CN116626179A - A heated cigarette aerosol component extraction device and a heated cigarette aerosol moisture determination method - Google Patents

Abstract

The invention discloses a heating coil smoke sol component extraction device and a heating coil smoke sol moisture determination method. The extraction device mainly comprises a catcher, a container and a peristaltic pump, wherein the catcher is connected with the container and the peristaltic pump in series through a hose; the main body part of the catcher is formed by sealing connection of a part A and a part B, an extraction cavity is formed in the catcher after the part A and the part B are connected in a sealing way, an interface A and an interface B are respectively arranged on the part A and the part B and are communicated with the extraction cavity, and a filter disc is arranged between the interface A and the interface B in the extraction cavity. The extraction device can directly collect and heat the aerosol released in the smoking process of the cigarettes in the smoking machine by using the collector, and can finish high-efficiency extraction of components in the aerosol without opening the collector, so that the loss of components to be detected in the aerosol in the processes of collecting and extracting the aerosol is reduced, and the measurement result is influenced.

Description

A heated cigarette aerosol component extraction device and heated cigarette aerosol moisture measurement fixed method

technical field

The invention relates to a heating cigarette aerosol component extraction device and a heating cigarette aerosol moisture determination method, which belong to the technical field of heating cigarette analysis and detection.

Background technique

The moisture content in the aerosol of heated cigarettes has a significant impact on the sensory quality. When the moisture content in the aerosol is low, the cigarette will be obviously dry during the smoking process; when the moisture content in the aerosol is high, it may cause the heated cigarette to burn the lips Or hot tongue. The research of Philip Morris International pointed out that the total mass of TPM of THS2.2 aerosol is 56.18mg/piece, of which the water content is as high as 44.65mg/piece, accounting for nearly 80%. Tar release in traditional cigarettes=TPM-nicotine release-moisture release, so accurate determination of moisture content in aerosol is of great significance for hazard assessment of heated cigarettes.

At present, the domestic tobacco industry mainly adopts YC/T345-2010 "Determination of Moisture in Tobacco and Tobacco Products by Gas Chromatography" to measure the amount of moisture released in heated cigarette aerosol. The main process is to take the Cambridge filter out of the trap and add a certain amount The extract was extracted and analyzed by gas chromatography. There is no standard for the determination of moisture content in heated cigarette aerosol.

Wang Kang and others from the Tobacco Quality Supervision and Inspection Station of Hubei Province smoked cigarettes according to the Canadian deep smoking mode. Propanol extractant, after shaking for 40 minutes, take 1mL of the extract into a chromatographic bottle for GC-TCD analysis, the moisture content in the heated cigarette aerosol is determined to be about 25.83-31.19mg/cigarette. This method provides a certain idea for the determination of moisture in the aerosol of heated cigarettes. However, since heated cigarettes contain hygroscopic atomizers such as glycerin and propylene glycol, the moisture content of aerosols is slightly higher than that of traditional cigarettes. In addition, because part of the moisture in the aerosol will condense on the inner wall of the trap, and only the moisture on the filter is extracted during extraction, the measurement result will be low. Moreover, since the trap needs to be opened to take out the filter piece during the test, part of the moisture will inevitably escape into the air, which further leads to low measurement results.

Contents of the invention

Aiming at the problems existing in the prior art, the first object of the present invention is to provide a device suitable for extracting aerosol components from heated cigarettes, which can not only achieve capture and extraction under relatively airtight conditions, but also reduce operating The volatilization loss of the components in the process aerosol can also achieve cyclic extraction to achieve efficient extraction and capture of the components to be measured in the aerosol on the filter, which effectively improves the accuracy of the measurement results, and has a wide range of applications, and can be used to detect any category The water content in the smoke aerosol can also be used to determine the content of key components such as nicotine, glycerin and propylene glycol in the smoke aerosol.

The second object of the present invention is to provide a method for measuring the moisture content of heated cigarette aerosol, which realizes the capture and extraction of the aerosol in the smoke by using a special trap in the same trap, and in the It is completed under relatively closed conditions, and realizes the circulation and efficient extraction of water in the aerosol, which effectively avoids the problem of low measurement results caused by the aerosol capture and extraction process. In addition, the method is easy to operate and the measurement results are accurate. And other advantages, can meet the requirements of rapid and accurate industrial determination.

To achieve the above technical purpose, the present invention adopts the following technical solutions:

The invention provides a device for extracting aerosol components from heated cigarettes, which includes a trap, a container and a peristaltic pump, and the trap is connected in series with the container and the peristaltic pump through a hose; the main part of the trap consists of part A (1-1) and part B (1-2) are sealed and connected, and the part A and part B are sealed and connected to form an extraction chamber in the trap, and the part A and part B are respectively provided with an interface A (1-1-2) and interface B (1-2-1) communicate with the extraction chamber, and a filter is provided between the interface A and the interface B in the extraction chamber.

The key point of the heating cigarette aerosol component extraction device of the present invention is to design a special trap. Compared with the traditional trap, an extraction chamber with a larger space is designed. The design of the extraction chamber can accommodate more extraction agents, especially The extraction agent forms a turbulent flow in the extraction chamber under the power of the peristaltic pump, which realizes the efficient extraction of the aerosol components on the filter and greatly improves the extraction efficiency. At the same time, the combined design of the trap, container and peristaltic pump can realize the cyclic extraction of the aerosol components on the filter. Compared with the general extraction process, it can reduce the amount of extraction agent and effectively reduce the concentration of the components to be tested during the extraction process. loss. In addition, the design of the trap is suitable for both the smoke machine and the extraction device. During the entire trapping and extraction process, there is no need to open the trap, which reduces the loss of the components to be measured during the trapping and extraction process and causes errors.

As a preferred solution, part A of the trap is provided with a cavity A (1-1-1) with one side opening, and part B is provided with a cavity B (1-2-2) with one side opening , and the inner diameter of the opening side of the cavity A matches the outer diameter of the opening side of the cavity B.

As a preferred solution, the outer wall of the opening side of the part B is provided with a sealing ring, and the part B is sealed and inserted in the part A, so that the cavity A and the cavity B communicate to form a sealed extraction cavity, and the filter Sheets (1-2-3) fit in the open side of cavity B. The outer wall of the opening side of part B is provided with a sealing ring, which can effectively prevent the smoke from escaping and the extraction agent from leaking out.

As a preferred solution, the interface A and the interface B are respectively sealed with a hose joint A (1-3) and a hose joint B (1-4).

As a preferred solution, an iron stand (4) is included, and the iron stand is used for fixing the catcher.

As a preferred solution, the trap is horizontally fixed on the iron platform; the hose connector A side of the trap faces upwards, the hose connector B side faces downwards, and the hose connector A passes through the hose Connect with the peristaltic pump, the hose connector B is connected to the container (2) through the hose; or, the hose connector B side of the trap faces upwards, the hose connector A side faces downwards, and the hose connector B passes through The hose is connected to the peristaltic pump, and the hose connector A is connected to the container through the hose.

As a preferred solution, the container is a top-sealed Erlenmeyer flask, and the container is provided with two liquid pipes, one end of the two liquid pipes is inserted into the bottom of the container from the top of the container, and the other end of the two liquid pipes passes through The hoses are connected to the peristaltic pump and the trap respectively.

As a preferred solution, both part A and part B of the trap are made of stainless steel. Compared with the traditional flue gas moisture trap, the polymer material is mostly used, and the stainless steel material has better thermal conductivity, making the aerosol in the flue gas easier to condense and collect.

As a preferred solution, both the cavity A and the cavity B are conical structures, and the total volume of the extraction cavity formed by the two is 3-5 cm ³ . The design of the cavity into a conical structure is not only conducive to condensation and trapping of the aerogel, but also conducive to the formation of a special turbulent flow of the extractant to improve the extraction efficiency of the components in the aerosol. The size of the extraction chamber enables it to accommodate an appropriate amount of extractant, increasing the contact area and time between the extractant and the filter, and improving extraction efficiency.

The present invention also provides a method for determining the moisture content of heated cigarette aerosol, comprising the following steps:

1) Install the trap in the smoking machine to trap the aerosol released during the smoking process of the heated cigarette;

2) After the suction is completed, the trap is disassembled and the extraction device is built, and the moisture in the aerosol captured by the trap is extracted in a circular manner;

3) Analyze the extract and calculate the moisture content in the aerosol.

The method for measuring the moisture content of the heated cigarette aerosol provided by the present invention can realize the capture of the aerosol in the smoke and the extraction process of the moisture in the aerosol in the same trap by using a special trap, and the whole process is carried out in a relatively airtight environment. Under certain conditions, it can reduce the detection error of the aerosol moisture content. At the same time, the extraction device built with the trap can realize the cyclic extraction of the moisture in the aerosol, improve the extraction efficiency, reduce the amount of extraction agent used, and reduce the subsequent detection error.

As a preferred scheme, 10-50ml extractant is added in the container (2) during the circulation extraction process, the flow rate of the extract is controlled by the peristaltic pump (3) to be 1-5ml/s, and the circulation extraction time is 5-30min .

As a preferred solution, the circulation extraction method adopts the extraction method of clockwise flow of extraction liquid, the extraction method of counterclockwise flow of extraction liquid, or the combination of clockwise flow of extraction liquid and counterclockwise flow of extraction liquid.

As a preferred solution, the extractant is methanol and/or isopropanol.

As a preferred solution, the number of smoked heated cigarettes is less than or equal to 5.

As a preferred solution, the analysis method is internal standard chromatographic analysis, and the chromatogram is gas chromatography or high performance liquid chromatography.

As a preferred scheme, in the internal standard method, the internal standard of the extract is methanol, the internal standard of nicotine is nicotine, the internal standard is dimethylquinoline, and the internal standard of glycerin and propylene glycol is 1,4-butanediol alcohol. The source of smoke is slightly different due to the different states of tobacco or tobacco products when they are heated or burned, so it is difficult to prepare smoke standard controls. The internal standard gas chromatography selects a certain amount of pure substances, and can accurately test the content of each component of the flue gas when there is no standard substance control.

Compared with the prior art, the beneficial technical effect brought by the technical solution of the present invention:

1) The extraction device suitable for heating cigarette aerosol components provided by the present invention adopts a special trap, which can not only realize the water content in the smoke aerosol, but also can be used to measure nicotine and glycerin in the smoke aerosol And the content of key ingredients such as propylene glycol.

2) In the technical solution provided by the present invention, the capture and extraction of the aerosol in the flue gas are all in the same trap by using a special trapping agent, and are completed under relatively closed conditions, realizing the aerosol in the aerosol The high-efficiency extraction of water effectively avoids the problem of low measurement results caused by aerosol capture and extraction.

Description of drawings

Figure 1 is an extraction device for heated cigarette aerosol components;

1 is a trap, 2 is a container, 3 is a peristaltic pump, and 4 is an iron stand;

Fig. 2 is a sectional view of each part of the catcher;

1-1 is part A, 1-2 is part B, 1-3 is hose joint A, 1-4 is hose joint B, 1-1-1 is cavity A, 1-1-2 is interface A , 1-2-1 is interface B, 1-2-2 is cavity B, 1-2-3 is filter.

Detailed ways

The present invention will be further described below in conjunction with specific embodiments. The following examples are intended to illustrate the present invention without further limiting the invention.

The optimal extraction conditions are determined:

1. Experimental method

(1) Preparation of experimental reagents

Extraction solution: use isopropanol as the extraction solution, the internal standard of water is methanol, the concentration is 6mg/ml, the internal standard of nicotine is dimethylquinoline, the concentration is 0.2mg/ml, the internal standard of glycerin and propylene glycol is 1, 4-butanediol at a concentration of 2 mg/ml.

Standard sample: Prepare an isopropanol solution with a moisture concentration of 10 mg/ml, a nicotine concentration of 0.4 mg/ml, a glycerin concentration of 10 mg/ml, and a propylene glycol concentration of 10 mg/ml.

(2) Experimental method

Put the Cambridge filter into the trap, press it twice to ensure the cap is tight, take 1ml of the standard sample through the small hole on the upper end of the trap and spread it slowly and evenly on the Cambridge filter, place it in the measuring device, and put it in the Erlenmeyer flask Load 20ml of extract solution and carry out the extraction experiment.

Water blank sample: put the Cambridge filter into the trap without adding standard sample, and extract the result according to the above method.

(3) Selection of extraction time

Select a flow rate of 300ml/min, the flow direction of the extract is clockwise, and the extraction time is respectively selected as 10, 15, 20, 25, and 30 min. After the extraction, the water content of the extract in the Erlenmeyer flask is measured. The measurement results are shown in Table 1. Measured value = moisture content determined by gas phase - moisture content of blank sample. It can be seen from Table 1 that the extraction time is preferably 20 and 25 min as the investigation condition of the orthogonal experiment.

The influence of table 1 extraction time on the moisture determination result

(4) Selection of the flow rate of the extract

Select the extraction time to be 30min, the flow direction of the extract is in a clockwise direction, and the flow rate of the extract is respectively selected to be 100, 150, 200, 250, 300ml/min, and the moisture content of the extract in the triangular flask is measured after the extraction is completed, and the measurement results are shown in Table 2 . Measured value = moisture content determined by gas phase - moisture content of blank sample. It can be seen from Table 2 that the flow rate of the extract is preferably 150, 200ml/min as the investigation condition of the orthogonal experiment.

Table 2 The influence of the flow rate of the extract on the moisture determination results

(5) Selection of the flow direction of the extract

Select the extraction time to be 30min, the flow rate of the extract to be 300ml/min, and the flow direction of the extract to be clockwise, counterclockwise, clockwise for 15min+counterclockwise for 15min, counterclockwise for 15min+clockwise for 15min, and measure the water content of the extract in the triangular flask after extraction , and the measurement results are shown in Table 2. Measured value = moisture content determined by gas phase - moisture content of blank sample. It can be seen from Table 3 that the flow direction of the extract is counterclockwise, counterclockwise + clockwise as the conditions of the orthogonal test.

Table 3 The influence of the flow direction of the extract on the moisture determination results

(6) Orthogonal test

The results of the single factor test were carried out by an orthogonal test with 3 factors and 2 levels, and the results are shown in Table 4. It can be seen from Table 4 that the influencing factors are: extraction time>flow direction>extraction flow rate, and the conditions of extraction time 20min, flow rate 150ml/min, counterclockwise + clockwise are preferred.

Table 4 Orthogonal test results

In the following examples, the extraction time is 20 minutes, the flow rate is 2.5ml/s, and the flow direction of the extract is 10 minutes counterclockwise and then 10 minutes clockwise.

Example 1

Choose the heated cigarette product produced by the domestic manufacturer A, balance it in a balance box with 22°C and 45% moisture for 48 hours after opening the package, use the heated cigarette smoking machine to smoke 5 heated cigarettes, put the φ44mm Cambridge filter into the customized trap The heated cigarette aerosol is captured in the collector. After the suction is completed, put the custom-made trap into the extraction device designed by the present invention for extraction, and compare it with the industry standard YC/T345-2010 vibration extraction method. Choose isopropanol for the extract, choose methanol as the internal standard of water, the concentration is 6mg/ml; choose dimethylquinoline as the internal standard for nicotine, the concentration is 0.2mg/ml; choose 1,4- Butanediol, the concentration is 2mg/ml. The measurement results are shown in Table 5. It can be seen from the results that the moisture content in the heated cigarette aerosol measured by the device of the present invention is 14.7% higher than that of the vibration extraction method, and the measurement result is more accurate; in addition, the device of the present invention is more accurate in determining the content of nicotine, glycerin, and propylene glycol than the vibration extraction method similar.

Table 5 vibration extraction and method result comparison of the present invention

Example 2

Choose the heated cigarette products produced by the domestic manufacturer B, balance them in a balance box with 22°C and 45% moisture for 48 hours after opening the package, use the heated cigarette smoking machine to smoke 5 heated cigarettes, put the φ44mm Cambridge filter into the customized trap The heated cigarette aerosol is captured in the collector. After the suction is completed, put the custom-made trap into the extraction device designed by the present invention for extraction, and compare it with the industry standard YC/T345-2010 vibration extraction method. Choose isopropanol for the extract, choose methanol for the internal standard of water, the concentration is 6mg/ml; choose dimethylquinoline for the internal standard of nicotine, the concentration is 0.2mg/ml; choose 1,4- Butanediol, the concentration is 2mg/ml. The measurement results are shown in Table 6. It can be seen from the results that the moisture content of the heated cigarette aerosol measured by the device of the present invention is 14.4% higher than that of the vibration extraction method, and the measurement results are more accurate; in addition, the device of the present invention is more accurate in determining the content of nicotine, glycerin, and propylene glycol than the vibration extraction method similar.

Table 6 vibration extraction and method result comparison of the present invention

Example 3

Choose the heated cigarette products produced by foreign manufacturers C, balance them in a balance box with 22°C and 45% moisture for 48 hours after opening the package, use the heated cigarette smoking machine to smoke 5 heated cigarettes, and put the φ44mm Cambridge filter into the customized trap The heated cigarette aerosol is captured in the collector. After the suction is completed, put the custom-made trap into the extraction device designed by the present invention for extraction, and compare it with the industry standard YC/T345-2010 vibration extraction method. Choose isopropanol for the extract, choose methanol for the internal standard of water, the concentration is 6mg/ml; choose dimethylquinoline for the internal standard of nicotine, the concentration is 0.2mg/ml; choose 1,4- Butanediol, the concentration is 2mg/ml. The measurement results are shown in Table 7. It can be seen from the results that the moisture content in the heated cigarette aerosol measured by the device of the present invention is 12.6% higher than that of the vibration extraction method, and the measurement results are more accurate; in addition, the device of the present invention is more accurate in determining the content of nicotine, glycerin, and propylene glycol than the vibration extraction method similar.

Table 7 vibration extraction and method result comparison of the present invention

Claims (15)

1. A heated cigarette aerosol composition extraction device, which is characterized in that:

comprises a catcher (1), a container (2) and a peristaltic pump (3); the catcher is connected with the container and the peristaltic pump in series through a hose;

the main body of the catcher is formed by sealing and connecting a part A (1-1) and a part B (1-2), an extraction cavity is formed in the catcher after the part A and the part B are connected in a sealing way, an interface A (1-1-2) and an interface B (1-2-1) are respectively arranged on the part A and the part B and are communicated with the extraction cavity, and a filter disc is arranged between the interface A and the interface B in the extraction cavity.

2. A heated cigarette aerosol composition extraction device as defined in claim 1 wherein: a cavity A (1-1-1) with one side open is arranged in a component A of the catcher, a cavity B (1-2-2) with one side open is arranged in a component B, and the inner diameter of the opening side of the cavity A is matched with the outer diameter of the opening side of the cavity B; the outer wall of the opening side of the component B is provided with a sealing ring, the component B is inserted in the component A in a sealing way, so that the cavity A and the cavity B are communicated to form a sealed extraction cavity, and the filter disc (1-2-3) is arranged in the opening side of the cavity B.

3. A heated cigarette aerosol composition extraction device as defined in claim 1 wherein: the hose connector A (1-3) and the hose connector B (1-4) are respectively and hermetically sleeved on the connector A and the connector B.

4. A heated cigarette aerosol composition extraction device as defined in claim 1 wherein: comprises an iron stand (4) for fixing the catcher.

5. The heated cigarette aerosol composition extraction device of claim 4, wherein: the catcher is horizontally fixed on the iron stand; the hose connector A side of the catcher is upward, and the hose connector B side is downward; the hose connector A is connected with the peristaltic pump (3) through a hose, and the hose connector B is connected with the container (2) through a hose; or the hose joint B side of the catcher faces upwards, and the hose joint A side faces downwards; the hose connector B is connected with the peristaltic pump through a hose, and the hose connector A is connected with the container through a hose.

6. A heated cigarette aerosol composition extraction device as defined in claim 1 wherein: the container is a conical bottle with a sealed top, the container is provided with two liquid pipelines, one ends of the two liquid pipelines are inserted into the bottom of the container from the top of the container, and the other ends of the two liquid pipelines are respectively connected with the peristaltic pump and the catcher through hoses.

7. A heated cigarette aerosol composition extraction device as defined in claim 1 wherein: the component A and the component B of the catcher are made of stainless steel.

8. A heated cigarette aerosol composition extraction device as defined in claim 1 wherein: the cavity A and the cavity B are both conical structures, and the total volume of an extraction cavity formed by the two structures is 3-5 cm ³ 。

9. A method for measuring the moisture of heated cigarette aerosol is characterized in that: the method comprises the following steps:

1) Installing a catcher in a smoking machine to catch aerosol released in the smoking process of the heated cigarettes;

2) After the suction is completed, the catcher is disassembled and the extraction device of any one of claims 1 to 8 is built, and the moisture in the aerosol captured by the catcher is circularly extracted;

3) The extract was analyzed to calculate the moisture content in the aerosol.

10. The method for measuring the moisture content of the heated cigarette aerosol as set forth in claim 9, wherein: in the circulating extraction process, 10-50 ml of extractant is added into a container, the flow rate of the extraction liquid is controlled to be 1-5 ml/s by a peristaltic pump, and the circulating extraction time is 5-30 min.

11. The method for measuring the moisture content of the heated cigarette aerosol as set forth in claim 9, wherein: the circulating extraction mode adopts an extraction mode of clockwise flow of the extraction liquid, an extraction mode of anticlockwise flow of the extraction liquid or an extraction mode of combining the clockwise flow of the extraction liquid and the anticlockwise flow of the extraction liquid.

12. The method for measuring the moisture content of the heated cigarette aerosol as set forth in claim 10, wherein: the extractant is methanol and/or isopropanol.

13. The method for measuring the moisture content of the heated cigarette aerosol as set forth in claim 9, wherein: the number of the heated cigarettes is less than or equal to 5.

14. The method for measuring the moisture content of the heated cigarette aerosol as set forth in claim 9, wherein: the analysis mode is internal standard method chromatographic analysis, and the chromatograph is gas chromatograph or high performance liquid chromatograph.

15. The method for measuring the moisture content of the heated cigarette aerosol as set forth in claim 9, wherein: in the internal standard method, the internal standard of the extract is methanol, the internal standard of the nicotine is dimethylquinoline, and the internal standard of the glycerol and the propylene glycol is 1, 4-butanediol.