosol generating substrate may contain from about 0.5 micrograms to about 25 micrograms of eucalyptol per puff of aerosol, or from about 2 micrograms to about 15 micrograms of eucalyptol per puff of aerosol, or from about 5 micrograms to about 10 microgram of eucalyptol per puff of aerosol.

Preferably, the aerosol of the present invention contains at least about 0.5 micrograms of eucalyptin per aerosol puff, more preferably at least about 2 micrograms of eucalyptin per aerosol puff, more preferably at least about 5 micrograms of eucalyptin per aerosol puff. Alternatively or additionally, the aerosol generated from the aerosol generating substrate contains up to about 25 micrograms of eucalyptin per aerosol puff, preferably up to about 15 micrograms of eucalyptin per aerosol puff, and more preferably up to about 10 micrograms of eucalyptin per aerosol puff. For example, an aerosol generated from an aerosol generating substrate may contain from about 0.2 micrograms to about 25 micrograms of eucalyptin per aerosol puff, or from about 0.5 micrograms of eucalyptin per aerosol puff to about 25 micrograms of eucalyptin per aerosol puff, or from approximately 2 micrograms to approximately 15 micrograms of eucalyptin per puff of aerosol, or approximately 5 micrograms to approximately 10 micrograms of eucalyptin per puff of aerosol.

Preferably, the aerosol of the present invention contains at least about 0.5 micrograms of 8-desmethyleucalyptin per puff of aerosol, more preferably at least about 2 micrograms of 8-desmethyleucalyptin per puff of aerosol, more preferably at least about 5 micrograms of 8-desmethyleucalyptin per puff of aerosol . Alternatively or additionally, the aerosol generated from the aerosol generating substrate contains up to about 25 micrograms of 8-desmethyleucalyptin per aerosol puff, preferably up to about 15 micrograms of 8-desmethyleucalyptin per aerosol puff, and more preferably up to about 10 micrograms of 8-desmethyleucalyptin per aerosol puff. For example, an aerosol generated from an aerosol generating substrate may contain from about 0.2 micrograms to about 25 micrograms of 8-desmethyleucalyptin per puff of aerosol, or from about 0.5 micrograms to about 25 micrograms of 8-desmethyleucalyptin per puff of aerosol, or from approximately 2 micrograms to approximately 15 micrograms of 8-desmethyleucalyptin per puff of aerosol, or approximately 5 micrograms to approximately 10 micrograms of 8-desmethyleucalyptin per puff of aerosol.

According to the present invention, the aerosol composition is such that the amount of eucalyptol per puff is no more than twice the amount of eucalyptin per puff. Therefore, the ratio of eucalyptol to eucalyptin in the aerosol is no more than 2:1.

Preferably, the amount of eucalyptol per puff of aerosol is no more than 1.5 times the amount of eucalyptin per puff of aerosol, resulting in a ratio of eucalyptol to eucalyptin in the aerosol of no more than 1.5:1. More preferably, the amount of eucalyptol per puff of aerosol is no more than 1.2 times the amount of eucalyptin per puff of aerosol, resulting in a ratio of eucalyptol to eucalyptin in the aerosol of no more than 1.2:1. More preferably, the amount of eucalyptol per puff of aerosol is less than or equal to the amount of eucalyptol per puff of aerosol, resulting in a ratio of eucalyptol to eucalyptin in the aerosol of no more than 1:1.

According to the present invention, the composition of the aerosol is such that the amount of eucalyptol per puff of the aerosol is no more than twice the amount of 8-desmethyleucalyptin per puff of the aerosol. Therefore, the ratio of eucalyptol to 8-desmethyleucalyptin in the aerosol is no more than 2:1.

Preferably, the amount of eucalyptol per puff of aerosol is no more than 1.5 times the amount of 8-desmethyleucalyptin per puff of aerosol, resulting in a ratio of eucalyptol to 8-desmethyleucalyptin in the aerosol of no more than 1.5:1. More preferably, the amount of eucalyptol per puff of aerosol is no more than 1.2 times the amount of eucalyptol per puff of aerosol, resulting in a ratio of eucalyptol to 8-desmethyleucalyptin in the aerosol of no more than 1.2:1. More preferably, the amount of eucalyptol per puff of aerosol is less than or equal to the amount of 8-desmethyleucalyptin per puff of aerosol, resulting in a ratio of eucalyptol to 8-desmethyleucalyptin in the aerosol of no more than 1:1.

Preferably, the ratio of eucalyptin to 8-desmethyleucalyptin in the aerosol is from about 1.2:1 to 1:1.

Certain ratios of eucalyptol to eucalyptin and 8-desmethyleucalyptin characterize the aerosol that is obtained from eucalyptus particles. In contrast, in an aerosol derived from eucalyptus oil, the ratio of eucalyptol to eucalyptin and the ratio of eucalyptol to 8-desmethyleucalyptin to eucalyptol will be significantly greater than 2:1. This is due to the relatively high proportion of eucalyptol in eucalyptus oil compared to eucalyptus plant material.

Preferably, the ratio of eucalyptin to eucalyptol in the aerosol of the present invention is at least about 1:1. This means that the amount of eucalyptin in the aerosol is at least the same as the amount of eucalyptol, and preferably more. Alternatively or in addition, the ratio of 8-desmethyleucalyptin to eucalyptol in the aerosol is at least 1:1. This means that the amount of 8-desmethyleucalyptin in the aerosol is at least the same as the amount of eucalyptol, and preferably more. These ratios are typical for aerosol obtained from eucalyptus particles. In an aerosol derived from eucalyptus oil, the ratio of eucalyptin to eucalyptol and the ratio of 8-desmethyleucalyptin to eucalyptol will be significantly less than 1. This is due to the relatively high proportion of eucalyptol in eucalyptus oil compared to eucalyptus plant material.

Preferably, the aerosol of the present invention further comprises at least about 0.1 milligrams of aerosol agent per puff of aerosol, more preferably at least about 0.2 milligrams of aerosol agent per puff of aerosol, and more preferably at least about 0.3 milligrams of aerosol agent per puff of aerosol. aerosol formation by inhaling the aerosol. Preferably, the aerosol contains up to 0.6 milligrams of an aerosol-forming agent per puff of an aerosol, more preferably up to 0.5 milligrams of an aerosol-forming agent per puff of an aerosol, more preferably up to 0.4 milligrams of an aerosol-forming agent per puff of an aerosol. For example, an aerosol may contain from about 0.1 milligram to about 0.6 milligram of aerosolizing agent per puff of aerosol, or from about 0.2 milligrams to about 0.5 milligrams of aerosolizing agent per puff of aerosol, or from about 0. 3 milligrams to approximately 0.4 milligrams of aerosol-forming agent per puff of aerosol. These values are based on a puff volume of 55 milliliters as defined above.

Aerosol-forming agents suitable for use in the present invention are presented above.

Preferably, the aerosol derived from the aerosol generating substrate of the present invention further contains at least about 2 micrograms of nicotine per puff of aerosol, more preferably at least about 20 micrograms of nicotine per puff of aerosol, more preferably at least about 40 micrograms of nicotine per puff of aerosol aerosol. Preferably, the aerosol contains up to about 200 micrograms of nicotine per puff of aerosol, more preferably up to about 150 micrograms of nicotine per puff of aerosol, more preferably up to about 75 micrograms of nicotine per puff of aerosol. For example, an aerosol may contain from about 2 micrograms to about 200 micrograms of nicotine per puff of aerosol, or from about 20 micrograms to about 150 micrograms of nicotine per puff of aerosol, or from about 40 micrograms to about 75 micrograms of nicotine per puff of aerosol. These values are based on a puff volume of 55 milliliters as defined above. In some embodiments of the present invention, the aerosol may contain zero micrograms of nicotine.

Alternatively or additionally, the aerosol of the present invention may optionally further contain at least about 0.5 milligrams of a cannabinoid compound per aerosol puff, more preferably at least about 1 milligram of a cannabinoid compound per aerosol puff, more preferably at least about 2 milligrams of a cannabinoid compound per aerosol puff. puff of aerosol. Preferably, the aerosol contains up to about 5 milligrams of a cannabinoid compound per aerosol puff, more preferably up to about 4 milligrams of a cannabinoid compound per aerosol puff, more preferably up to about 3 milligrams of a cannabinoid compound per aerosol puff. For example, an aerosol may contain from about 0.5 milligrams to about 5 milligrams of a cannabinoid compound per puff of an aerosol, or from about 1 milligram to about 4 milligrams of a cannabinoid compound per puff of an aerosol, or from about 2 milligrams to about 3 milligrams of a cannabinoid compound per puff of an aerosol. In some embodiments of the present invention, the aerosol may contain zero micrograms of a cannabinoid compound. These values are based on a puff volume of 55 milliliters as defined above.

Preferably the cannabinoid compound is selected from CBD and THC. More preferably, the cannabinoid compound is CBD.

Carbon monoxide may also be present in the aerosol of the present invention and can be measured and used to further characterize the aerosol. Oxides of nitrogen, such as nitric oxide and nitrogen dioxide, may also be present in the aerosol and can be measured and used to further characterize the aerosol.

The aerosol of the present invention containing characteristic eucalyptus particle compounds may be formed from particles having a mass median aerodynamic diameter (MMAD) in the range of from about 0.01 to 200 microns or from about 1 to 100 microns. Preferably, if the aerosol contains nicotine, as described above, the aerosol contains particles having an MMAD in the range of about 0.1 to about 3 microns to optimize delivery of nicotine from the aerosol.

The mass median aerodynamic diameter (MMAD) of an aerosol refers to the aerodynamic diameter at which half the mass of the aerosol particles is composed of particles with an aerodynamic diameter that is greater than the MMAD, and half is composed of particles with an aerodynamic diameter that is less than the MMAD. Aerodynamic diameter is defined as the diameter of a spherical particle with a density of 1 g/cm ³ that has the same settling velocity as the particle being characterized.

The mass median aerodynamic diameter of the aerosol according to the present invention can be determined in accordance with section 2.8 of Schaller et al., “Evaluation of the Tobacco Heating System 2.2. Part 2: Chemical composition, genotoxicity, cytotoxicity and physical properties of the aerosol,” Regul. Toxicol. and Pharmacol., 81 (2016) S27-S47.

Specific embodiments will now be described, by way of example only, with reference to the accompanying drawings, in which:

in fig. 1 depicts a first embodiment of an aerosol generating article substrate as described herein;

in fig. 2 illustrates an aerosol generating system that includes an aerosol generating article and an aerosol generating device that includes an electrical heating element;

in fig. 3 illustrates an aerosol generating system that includes an aerosol generating article and an aerosol generating device that includes a combustible heating element;

in fig. 4a and 4b depict a second embodiment of an aerosol generating article substrate as described herein;

in fig. 5 depicts a third embodiment of an aerosol generating article substrate as described herein;

in fig. 6 is a cross-sectional view of a filter 1050 further comprising an aerosol modifying element, wherein

in fig. 6a shows an aerosol modifying element in the form of a spherical capsule or ball inside the filter rod.

In fig. 6b shows an aerosol modifying element in the form of a thread inside the filter rod.

In fig. 6c shows an aerosol modifying element in the form of a spherical capsule inside a cavity in the filter;

in fig. 7 is a cross-sectional view of the rod of the aerosol generating substrate 1020, which further includes an aerosol modifying element in the form of a ball; And

in fig. 8 shows an experimental setup for collecting aerosol samples to be analyzed in order to measure representative compounds.

In fig. 1 depicts a heated aerosol generating article 1000 that contains a substrate as described herein. Product 1000 contains four elements; an aerosol generating substrate 1020, a hollow cellulose acetate tube 1030, a separating element 1040, and a mouthpiece filter 1050. These four elements are arranged in series, aligned on the same axis, and combined with cigarette paper 1060 to form the aerosol generating article 1000. The article 1000 has a mouth end 1012 that the user inserts into his or her mouth during use, and a distal end 1013 located at the opposite end of the article from the mouth end 1012. An embodiment of the aerosol generating article shown in FIG. 1 is particularly suitable for use with an electrical aerosol generating device comprising a heater for heating the aerosol generating substrate.

When assembled, the 1000 has a length of approximately 45 millimeters, an outer diameter of approximately 7.2 millimeters, and an inner diameter of approximately 6.9 millimeters.

The aerosol generating substrate 1020 includes a rod formed from a sheet of homogenized plant material containing eucalyptus particles either alone or in combination with tobacco particles. Several examples of homogenized plant material suitable for forming the aerosol generating substrate 1020 are shown in Table 1 below (see Samples A-D). The sheet is assembled, corrugated and wrapped in filter paper (not shown) to form a strand. The leaf contains additives, including glycerol, as an aerosol-forming agent.

The aerosol generating article 1000 shown in FIG. 1 is configured to engage with an aerosol generating device for consumption. Such an aerosol generating device includes means for heating the aerosol generating substrate 1020 to a temperature sufficient to generate an aerosol. Typically, the aerosol generating device may include a heating element that surrounds the aerosol generating article 1000 in proximity to the aerosol generating substrate 1020, or a heating element that is inserted into the aerosol generating substrate 1020.

Once engaged with the aerosol generating device, the user takes a puff from the mouth end 1012 of the smoking article 1000 and the aerosol generating substrate 1020 is heated to a temperature of approximately 375 degrees Celsius. At this temperature, volatile compounds are released from the aerosol generating substrate 1020. These compounds condense to form an aerosol. The aerosol is drawn through the 1050 filter and into the user's mouth.

In fig. 2 illustrates a portion of an electrical aerosol generating system 2000 that uses a heating plate 2100 to heat an aerosol generating substrate 1020, an aerosol generating article 1000. The heating plate is installed inside the aerosol generating article housing chamber of the aerosol generating electrical device 2010. The aerosol generating device defines a plurality of air holes 2050 to allow air to flow to the aerosol generating article 1000. The air flow is indicated by arrows in Fig. 2. The aerosol generating device contains a power supply and an electronic circuit, which are shown in FIG. 2 are not shown. The aerosol generating article 1000 shown in FIG. 2, similar to that shown in FIG. 1.

In an alternative configuration shown in FIG. 3, the aerosol generating system is shown with a combustible heating element. Although it is assumed that the product 1000 shown in FIG. 1 is used in conjunction with the aerosol generating device 1001 shown in FIG. 3, contains a combustible heat source 1080 that can be ignited and can transfer heat to the aerosol generating substrate 1020 to generate a respirable aerosol. The combustible heat source 80 is a carbon element that is positioned adjacent to the aerosol generating substrate at the distal end 13 of the rod 11. The elements, which are substantially the same as those shown in FIG. 1 are designated by the same numbers.

In fig. 4a and 4b depict a second embodiment of a heated aerosol generating article 4000a, 4000b. The aerosol generating substrate 4020a, 4020b includes a first downstream rod 4021 formed from particulate plant material comprising primarily eucalyptus particles and a second upstream rod 4022 formed from particulate plant material. containing mainly tobacco particles. Homogenized plant material suitable for use in the first downstream extension is shown in Table 1 below as Sample A. Homogenized plant material suitable for use in the second upstream extension is shown in Table 1 below as Sample E.

In each of the extensions, the homogenized plant material is presented in the form of sheets that are corrugated and wrapped in filter paper (not shown). Both sheets contain additives, including glycerol, as an aerosol-forming agent. In the embodiment shown in FIG. 4a, the rods are combined end-to-end to form a rod and are each of equal length approximately 6 mm. In a more preferred embodiment (not shown), the second rod is preferably longer than the first rod, for example preferably 2 mm longer, more preferably 3 mm longer, whereby the second rod is 7 or 7.5 mm long and the first rod has a length of 5 or 4.5 mm, to ensure the desired ratio of eucalyptus particles in the substrate. In fig. 4b, the support member 1030 for the cellulose acetate tube is not shown.

An article 4000a, 4000b similar to the article 1000 shown in FIG. 1 is particularly suitable for use with an electrical aerosol generating system 2000 that includes the heater shown in FIG. 2. Elements that are substantially the same as those shown in FIG. 1 are designated by the same numbers. One skilled in the art would appreciate that a combustible heat source (not shown) could instead be used with the second embodiment in place of the electrical heating element in a configuration similar to the configuration containing the combustible heat source 1080 in the product 1001 shown in FIG. 3.

In fig. 5 depicts a third embodiment of a heated aerosol generating article 5000. The aerosol generating substrate 5020 includes a rod formed from a first sheet of homogenized plant material formed from particulate plant material containing primarily eucalyptus particles and a second sheet of homogenized plant material containing primarily molded leaf tobacco. Homogenized plant material suitable for use as the first sheet is shown in Table 1 below as Sample A. Homogenized plant material suitable for use as the second sheet is shown in Table 1 below as Sample E.

A second sheet overlaps the first sheet, and the combined sheets are corrugated, gathered, and at least partially wrapped with filter paper (not shown) to form a rod, which is a portion of the rod. Both sheets contain additives, including glycerol, as an aerosol-forming agent. An article 5000 similar to the article 1000 shown in FIG. 1 is particularly suitable for use with an electrical aerosol generating system 2000 that includes the heater shown in FIG. 2. Elements that are substantially the same as those shown in FIG. 1 are designated by the same numbers. One skilled in the art would appreciate that a combustible heat source (not shown) could instead be used with the third embodiment in place of the electric heating element in a configuration similar to the configuration containing the combustible heat source 1080 in the product 1001 depicted in FIG. 3.

In fig. 6 is a cross-sectional view of filter 1050 further comprising an aerosol modifying element. In fig. 6a, filter 1050 further includes an aerosol modifying element in the form of a spherical capsule or bead 605.

In the embodiment shown in FIG. 6a, capsule or bead 605 is inserted into filter segment 601 and surrounded on all sides by filter material 603. In this embodiment, the capsule includes an outer shell and an inner center portion, and the inner center portion contains liquid flavor. A liquid flavoring agent is intended to impart flavor to an aerosol during use of an aerosol-generating product equipped with a filter. Capsule 605 releases at least a portion of the liquid flavor when the filter is subjected to external force, such as by squeezing by a consumer. In the embodiment shown, the capsule is generally spherical, with a substantially continuous outer shell containing liquid flavor.

In the embodiment shown in FIG. 6b, the filter segment 601 includes a filter media rod 603 and a central flavor transfer thread 607 that extends axially through the filter media rod 603 parallel to the longitudinal axis of the filter 1050. The central flavor transfer thread 607 has a substantially the same length as the filter media rod 603 so that the ends of the central flavor transfer thread 607 are visible at the ends of the filter segment 601. In FIG. 6b, the filter material 603 is cellulose acetate tow. The central flavor transfer thread 607 is formed from a twisted filter ficell and filled with an aerosol modifying agent.

In the embodiment shown in FIG. 6c, the filter segment 601 contains more than one filter media 603, 603'. Preferably, the filter material rods 603, 603' are formed from cellulose acetate, whereby they can filter the aerosol provided by the aerosol generating article. The wrap 609 is wrapped around the filter rods 603, 603' and connects them. Located within cavity 611 is a capsule 605 comprising an outer shell and an inner center portion, and the inner center portion contains a liquid flavoring agent. The rest of the capsule is similar to the embodiment shown in FIG. 6a.

In fig. 7 is a cross-sectional view of an aerosol generating substrate 1020, which further includes an aerosol modifying element in the form of a ball 705. The aerosol generating substrate 1020 includes a rod 703 formed from a sheet of homogenized plant material containing tobacco particles and eucalyptus particles. The flavor delivery material in the 705 bead contains a flavor additive that is released when the material is heated above 220 degrees Celsius. The flavoring agent is thus released into an aerosol when part of the rod is heated during use.

Example

Various samples of homogenized plant material for use in the aerosol generating substrate of the present invention, as described above with reference to the figures, were prepared from aqueous slurries having the compositions shown in Table 1. Samples A-D contain eucalyptus particles in accordance with the present invention. Sample E contains only tobacco particles and is included for comparison purposes only.

Particulate plant material in all samples constituted 75 percent of the dry weight of the homogenized plant material, with glycerol, guar gum, and cellulose fibers comprising the remaining 25 percent of the dry weight of the homogenized plant material. In the table below, % DWB stands for "dry weight basis", in this case percentage by weight calculated relative to the dry weight of the homogenized plant material. Eucalyptus powder was formed from the leaves of Eucalyptus globulus , which were first crushed by impact grinding to D95=300 microns, and further ground to a final D95=174.6 microns by triple impact grinding.

Table 1. Dry matter content in pulps, extruder weight and grammage of molded sheet

Sample Eucalyptus powder
(%DWB) Tobacco
(%DWB) Glycerol
(%DWB) Guar Gum (% DWB) Cellulose fibers
(%DWB) Rod weight 12 mm (mg/
product) Grammage (g to m ² ) A 75 0 18 3 4 233 194 B 15 60 18 3 4 280 204 C 7.5 67.5 18 3 4 303 195 D 2.5 72.5 18 3 4 320 203 E 0 75 18 3 4 Indefined Indefined

The pulps were molded using a molding bar (0.6 mm) on a glass plate, dried in an oven at 140 degrees Celsius for 7 minutes, and then dried in a second oven at 120 degrees Celsius for 30 seconds.

For each of the homogenized plant material samples AE, the rods were prepared from one continuous sheet of homogenized plant material, each sheet having a width of from 100 mm to 125 mm. The individual sheets had a thickness of approximately 220 microns and a grammage of approximately 200 g/m ² _. The cutting width of each sheet was adapted based on the thickness of each sheet to produce rods of comparable volume. The sheets were corrugated to a height of 165 microns to 170 microns and rolled into rods having a length of approximately 12 mm and diameters of approximately 7 mm, wrapped in paper wrapper.

For each of the rods, an aerosol generating article was manufactured having an overall length of approximately 45 mm and having the design shown in FIG. 3, which comprises from the downstream end: a cellulose acetate filter (approximately 7 mm long) at the mouth end, an aerosol separator containing a corrugated sheet of polylactic acid polymer (approximately 18 mm long), a hollow acetate tube ( approximately 8 mm long) and an aerosol-generating substrate rod.

For homogenized plant material sample A, in which eucalyptus particles constituted 100 percent particulate plant material, representative compounds were extracted from the homogenized plant material strand using methanol as detailed above. The extract was analyzed as described above to confirm the presence of characteristic compounds and measure the amounts of characteristic compounds. The results of this analysis are shown below in Table 2, in which the amounts indicated correspond to the amount per aerosol generating article, wherein the aerosol generating article substrate of the aerosol generating article contained 233 mg of sample A of the homogenized plant material. For comparative purposes, the quantities of the representative compound present in the particulate plant material (eucalyptus particles) used to prepare sample A are also shown.

Table 2. Quantities of eucalyptus-specific compounds in particulate plant material and aerosol-generating substrate

Characteristic connection Amount in particulate plant material
(micrograms per product) Quantity
(micrograms per product) Eucalyptus 1847.83 1463.42 8-Desmethyleucalyptin 2077.22 1659.33 Eucalyptol 953.28 287.68

For each of samples B-D containing a proportion of eucalyptus particles, the amount of representative compounds can be estimated from the values in Table 2, assuming that the amount is present in proportion to the weight of the eucalyptus particles.

Basic aerosol streams of aerosol-generating articles containing aerosol-generating substrates formed from samples A-E of homogenized plant material were generated in accordance with Test Method A as defined above. For each sample, the aerosol that was collected was captured and analyzed.

As described in detail above, in Test Method A, aerosol generating products were tested using a commercially available iQOS® Non-Combustion Heating System Tobacco Heating System 2.2 Holder (THS2.2 Holder) from Philip Morris Products SA. The aerosol-generating products were heated according to a Health Canada approved machine smoking schedule for 30 puffs with a puff volume of 55 mL, a puff duration of 2 seconds, and a puff interval of 30 seconds (as described in ISO/TR 19478-1:2014).

The aerosol generated during the smoking test was collected on a Cambridge filter pad and extracted using a liquid solvent. In fig. 10 shows a device suitable for generating and collecting aerosol from aerosol generating articles.

The aerosol generating device 111 shown in FIG. 10 is a commercially available tobacco heating device (IQOS). The contents of the main stream of aerosol generated during the Health Canada approved smoking test, as detailed above, were collected in the aerosol collection chamber 113 on the aerosol collection line 120. The 140 glass fiber filter pad is a 44mm Cambridge fiberglass filter pad (CFP) in accordance with ISO 4387 and ISO 3308 standards.

For LC-HRAM-MS analysis:

Extraction solution 170, 170a, which in this case is methanol and internal standard solution (ISTD), is present in a volume of 10 ml in each microimpinger 160, 160a. Each of the cold baths 161, 161a contains a mixture of dry ice and isopropyl ether to maintain each of the microimpingers 160, 160a at a temperature of approximately -60°C. The vapor-gas phase is captured in the extraction solution 170, 170a when the aerosol passes in the form of bubbles through microimpingers 160, 160a. The combined solutions from the two microimpingers are separated as vapor-gas phase solution 180 captured in the impinger at step 181.

The CFP and impinger vapor phase solution 180 are combined in a clean Pyrex® tube at step 190. At step 200, all particulate material is extracted from the CFP using the impinger vapor phase solution 180 (which contains methanol as a solvent) by vigorous shaking (with CFP disintegration), vigorous stirring for 5 minutes and finally centrifugation (4500 g, 5 minutes, 10ºC). Aliquots (300 μL) of the reconstituted whole aerosol extract 220 were transferred to a silanized chromatography vial and diluted with methanol (700 μL) since the extraction solution 170, 170a already contained an internal standard solution (ISTD). The vials were capped and the contents were mixed for 5 minutes using an Eppendorf thermomixer (5°C; 2000 rpm).

Aliquots (1.5 μL) of diluted extracts were injected and analyzed by LC-HRAM-MS in both full scan and fragmentation modes, depending on the data, to identify compounds.

For GCxGC-TOFMS analysis:

As described above, when samples are obtained for GCxGC-TOFMS experiments, various solvents are suitable for the extraction and analysis of polar compounds, non-polar compounds and volatile compounds isolated from the total aerosol. The experimental setup is identical to that described for sample collection for the LC-HRAM-MS method, except as noted below.

Non-polar and polar components

Extraction solution 171,171a is present in a volume of 10 ml and is an 80:20 v/v mixture of dichloromethane and methanol, also containing retention index marker (RIM) compounds and a stable isotopically labeled internal standard (ISTD). Each of the cold baths 162, 162a contains a mixture of dry ice and isopropanol to maintain each of the microimpinger 160, 160a at a temperature of approximately -78°C. The vapor-gas phase is captured in the extraction solution 171, 171a when the aerosol passes in the form of bubbles through microimpingers 160, 160a. The combined solutions from the two microimpingers are separated as vapor-gas phase solution 210 captured in the impinger at step 182.

Non-polar components

The CFP and impinger vapor phase solution 210 are combined in a clean Pyrex® tube at step 190. At step 200, all particulate material is extracted from the CFP using the impinger vapor phase solution 210 (which contains dichloromethane and methanol as solvent) by thorough shaking (disintegrating the CFP), vigorous stirring for 5 minutes and finally centrifugation (4500 g, 5 minutes, 10ºC) to separate the polar and non-polar components of the whole extract 230 aerosol.

At step 250, a 10 mL aliquot 240 of the whole aerosol extract 230 was taken. At step 260, a 10 mL aliquot of water is added and the entire sample is vortexed and centrifuged. The non-polar fraction 270 was separated, dried using sodium sulfate and analyzed by GCxGC-TOFMS in full scan mode.

Complete Components

ISTD and RIM compounds were added to the polar 280 fraction, which was then directly analyzed by GCxGC-TOFMS in full scan mode.

Each smoking replicate (n=3) contains an accumulated captured and recovered nonpolar fraction of 270 and a polar fraction of 280 for each sample.

Volatile components

All aerosol was captured using two micro-impingers 160, 160a arranged in series. Extraction solution 172, 172a, which in each case is N,N-dimethylformamide (DMF) containing retention index marker (RIM) and stable isotopically labeled internal standard (ISTD) compounds, is present in a volume of 10 ml in each microimpinger 160, 160a. Each of the cold baths 161, 161a contains a mixture of dry ice and isopropyl ether to maintain each of the microimpingers 160, 160a at a temperature of approximately -60°C. The vapor-gas phase is captured in the extraction solution 170, 170a when the aerosol passes in the form of bubbles through microimpingers 160, 160a. The combined solutions from the two microimpingers are separated as the volatile phase 211 in step 183. The volatile phase 211 is analyzed separately from the other phases and injected directly into the GCxGC-TOFMS method by cold injecting directly into the column without further preparation.

Table 3 below shows the levels of representative compounds from eucalyptus particles in an aerosol generated from an aerosol generating article containing Sample A of homogenized plant material containing only eucalyptus particles. For comparative purposes, Table 3 also shows the levels of representative compounds in the aerosol generated from an aerosol generating article that contains Sample E of homogenized plant material containing only tobacco particles (hence not prepared in accordance with the present invention).

Table 3. Content of characteristic compounds in aerosol

Compound Sample A
(micrograms per product) Sample A (micrograms per gram) Sample A (micrograms per 55 ml puff) Sample E
(micrograms per product) Eucalyptus 99.27 425 8.27 0.02 8-Desmethyleucalyptin 88.45 380 7.37 0.03 Eucalyptol 80.12 340 6.68 0.00

Relatively high levels of characteristic compounds were measured in the aerosol generated from sample A. The ratio of eucalyptol to eucalyptin and the ratio of eucalyptol to 8-desmethyleucalyptin were less than 1. Thus, the levels of characteristic compounds indicated the presence of eucalyptus particles in the sample. In contrast, for tobacco-only Sample E, which contained essentially no eucalyptus particles, levels of the signature compounds were found to be at or near zero.

For each of the samples B-D containing a proportion of eucalyptus particles, the amount of representative compounds in the aerosol can be estimated based on the values in Table 3, assuming that the amount is present in proportion to the weight of eucalyptus particles in the aerosol-generating substrate from which the aerosol is generated.

Other compounds identified in the aerosol generated from sample A that are specific to eucalyptus include epiglobulol (CAS number 88728-58-9, 64.13 microgram/item); ice (CAS number 21747-46-6, 51.64 micrograms/item); Tasmanone (CAS No. 22595-52-4, 39.12 micrograms/item); alloaromadendren (CAS number 25246-27-9, 29.99 micrograms/item); alpha-terpineol acetate (CAS number 10581-37-0, 25.19 micrograms/item); euglobal III (CAS number 76449-26-8, 21.66 micrograms/item). Such compounds may also be used to identify and evaluate the presence and quantities of eucalyptus plant material in an article.

Table 4 below shows more generally the composition of an aerosol generated from an aerosol generating article containing Sample A (eucalyptus only) compared to the composition of an aerosol generated from a tobacco-only Sample E (tobacco only). This reduction is the reduction provided by replacing the tobacco particles in the homogenized sample E plant material with eucalyptus particles.

Table 4. Aerosol composition

Aerosol component Sample E Sample A Decrease (%) Nicotine (mg/product) 1.25 0 -100% Glycerol (mg/product) 4.9 4.5 -8% All particulate material (mg/item) 54 35 -35% Carbon monoxide (mg/item) 0.53 0.60 13% Propionic aldehyde (µg/product) 14.3 8.6 -40% Crotonaldehyde (µg/product) 1.9 1.4 -26% Methyl ethyl ketone (µg/product) 7.6 4.8 -37% Butyraldehyde (µg/product) 14.1 8.8 -38% Acetaldehyde (mg/product) 211 72 -66% Phenol (mg/product) 1.5 0.68 -55% o-cresol (µg/product) 0.08 0.045 -44% Pyrocatechol (mg/product) 13.9 5.4 -61% Hydroquinone (mg/item) 6.9 2.2 -68% Acrylonitrile (µg/product) 0.150 0.088 -41% Styrene (µg/product) 0.63 0.48 -24% Isoprene (mg/product) 1.95 0.94 -52% Pyridine (µg/product) 8.0 2.11 -74% Benzo[a]pyrene (µg/product) 0.70 <0.054 -92% Benz[a]anthracene (µg/product) 1.60 <0.047 -97% Pyrene (µg/product) 5.2 0.054 -99%

As shown in Table 4, an aerosol produced from Sample A containing 100 percent by weight eucalyptus powder on a dry weight basis of particulate plant material resulted in reduced levels of propionaldehyde, crotonaldehyde, methyl ethyl ketone, butyraldehyde, acetaldehyde, phenol, o- cresol, catechol, hydroquinone, acrylonitrile, styrene, isoprene, pyridine, benzo[a]pyrene, benzo[a]anthracene, pyrene and total particulate material compared to the aerosol level in Sample E obtained using 100 percent by weight tobacco based on the dry weight of particulate plant material.

Claims (44)

1. An aerosol-generating article containing an aerosol-generating substrate, wherein the aerosol-generating substrate contains homogenized plant material, the homogenized plant material contains at least 2.5 percent by weight of eucalyptus particles on a dry weight basis, an aerosol-generating substance, and binder, wherein the aerosol-generating substrate contains: at least 0.04 mg of eucalyptol per gram of substrate on a dry weight basis; at least 0.2 mg of eucalyptin per gram of substrate on a dry weight basis; And at least 0.2 mg 8-desmethyleucalyptin per gram of substrate on a dry weight basis. 2. The aerosol generating product of claim 1, wherein the amount of eucalyptin per gram of substrate is at least 3 times the amount of eucalyptol per gram of substrate, and wherein the amount of 8-desmethyleucalyptin per gram of substrate is at least 3 times the amount eucalyptol per gram of substrate. 3. An aerosol-generating product according to claim 1 or 2, wherein when the aerosol-generating substrate is heated according to Test Method A, an aerosol is generated containing: at least 10 micrograms of eucalyptol per gram of substrate on a dry weight basis; at least 10 micrograms of eucalyptin per gram of substrate on a dry weight basis; And at least 10 micrograms of 8-desmethyleucalyptin per gram of substrate on a dry weight basis, wherein the amount of eucalyptol per gram of substrate is not more than twice the amount of eucalyptin per gram of substrate, and wherein the amount of eucalyptol per gram of substrate is not more than twice the amount of 8-desmethyleucalyptin per gram of substrate, wherein during Test Method A, the aerosol generating substrate is heated in the holder of the tobacco heating system 2.2 according to a Health Canada approved machine smoking regime as defined in ISO/TR 19478-1:2014. 4. The aerosol generating product of claim 3, wherein the aerosol generated by heating the aerosol generating substrate further contains at least 0.1 milligrams of nicotine per gram of substrate. 5. An aerosol-generating product according to claim 3 or 4, in which the amount of eucalyptol per gram of substrate is no more than 1.2 times the amount of eucalyptol per gram of substrate, and the amount of eucalyptol per gram of substrate is no more than 1, 2 times the amount of 8-desmethyleucalyptin per gram of substrate. 6. The aerosol generating product of any one of the preceding claims, wherein the homogenized plant material further comprises up to 97 percent by weight of tobacco particles on a dry weight basis. 7. The aerosol generating product according to claim 6, wherein the weight ratio of eucalyptus particles to tobacco particles is not more than 1:4. 8. An aerosol generating product according to any of the preceding claims, wherein the binder contains guar gum. 9. The aerosol generating article of any one of the preceding claims, wherein the homogenized plant material in the aerosol generating substrate is in the form of a molded sheet. 10. An aerosol-generating product according to any one of claims. 1-8, in which homogenized plant material in the aerosol-generating substrate is formed by a papermaking method. 11. The aerosol generating article of any one of the preceding claims, wherein the aerosol generating substrate comprises one or more sheets of homogenized plant material, wherein each of the one or more sheets of homogenized plant material is individually characterized by one or more of the following: thickness from 100 microns to 600 microns; or grammage from 100 g/ ^m2 to 300 g/ ^m2 . 12. The aerosol generating product according to claim 11, wherein the aerosol generating substrate comprises a current collector. 13. An aerosol-generating article according to any of the preceding claims, wherein, when the aerosol-generating substrate is heated according to Test Method A, the aerosol generated from the aerosol-generating substrate contains: eucalyptol in an amount of at least 0.2 micrograms per puff of aerosol; eucalyptin in an amount of at least 0.2 micrograms per puff of aerosol; And 8-desmethyleucalyptin in an amount of at least 0.2 micrograms per puff of aerosol, wherein the aerosol puff has a volume of 55 milliliters generated by the smoking machine, wherein the amount of eucalyptol per puff is no more than twice the amount of eucalyptol per puff, and wherein the amount of eucalyptol per puff is not more than twice the amount of 8-desmethyleucalyptin per puff puff, wherein during Test Method A, the aerosol generating substrate is heated in the holder of the tobacco heating system 2.2 according to a Health Canada approved machine smoking regime as defined in ISO/TR 19478-1:2014. 14. An aerosol generating substrate comprising homogenized plant material that contains at least 2.5 percent by weight of eucalyptus particles on a dry weight basis, an aerosol generating agent and a binder, wherein the aerosol generating substrate comprises: at least 0.04 mg of eucalyptol per gram of substrate on a dry weight basis; at least 0.2 mg of eucalyptin per gram of substrate on a dry weight basis; And at least 0.2 mg 8-desmethyleucalyptin per gram of substrate on a dry weight basis. 15. An aerosol generating system containing: an aerosol generating device comprising a heating element; And aerosol generating product according to any one of claims. 1-13. 16. An aerosol obtained by heating the aerosol-generating substrate according to claim 14, containing: eucalyptol in an amount of at least 0.2 micrograms per puff of aerosol; eucalyptin in an amount of at least 0.2 micrograms per puff of aerosol; And 8-desmethyleucalyptin in an amount of at least 0.2 micrograms per puff of aerosol, wherein the aerosol puff has a volume of 55 milliliters generated by the smoking machine, wherein the amount of eucalyptol per puff is not more than twice the amount of eucalyptol per puff, and wherein the amount of eucalyptol per gram of homogenized plant material is not more than twice the amount 8 -desmethyleucalyptin for a puff. 17. A method for manufacturing an aerosol-generating substrate, including the following steps: forming a pulp containing eucalyptus particles, water, an aerosol forming agent, a binder and optionally tobacco particles; casting or extruding pulp into sheet or filament form; And drying the sheet or threads at a temperature of 80 to 160 degrees Celsius.