CN120818405A - Preparation method of water-soluble essence sustained release agent, aerosol generating product and cigarette case - Google Patents

Abstract

The invention discloses a preparation method of a water-soluble essence sustained release agent, the water-soluble essence sustained release agent, an aerosol generating product and a cigarette case, which comprises the steps of respectively weighing water-soluble essence and beta-cyclodextrin, wherein the mass ratio of the water-soluble essence to the beta-cyclodextrin is 50-60:1, 60-70:1, 70-80:1, 80-90:1 or 90-100:1, adding the beta-cyclodextrin into the water-soluble essence, stirring, wherein the stirring speed is 750-770r/min, 770-790r/min, 790-810 r/min, 810-830 r/min or 830-850 r/min, obtaining a mixed solution, and homogenizing the mixed solution to obtain the water-soluble essence sustained release. The invention adopts a simple, effective and low-cost method to prepare the essence sustained release agent which can regulate and control the fragrance release rate, prolong the fragrance retention time and optimize the smoke quality, thereby providing technical support for the development of low-tar harm reduction in the cigarette industry. And in the preparation process, no water component is added, and the water-soluble essence slow release agent with high stability is obtained by matching with the selection of technological parameters.

Description

Preparation method of water-soluble essence sustained release agent, aerosol generating product and cigarette case

Technical Field

The invention belongs to the technical field of flavoring of tobacco products, and particularly relates to a preparation method of a water-soluble essence sustained-release agent, the water-soluble essence sustained-release agent, an aerosol generating product and a cigarette case.

Background

In the technical field of cigarette flavoring, the addition of essence is an important means for improving the sensory quality of cigarettes. In the traditional cigarette flavoring technology, the water-soluble essence often causes rapid loss of aroma components in the storage and smoking processes due to strong volatility, and long-acting slow release of aroma substances is difficult to realize, so that the durability and stability of cigarette aroma are affected. In addition, the conventional flavoring method is easy to cause the defect of insufficient coordination between the essence and the smoke, possibly causes the problems of enhanced delayed stimulation, single taste-absorbing layering and the like, and is difficult to meet the requirements of consumers on high-quality cigarettes.

Meanwhile, with the deep development of the cigarette industry in China to the direction of 'low-tar harm reduction', higher requirements are put on the essence adding technology, the quality of aroma is required to be improved, the release of harmful substances is reduced by optimizing the slow release performance of the essence while the content of tar is low, and the soft, fine and low-irritation characteristics of smoke are realized.

Aiming at the problems, some prior arts have tried to improve the stability of essence by adopting slow release technology such as microcapsule embedding. However, these methods often have limitations such as complex process, relatively high cost, or unsatisfactory slow release effect.

In addition, the prior art also discloses improving cigarette quality by preparing a fragrance slow-release agent for cigarettes, for example CN107365628A discloses adding water and water-soluble essence and spice into a beaker, wherein the weight percentage of the water-soluble essence and spice is 0.25% -50%, a first clear solution obtained after full stirring is a base solution, hydroxypropyl-beta-cyclodextrin is fully dissolved in the base solution, the weight ratio of the hydroxypropyl-beta-cyclodextrin to the base solution is 1:1-1:10, a second clear solution obtained after full stirring is an inclusion agent, a mixture of an alcohol solvent and the alcohol-soluble essence and spice is added into the beaker, the solution obtained after full stirring is an inclusion object, the inclusion object is slowly dripped into the inclusion agent, and after the dripping is completed, the mixture is fully stirred, and then the mixture is left stand. On one hand, in the prior art, water is required to be added into water to prepare base solution, the existence of water components can lead to that the smoking articles containing the slow release agent are more easily wetted, the service life of the smoking articles is shortened, and the water components can be further evaporated to release heat during smoking, so that the smoking taste temperature of the smoking articles is improved. On the other hand, the aroma of the prior art is based on the mutual supplementation of the water-soluble essence and the alcohol-soluble aromatic substances for cigarettes, and impurities in the alcohol-soluble aromatic substances are increased in the dripping process, so that the durability and the stability of the aroma of the cigarettes are also influenced.

Disclosure of Invention

The invention aims to provide a preparation method of a water-soluble essence sustained release agent, the water-soluble essence sustained release agent, an aerosol generating product and a cigarette case, and the purposes of simplifying the preparation process, having high stability, prolonging the action time and the storage time of aroma in the smoking process of cigarettes and improving the smoking quality are achieved.

In order to solve the technical problems, the invention adopts the following technical scheme:

in a first aspect, the invention provides a preparation method of a water-soluble essence sustained release agent, which comprises the following steps:

step A, respectively weighing water-soluble essence and beta-cyclodextrin, wherein the mass ratio of the water-soluble essence to the beta-cyclodextrin is 50-60:1, 60-70:1, 70-80:1, 80-90:1 or 90-100:1;

adding beta-cyclodextrin into water-soluble essence, and stirring at a rotation speed of 750-770 r/min, 770-770 r/min, 790-810 r/min, 810-830 r/min or 830-850 r/min to obtain a mixed solution;

And C, homogenizing the mixed solution to obtain the water-soluble essence slow release.

Further, the water-soluble essence comprises one or more of vanilla essence, orange essence, tobacco extract, mel, sweetener, glycyrrhrizae radix extract, fructus Jujubae extract, fructus fici extract, tea extract, flos Lupuli extract, mume fructus extract, blackcurrant extract, and apple extract.

Further, in the step C, the homogenizing treatment comprises homogenizing at room temperature for 15-25 min at 10000 r/min.

Further, the step B comprises the following steps:

Step B1, heating the water-soluble essence in a water bath at 25-27 ℃, 27-29 ℃, 29-31 ℃, 31-33 ℃ or 33-35 ℃;

and B2, adding the beta-cyclodextrin into the water-soluble essence and stirring under the condition of keeping water bath heating.

Further, in the step B2, the stirring time is 25-27 min, 27-29 min, 29-31 min, 31-33 min or 33-35 min.

The invention further claims a water-soluble essence sustained release agent prepared by any one of the technical schemes.

In a second aspect, the invention provides an aerosol-generating article comprising a water-soluble flavour slow-release formulation prepared according to any one of the above-mentioned techniques.

Wherein the aerosol-generating article is a smoking article comprising an aerosol-forming substrate which upon heating generates an aerosol which is directly inhalable into a user's lungs through a user's mouth.

Preferably, the aerosol-forming substrate is a solid aerosol-forming substrate. The aerosol-forming substrate may comprise both solid and liquid components.

Preferably, the aerosol-forming substrate comprises nicotine. In some preferred embodiments, the aerosol-forming substrate comprises tobacco.

Preferably, the solid aerosol-forming substrate may comprise one or more of a powder, granule, pellet, chip, strand, stick or sheet, containing one or more of herbal leaf, tobacco rib, flat tobacco and homogenized tobacco.

Alternatively or additionally, the aerosol-forming substrate may comprise tobacco-free aerosol-forming material. For example, the aerosol-forming material may be a tablet comprising nicotine salt and an aerosol-forming agent.

In this patent, an aerosol-former is used to describe any suitable known compound or mixture of compounds that, in use, promotes aerosol formation and is substantially resistant to thermal degradation at the operating temperature of the aerosol-generating article.

Preferably, suitable aerosol formers are known in the art and include, but are not limited to, polyols such as propylene glycol, triethylene glycol, 1, 3-butanediol, and glycerol, esters of polyols such as monoacetin, diacetin, or triacetin, and aliphatic esters of mono-, di-, or polycarboxylic acids such as dimethyl dodecanedioate and dimethyl tetradecanedioate. Preferred aerosol formers are polyols or mixtures thereof, such as propylene glycol, triethylene glycol, 1, 3-butanediol, and most preferably glycerol.

Preferably, the aerosol-forming substrate may comprise a single aerosol-former. Alternatively, the aerosol-forming substrate may comprise a combination of two or more aerosol-formers.

Preferably, the aerosol-forming substrate has an aerosol former content of greater than 5% by dry weight. More preferably, the aerosol-forming substrate may have an aerosol former content of between about 5% and about 30% by dry weight. In one embodiment, the aerosol-forming substrate has an aerosol former content of about 20% by dry weight.

Preferably, the aerosol-generating article may have the appearance of a conventional cigarette, with the cigarette items such as cigarettes and their specifications generally being named according to the length of the cigarette, as described below. The term "standard" generally means a cigarette having a length of 68mm to 75mm, for example, about 68mm to about 72mm, the term "short" or "mini" means a cigarette having a length of 68mm or less, the term "superscalar" generally means a cigarette having a length of 75mm to 91mm, for example, about 79mm to about 88mm, the term "long" or "lengthened" generally means a cigarette having a length of 91mm to 105mm, for example, about 94mm to about 101mm, and the term "ultralong" generally means a cigarette having a length of about 110mm to about 121 mm. In addition, the smoking article is named according to the cigarette outer periphery, as described below. The term "standard" means a cigarette of an outer periphery of about 23mm to 25mm, the term "thick" means a cigarette of an outer periphery of 25mm or more, the term "thin" means a cigarette of an outer periphery of about 22mm to 23mm, the term "slender" means a cigarette of an outer periphery of about 19mm to 22mm, the term "ultra-fine" means a cigarette of an outer periphery of about 16mm to 19mm, and the term "fine" means a cigarette of an outer periphery of about 16mm or less. Thus, an oversized and ultrafine cigarette has a length of, for example, about 83mm and an outer circumference of about 17 mm. Standard, out-of-standard cigarettes, i.e. cigarettes having a length of 75mm to 91mm and a circumference of 23mm to 25mm, are favored by many customers. Cigarette articles of various sizes may also be manufactured with filters of different lengths. In general, short filters are used for cigarette articles of a standard that are short in both length and circumference. Typically, filter lengths range from 15mm for use with "short" and "standard" gauge cigarette articles to 30mm for use with "ultra-long" and "ultra-fine" gauge cigarette articles.

Further, the aerosol-generating article comprises a cigarette paper, a forming paper and/or a tipping paper;

the water-soluble essence slow release agent is coated in cigarette paper, forming paper and/or tipping paper,

The coating amount of the water-soluble essence slow-release agent is 0.3-0.4 mu L/mm ²,0.4～0.5μL/mm²,0.5～0.6μL/mm² or 0.6-0.7 mu L/mm ².

In a third aspect, the invention provides a cigarette case, which comprises the water-soluble essence slow release agent prepared by any one of the technical schemes.

Further, the cigarette case comprises a case piece, the water-soluble essence slow-release agent is coated in the case piece, and the coating amount of the water-soluble essence slow-release agent is 0.3-0.4 mu L/mm ²,0.4～0.5μL/mm²,0.5～0.6μL/mm² or 0.6-0.7 mu L/mm ².

Further, the cigarette case comprises lining paper, the water-soluble essence slow release agent is coated in the lining paper,

The coating amount of the water-soluble essence slow-release agent is 0.3-0.4 mu L/mm ²,0.4～0.5μL/mm²,0.5～0.6μL/mm² or 0.6-0.7 mu L/mm ².

The invention provides a preparation method of a water-soluble essence sustained release agent, the water-soluble essence sustained release agent, an aerosol generating product and a cigarette case, and aims to prepare the essence sustained release agent capable of regulating and controlling the aroma release rate, prolonging the aroma retention time and optimizing the smoke quality by adopting a simple, effective and low-cost method by utilizing the synergistic effect of the sustained release characteristic of beta-cyclodextrin and the water-soluble essence through an innovative liquid film forming technology, thereby providing technical support for the development of low-tar harm reduction in the cigarette industry. And in the preparation process, no water component is added, and the water-soluble essence slow release agent with high stability is obtained by matching with the selection of technological parameters.

The invention has the following beneficial effects:

(1) According to the invention, through the blending effect of the beta-cyclodextrin and the water-soluble essence, the volatilization rate of the essence is effectively delayed by utilizing the inclusion characteristic of the hydrophobic inner cavity of the beta-cyclodextrin on the essence molecules, and compared with the traditional flavoring technology, the slow release agent can continuously and stably release the fragrance in the storage and smoking processes of cigarettes, so that the fragrance retention time of the fragrance substances is obviously prolonged, the problem of fragrance attenuation caused by rapid loss of the essence is avoided, and the durability and stability of the fragrance of cigarettes are improved.

(2) The invention has simple raw materials and preparation process, can reduce the cost in the actual production process and the influence on the cigarette taste, and can ensure that the sustained release agent has better stability than low-speed stirring through homogenizing high-speed shearing, thereby having better sustained release effect.

(3) After the water-soluble essence sustained release agent prepared by the invention is applied to cigarettes, the aroma of the water-soluble essence can be fully coordinated and fused with the smoke of the cigarettes, so that a light and pure aroma style is formed. Meanwhile, the slow release effect of the beta-cyclodextrin enables aroma components to be uniformly released in the smoke, the layering sense of the odor absorption is enhanced, the irritation of the smoke is reduced, the smoke texture becomes softer and finer, and the sucking experience of consumers is remarkably improved.

(4) According to the invention, through accurately regulating and controlling the slow release performance of the essence, the release of harmful substances in the smoke is effectively reduced while the tar content is reduced. The inclusion of the beta-cyclodextrin can reduce degradation products of the essence at high temperature, and further improve the safety of smoke. In addition, the application of the sustained release agent can optimize the smoking quality of cigarettes, so that the product still keeps rich fragrance and comfortable taste under the precondition of low tar, accords with the development direction of the low tar harm reduction transformation of the cigarette industry in China, and provides technical support for improving the comprehensive competitiveness of the cigarette products.

(5) The slow release agent can be added to different positions of cigarettes (such as cigarette paper, forming paper and the like), and the addition position and the dosage of the slow release agent are controlled, so that the diversified flavoring effect can be realized. The flexibility not only enriches the aroma design space of cigarettes, but also provides a new technical path for the development of personalized and differentiated products.

Drawings

The foregoing and other aspects of the invention will be better understood when read in conjunction with the following drawings. It should be noted that the drawings are only examples of the claimed technical solutions.

FIG. 1 is a schematic flow chart of a preparation method of a water-soluble essence sustained-release agent;

FIG. 2 is a chromatogram of the detection component of the water-soluble vanilla sustained release agent of example 1 according to the present invention by GC-MS;

FIG. 3 is a thermal gravimetric experimental comparison chart of the water-soluble vanilla slow release formulation of example 1 of the present invention (a is the release profile of the water-soluble vanilla, b is the release profile of the vanilla with beta-cyclodextrin added);

fig. 4 is a chart showing fourier infrared spectrum comparison of the water-soluble vanilla sustained release agent of example 1 in the present invention.

Detailed Description

The detailed features and advantages of the present patent are described in detail in the following detailed description, which is sufficient to enable those skilled in the art to understand the technical disclosure of the patent and to practice it, and the related objects and advantages of the patent are readily understood by those skilled in the art from the description, claims and drawings disclosed herein.

In this specification and in the claims, reference will be made to a number of terms which, unless otherwise indicated, will be defined to have the following meanings:

the terms "comprising" or "having" are intended to be inclusive in a manner similar to the term "comprising," and also to encompass other forms of the term, such as the singular and the plural of the term in the english language, as well, including but not limited to, and are not intended to exclude, for example, other elements, components, integers or steps.

All numbers expressing quantities of ingredients, properties (e.g., weight average molecular weight), reaction conditions, and so forth, used are to be understood as being modified in all instances by the term "within the limits of unavoidable errors" or "about". Accordingly, the numerical values set forth herein are approximations that may vary depending upon the desired properties sought to be obtained by the present patent. At the very least, and not as an attempt to limit the application of the doctrine of equivalents to the scope of the claims, each numerical value should at least be construed in light of the number of reported significant digits and by applying ordinary rounding techniques.

All other terms used herein are intended to have the ordinary meaning known to those of ordinary skill in the art to which they pertain in the art in this patent, and more particularly, the meaning of how the patent claim can be implemented will be determined directly and unambiguously by those of ordinary skill in the art after reading the patent claims, specification, and drawings.

Even if there is no detailed description, omission or ambiguity in the claims, the description and the drawings of this patent, those skilled in the art can still obtain the only correct understanding by reading the claims, the description and the drawings without multiple reasoning or experiments, and effectively exclude various incorrect understanding modes which are not carried out for achieving the purpose of this patent.

One of ordinary skill in the art will preferably choose to read the patent claims, specification and drawings to reasonably interpret the terms, will choose to reasonably interpret the terms with reference to the relevant definitions in other documents disclosed by the inventor prior to the filing date, will choose to reasonably interpret the terms with reference to the references cited in the patent, and will choose to reasonably interpret the terms with reference to technical dictionaries, technical manuals, tool books, textbooks, national or industry technical standards, etc. commonly employed by those of skill in the art.

All references cited in this disclosure are incorporated by reference in their entirety into this specification to the extent they do not contradict the disclosure of the present disclosure. It will be apparent to those of skill in the art that products (devices, elements, apparatuses, compounds, compositions, materials, etc.) and methods (processes, steps, conditions, parameters, equipment, and test methods, apparatuses, etc.) other than those specifically described herein may be applied to practice of the application fully disclosed herein without undue experimentation. This patent is intended to cover all art-known functional equivalents of the methods, apparatus elements, materials, processes, and techniques specifically recited in this specification.

Furthermore, throughout the specification, reference is made to a number of publications. The disclosures of these publications in their entireties are hereby incorporated by reference into this application in order to more fully describe the state of the art to which the presently disclosed subject matter pertains. To the extent that is contained in the disclosure and in the statements that reference that disclosure, the disclosure is also incorporated by reference herein individually and specifically.

The various components used in this patent can be prepared by a variety of known methods well disclosed in the chemical literature.

Before the present patent materials, compounds, compositions, articles, devices, and methods are disclosed and described, it is to be understood that the aspects described below are not limited to specific synthetic methods or specific reagents as such may, of course, vary. It is also to be understood that the terminology used herein is for the purpose of describing particular aspects only and is not intended to be limiting. The tobacco shreds of the tobacco shred section are made of the cured tobacco leaves of the three-channel Mian-chi pond C3F Qin 96 of the river south of 2021, which are not particularly described below.

The inventors have also used flue-cured tobacco leaves for testing tobacco seed varieties including Chenzhou Guiyang B2F, C B2F, X F, yongzhou Lanshan B3F, C2F, X F, sanjingyan Miao B2F, C3F, X3F, guizhou Zunyi B2F, C2F, X2F, pichia square B3F, C3F, X2F, guizhou Pichia B2F, C2F, X F, yunnan Yuxi B3F, C3F, X F, yunnan Kunming B2F, C3F, X F, yunnan Canadian B2F, C3F, X F, including safflower Dajinyuan, cui 1, qin smoke 96, and the like. In addition, the inventors have used burley, aromatic, cigar, yellow sun-cured, and clove to conduct the test. The present patent is also applicable to the above-described raw materials unless otherwise specified below.

As shown in fig. 1, the invention provides an embodiment of a preparation method of a water-soluble essence sustained release agent, which comprises the following steps:

step A, respectively weighing water-soluble essence and beta-cyclodextrin, wherein the mass ratio of the water-soluble essence to the beta-cyclodextrin is 50-60:1, 60-70:1, 70-80:1, 80-90:1 or 90-100:1;

And B1, heating the water-soluble essence in a water bath at 25-27 ℃, 27-29 ℃, 29-31 ℃, 31-33 or 33-35 ℃, setting the temperature condition to be about 25-35 ℃, wherein the temperature is too low to be beneficial to the dissolution of beta-cyclodextrin (possibly resulting in too long stirring time), and the essence is lost when the temperature is too high.

And B2, adding the beta-cyclodextrin into the water-soluble essence and stirring under the condition of keeping water bath heating. Stirring at a rotation speed of 750-770 r/min, 770-770 r/min, 790-720 r/min, 810-830 r/min or 830-850 r/min, the stirring time is 25-27 min, 27-29 min, 29-31 min, 31-33 min or 33-35 min.

And C, homogenizing the mixed solution to obtain a homogenized solution, and standing the homogenized solution to obtain the water-soluble essence sustained release agent.

Wherein, the standing condition is natural standing at room temperature for about 3 h.

According to the invention, water is not added in the preparation process of the water-soluble essence sustained release agent, the characteristic that essence is water-soluble is selected, and the sustained release agent prepared from the water-soluble vanilla essence and beta-cyclodextrin is coated on the parts such as lining paper, cigarette paper, forming paper, tipping paper and the like of a cigarette case, so that water vapor is contacted with the water-soluble essence sustained release agent along with respiration in the smoking process of the cigarette as a triggering condition, and the fragrance of the cigarette can be effectively released. Compared with the water adding formula in the prior art, the quality is more stable, the evaporation heat of water is reduced during smoking, and especially, the water adding formula is not suitable for the situation that the first few cigarettes are hot during smoking, so that the market application degree of the essence slow-release agent is widely improved.

Example 1

The preparation steps of the water-soluble vanilla sustained release agent in the embodiment are as follows:

(1) 75g of water-soluble vanilla essence (from Hubei Zhongyan industries, inc.) was weighed out.

(2) 1G of beta-cyclodextrin (provided by Shanghai Ala Biochemical technology Co., ltd., purity: not less than 98%) was weighed for use.

(3) Heating vanilla essence in 35 deg.C water bath, starting stirrer, adding beta-cyclodextrin, and stirring at 800r/min for 30min.

(4) After stirring, the sample was placed in LYD500W-T homogenizer (from Shanghai Lan Intelligent science and technology Co., ltd.) at room temperature, and homogenized at 10000r/min for 20min to obtain slow release preparation of vanilla essence.

Example 2

The preparation method of the water-soluble Yunyan extract sustained release agent in the embodiment comprises the following steps:

(1) 75g of water-soluble Yunyan extract (from Hubei Zhongyan industry Limited liability company, the main component of which is ketone, etc.) is weighed.

(2) 1G of beta-cyclodextrin (provided by Shanghai Ala Biochemical technology Co., ltd., purity: not less than 98%) was weighed for use.

(3) Heating the Yunyan extract in 35 ℃ water bath, starting a stirrer, adding beta-cyclodextrin, and stirring at a constant speed for 30min under the rotating speed of 800 r/min.

(4) After stirring, placing the sample into LYD500W-T homogenizer (from Shanghai Lanyu intelligent technology Co., ltd.) at room temperature, homogenizing at 10000r/min for 20min to obtain the slow release preparation of Yunyan extract.

Example 3

Preparation of water-soluble sweet orange essence slow-release agent

75G of water-soluble orange essence (from Hubei Zhongyan industries, inc.) was weighed out.

1G of beta-cyclodextrin (provided by Shanghai Ala Biochemical technology Co., ltd., purity: not less than 98%) was weighed for use.

Heating sweet orange essence in 35 ℃ water bath, starting a stirrer, adding beta-cyclodextrin, and stirring at a constant speed for 30min under the rotation speed of 800 r/min.

After stirring, the sample was placed in LYD500W-T homogenizer (from Shanghai Lanyu Intelligent technology Co., ltd.) at room temperature, and homogenized for 20min at 10000r/min to obtain the slow release preparation of sweet orange essence.

Example 4

The embodiment provides application of water-soluble vanilla essence in cigarette case lining paper, and the vanilla essence slow release agent prepared in the embodiment 1 is uniformly coated in the cigarette case lining paper at a concentration of 0.5 mu L/mm ². The cigarette case can be prepared by adopting a method in the prior art, for example, a preparation method of CN204660443U, an inner case body formed by folding inner lining paper is embedded in the case body, the top seal of the inner lining paper is in a shape like a Chinese character 'Hui', a cigarette taking opening is arranged in the middle of the inner lining paper, a layer of moisture-preserving paste with the same width as the width of the case body is arranged outside the inner lining paper, the moisture-preserving paste covers the cigarette taking opening, at least one quarter of the front surface and the back surface of the case body are respectively stuck at two ends of the moisture-preserving paste, the moisture-preserving paste comprises a smooth area and a sticking area, the smooth area corresponds to the cigarette taking opening, and the sticking area is provided with viscose. Moisture-preserving paste attached to front surface of box one end of the upper part is provided with a lifting lug. The adhesive needs to adhere to one fourth of the front and back surfaces of the cigarette case body and the lining paper at the top, but the adhesive is not adhered to the smooth area of the cigarette taking port on the corresponding lining paper, so as to avoid adhering to the cigarettes inside.

Example 5

The present example provides the use of water-soluble vanilla essence in cigarette paper, and the vanilla essence slow release agent prepared in example 1 is uniformly coated in cigarette paper at a concentration of 0.5 μl/mm ². The prior art methods can be used to prepare cigarette products such as CN107348563a, where the cut tobacco segments are made up of tobacco wrapped with cigarette paper, the filter is made up of a plug wrap wrapped with a plug wrap, and the filter and cut tobacco segments are combined together by tipping paper to form a cigarette. The length of the tipping paper of the cigarette after the cigarette is rolled is 37mm, the length of the filter tip is 30mm, the length of the cut tobacco section (namely the cut tobacco filling section) is 54mm, the length of the whole cigarette is 84mm, the length of the hasp sections of the tipping paper and the cigarette paper is 7mm, the circumference of the conventional cigarette is 24.2mm, the width of the tipping paper is 27mm, and the length of the hasp sections at the two ends of the tipping paper is 2.8mm.

Example 6

This example provides the use of water-soluble vanilla essence in forming paper, and the vanilla essence slow release agent prepared in example 1 was uniformly coated in forming paper at 0.5 μl/mm ². The prior art methods can be used to prepare cigarette products such as CN107348563a, where the cut tobacco segments are made up of tobacco wrapped with cigarette paper, the filter is made up of a plug wrap wrapped with a plug wrap, and the filter and cut tobacco segments are combined together by tipping paper to form a cigarette. The length of the tipping paper of the cigarette after the cigarette is rolled is 37mm, the length of the filter tip is 30mm, the length of the cut tobacco section (namely the cut tobacco filling section) is 54mm, the length of the whole cigarette is 84mm, the length of the hasp sections of the tipping paper and the cigarette paper is 7mm, the circumference of the conventional cigarette is 24.2mm, the width of the tipping paper is 27mm, and the length of the hasp sections at the two ends of the tipping paper is 2.8mm.

Example 7

The present example provides the use of water-soluble vanilla essence in tipping paper, and the vanilla essence slow release agent prepared in example 1 was uniformly coated in tipping paper at 0.5 μl/mm ². The prior art methods can be used to prepare cigarette products such as CN107348563a, where the cut tobacco segments are made up of tobacco wrapped with cigarette paper, the filter is made up of a plug wrap wrapped with a plug wrap, and the filter and cut tobacco segments are combined together by tipping paper to form a cigarette. The length of the tipping paper of the cigarette after the cigarette is rolled is 37mm, the length of the filter tip is 30mm, the length of the cut tobacco section (namely the cut tobacco filling section) is 54mm, the length of the whole cigarette is 84mm, the length of the hasp sections of the tipping paper and the cigarette paper is 7mm, the circumference of the conventional cigarette is 24.2mm, the width of the tipping paper is 27mm, and the length of the hasp sections at the two ends of the tipping paper is 2.8mm.

To further illustrate the advantages of the present invention, the following performance tests were performed on the various embodiments.

1. Macroscopic morphology and odor assessment

The water-soluble essence sustained release agents prepared in examples 1 to 7 were subjected to macroscopic morphology and odor evaluation, and the evaluation results are shown in Table 1.

TABLE 1 macroscopic morphology and odor evaluation results of the Water-soluble essence sustained-release formulations of examples 1-7

Examples	Macroscopic morphology and odor
		Example 1	The slow release agent is light purple, and the herb smell in the smoke is intense during suction, and the smoke is fresh and natural
Example 2	The sustained release agent is dark yellow, and the smoke has rich taste and gradation during suction
		Example 3	The slow release agent is pale yellow, and the smoke is fragrant with the fragrance of the orange during suction, and the smoke is fresh and sweet after taste
Example 4	Fresh vanilla fragrance can be smelled by opening the cigarette case
		Example 5	When the cigarette case is opened, the elegant vanilla flavor can be smelled, and the cigarettes are taken out to smell the intense vanilla flavor
Example 6	When the cigarette case is opened, the elegant vanilla flavor can be smelled, and the cigarettes taken out and smoked have stronger vanilla flavor
		Example 7	When the cigarette case is opened, the elegant vanilla flavor can be smelled, and the cigarettes taken out and smoked have stronger vanilla flavor

2. Qualitative analysis of the composition

The liquid state vanilla sustained release agent obtained in example 1 was subjected to qualitative analysis of components by GC-MS under the following conditions:

The components of the essence released by the microcapsules are analyzed by adopting headspace sample injection-GC/MS, wherein a chromatographic column is an HP-1MS column, the sample injection temperature is 180 ℃, the split ratio is 10:1, the carrier gas is He and 99.999%, the flow rate is 1.0mL/min, the temperature raising program is that the temperature is raised to 180 ℃ at 10 ℃ per min (17 min) at 35 ℃ per min, and the solvent delay is 0min. Scanning by adopting a selective ion monitoring mode (SIM), searching by adopting an NIST spectrum library, and carrying out qualitative determination by combining characteristic ions of the standard sample and the target object.

The results of the detection are shown in FIG. 2 and Table 2, and 25 components were detected in total.

TABLE 2 GC-MS detection results of water-soluble vanilla sustained release agent

Where PK is indicated as peak number, RT is indicated as time in minutes (min) required for separating the compounds in the sample, area Pct is indicated as peak Area ratio, library/ID is indicated as substance where a vanilla slow release agent may be present, ref is indicated as reference, CAS is indicated as chemical CAS number, qual is indicated as mass.

The ingredients contained in the water-soluble vanilla slow release formulation of example 1 were determined by analysis of all possible substances and searching in the NIST library, based on a matching probability of more than 90%, and are specifically shown in table 3.

TABLE 3 ingredients determined to be present in the water-soluble vanilla controlled release formulation

As can be seen from Table 3, the water-soluble essence sustained-release agent prepared by the invention has better fragrance quality only by adding the water-soluble essence and matching with a specific process, and compared with the prior art, the alcohol-soluble aromatic substance component and the alcohol-soluble aromatic substance component can be completely omitted, thereby further ensuring the fragrance quality of the water-soluble essence sustained-release agent.

3. Thermogravimetric experiments

The same amount of water-soluble vanilla essence and the water-soluble vanilla essence slow release agent of the example 1 (i.e. the vanilla essence added with beta-cyclodextrin) are respectively and strictly coated on the same-size aroma-carrying paper, and the quality of the aroma-carrying paper is controlled to be equal before the beginning of the thermal gravimetric experiment.

The water-soluble vanilla essence and the water-soluble vanilla essence slow release agent added with beta-cyclodextrin are respectively and evenly coated on the forming paper with the thickness of 3x3mm ² according to the adding amount of 0.5 mu L for temperature programming experiment, and the temperature programming condition is that the temperature is raised to 100 ℃ from room temperature at the temperature raising rate of 10 ℃ per minute and the temperature is kept for 600 minutes.

As can be seen from the graph 3, the rate of mass decrease of the vanilla essence is obviously greater than that of the vanilla essence added with the beta-cyclodextrin in the temperature range of 10 ℃ per minute to 150 ℃, which shows that the release rate of the vanilla essence is obviously reduced in the temperature increasing process after the beta-cyclodextrin is added, the slow release effect is achieved, and the mass of the vanilla essence is lost by 5.5% when the temperature is increased to 150 ℃, and the loss of the vanilla essence added with the beta-cyclodextrin is 4.5%, which shows that the fragrance release amount of the vanilla essence added with the beta-cyclodextrin is smaller than that of the vanilla essence in the same temperature increasing process, and the slow release effect is obvious. In the subsequent constant temperature process of 150 ℃, the quality of the two is uniformly reduced, and after the temperature is kept constant for 10 hours, the quality of the vanilla essence added with the beta-cyclodextrin is 3.5 percent higher than that of the vanilla essence, which indicates that part of the vanilla essence is still coated and not released as the vanilla essence under the action of the beta-cyclodextrin, and further indicates that the slow release performance of the vanilla essence added with the beta-cyclodextrin is better than that of the vanilla essence and has quite stability in the relatively high constant temperature process.

4. Fourier infrared spectroscopy

Fourier infrared spectroscopy analysis can utilize vibration and rotational transitions of molecules to identify and study compounds. In an inclusion reaction, changes in the shape, intensity, and relative position of the infrared absorption peaks of the guest or host molecules can provide important information for the inclusion compound. The fourier infrared spectra of the water-soluble vanilla essence in liquid form and the water-soluble vanilla essence slow release formulation of example 1 (i.e., the liquid form with the added beta-cyclodextrin vanilla essence) were compared. Generally speaking, vanilla contains a large amount of aromatic compounds of alcohols, esters and aldehydes.

As can be seen in the IR spectrum of FIG. 4, the vanilla extract exhibits distinct absorption peaks at 3364, 2973 and 1048cm ^-1 due to O-H vibration, C-H stretching vibration of methylene and C-O-C stretching vibration of the aroma in the vanilla extract, and further, peaks at 1674, 1088 and 1048cm ^-1 are due to vibration of bound water, stretching of the aroma C-OH and stretching of C-O-C.

In the infrared spectrum of vanilla with added beta-cyclodextrin, similar to vanilla, characteristic peaks at 3373, 2973, 1674, 1088 and 1048cm ^-1 were located. However, the characteristic peaks of the vanilla essence move in the infrared spectrum of the clathrate, which indicates that the molecular structure of the vanilla essence changes, the aroma substance changes, and the aroma effect of the vanilla essence is weakened due to the change of the molecular structure.

The terms and expressions which have been employed herein are used as terms of description and not of limitation. The use of these terms and expressions is not meant to exclude any equivalents of the features shown and described (or portions thereof), and it is recognized that various modifications are possible and are intended to be included within the scope of the claims. Other modifications, variations, and alternatives are also possible. Accordingly, the claims should be looked to in order to cover all such equivalents.

Also, it should be noted that while the present invention has been described with reference to the particular embodiments presently, it will be appreciated by those skilled in the art that the above embodiments are provided for illustration only and that various equivalent changes or substitutions may be made without departing from the spirit of the invention, and therefore, the changes and modifications to the above embodiments shall fall within the scope of the claims of the present invention as long as they are within the true spirit of the invention.

Claims (10)

1. A method for preparing a water-soluble flavor sustained-release agent, comprising the following steps: Step A: Weighing a water-soluble flavor and β-cyclodextrin respectively, wherein the mass ratio of the water-soluble flavor to the β-cyclodextrin is 50-60:1, 60-70:1, 70-80:1, 80-90:1 or 90-100:1; Step B: adding the β-cyclodextrin to the water-soluble essence and stirring at a stirring speed of 750-770 r/min, 770-790 r/min, 790-810 r/min, 810-830 r/min or 830-850 r/min to obtain a mixed solution; Step C: The mixed solution is homogenized to obtain the water-soluble flavor sustained release. 2. The method for preparing a water-soluble flavor sustained-release agent according to claim 1, wherein the water-soluble flavor comprises one or more of vanilla essence, sweet orange essence, tobacco extract, honey, sweetener, licorice extract, red date extract, fig extract, tea extract, hop extract, plum extract, blackcurrant extract, and apple extract. 3. The method for preparing a water-soluble flavor sustained-release agent according to claim 1, characterized in that in the step C, the homogenization treatment comprises homogenizing at 10,000 r/min for 15 to 25 minutes at room temperature. 4. The method for preparing a water-soluble flavor sustained-release agent according to claim 1, wherein step B comprises the following steps: Step B1: heating the water-soluble flavor in a water bath at a temperature of 25-27°C, 27-29°C, 29-31°C, 31-33°C or 33-35°C; Step B2: While maintaining the water bath heating, add the β-cyclodextrin to the water-soluble flavor and stir. 5. The method for preparing a water-soluble flavor sustained-release agent according to claim 4, characterized in that in step B2, the stirring time is 25-27 min, 27-29 min, 29-31 min, 31-33 min or 33-35 min. 6. A water-soluble flavor sustained-release agent prepared according to the method for preparing a water-soluble flavor sustained-release agent according to any one of claims 1 to 5. 7. An aerosol-generating product, characterized in that the aerosol-generating product comprises the water-soluble flavor sustained-release agent according to claim 6. 8. The aerosol-generating article according to claim 7, wherein the aerosol-generating article comprises cigarette paper, plug wrapping paper and/or tipping paper; The water-soluble flavor sustained-release agent is applied to the cigarette paper, the plugging paper and/or the tipping paper, The coating amount of the water-soluble flavor sustained-release agent is 0.3-0.4 μL/mm ² , 0.4-0.5 μL/mm ² , 0.5-0.6 μL/mm ² or 0.6-0.7 μL/mm ² . 9. A cigarette box, characterized in that the cigarette box comprises the water-soluble flavor sustained-release agent according to claim 6. 10. The cigarette box according to claim 9, wherein the cigarette box comprises an inner lining paper and a box sheet, and the water-soluble flavor sustained-release agent is applied to the inner lining paper and/or the box sheet. The coating amount of the water-soluble flavor sustained-release agent is 0.3-0.4 μL/mm ² , 0.4-0.5 μL/mm ² , 0.5-0.6 μL/mm ² or 0.6-0.7 μL/mm ² .