CN108303477B - Method for detecting alcohols and other compounds in mainstream smoke of cigarette without burning during heating - Google Patents
Method for detecting alcohols and other compounds in mainstream smoke of cigarette without burning during heating Download PDFInfo
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- CN108303477B CN108303477B CN201810010611.2A CN201810010611A CN108303477B CN 108303477 B CN108303477 B CN 108303477B CN 201810010611 A CN201810010611 A CN 201810010611A CN 108303477 B CN108303477 B CN 108303477B
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Abstract
The invention provides a detection method of alcohol compounds (1, 2-propylene glycol, glycerol and menthol), phenols and free nicotine in main stream smoke of a heated non-burning cigarette, which comprises the following steps: (1) preparing a test solution; the method comprises the steps of trapping alcohol compounds in mainstream smoke of the heated non-combustible cigarette by using a filter disc; (2) preparing a standard solution; (3) measuring the content of alcohol compounds in the main stream smoke of the heated non-burning cigarette by adopting a gas chromatography; wherein the gas chromatography conditions comprise: a chromatographic column: CP-1301 silica gel column capillary column; the method can accurately, efficiently and environmentally detect the contents of main alcohol compounds (1, 2-propylene glycol, glycerol and menthol) phenols and free nicotine in the mainstream smoke of the cigarettes.
Description
Technical Field
The invention relates to the technical field of analytical chemistry, in particular to a method for detecting 1, 2-propylene glycol, glycerol and menthol in mainstream smoke of a cigarette which is not burnt by heating; a method for detecting phenolic compounds in mainstream smoke of a heated non-burning cigarette; a method for detecting free nicotine in mainstream smoke of a heated non-combustible cigarette.
Background
Heating of a non-combustible tobacco product (HNB) means that the non-combustible tobacco product is heated for smoking, chemical components in cigarettes are vaporized to generate smoke, and therefore the smoking requirement of people is met. Less harmful substances are present in the mainstream smoke of a non-burning tobacco product because heating of the non-burning tobacco product merely vaporizes or cracks the tobacco material by heating (without burning). Wherein, the 1, 2-propylene glycol, glycerol and other polyol compounds can keep the moisture of the tobacco products, can reduce the breakage in the processing process, simultaneously has the functions of reducing the irritation and improving the taste, and is a humectant commonly used in the tobacco products; meanwhile, the propylene glycol and the glycerol can be used as carriers for heating non-combustion smoke to assist the volatilization of components in the raw materials; menthol, as a necessary additive for mint-type cigarettes, is present in most non-combustible cigarettes. Therefore, accurate measurement of target substances such as 1, 2-propanediol, glycerol, and menthol is required.
In the prior art, reports of simultaneously measuring the contents of propylene glycol, glycerol and menthol in the smoke which is not heated and combusted are not found. The contents of the propylene glycol and the glycerol in the heated non-burning smoke are different from those of the electronic smoke sol, and the mainstream smoke matrix of the electronic smoke sol has larger difference with the conventional burning cigarette and the electronic cigarette matrix and has higher water content; the menthol content in the electronic smoke is higher than that of electronic smoke sol, so that the problem to be solved is how to accurately and simultaneously measure the contents of propylene glycol, glycerol and menthol in the smoke which is not heated and combusted, and eliminate the influence of high moisture content on gas chromatography.
Phenolic compounds are important harmful components in cigarette mainstream smoke and are listed in 46 harmful component lists of Canadian government and a regulatory component list recommended by WHO 'tobacco product regulatory research group', so that accurate determination of volatile phenolic compounds in cigarette smoke has important significance for cigarette harmfulness evaluation.
A heating non-combustion tobacco product (HNB) is composed of a tobacco rod (also called a heating rod) which is about half of a common cigarette in length, and chemical components in the tobacco rod are vaporized to generate smoke by sucking the heating non-combustion tobacco product, so that the smoking requirement of people is met. Because the product of the tobacco product which is not burnt is not heated, and only the substances of the cigarettes are vaporized or cracked by heating, the main stream smoke of the tobacco product which is not burnt is less in harmful substances, and simultaneously, because the product contains a large amount of glycerol, the main stream smoke matrix of the product has larger difference with the conventional burning cigarette matrix and has higher water content. When the phenol compounds in the mainstream smoke of the heating non-combustible tobacco product are measured, the substrate concentration is also improved when the detection sensitivity of the method is improved by simply increasing the smoking number of cigarettes, and the separation of the target objects is influenced.
At present, the high performance liquid chromatography specified in YC/T255-2008 is commonly adopted for detecting phenolic compounds in mainstream smoke of cigarettes in China, the method adopts a Cambridge filter to collect the phenolic compounds in the mainstream smoke, then an extraction solvent is added to ultrasonically extract the phenolic compounds on the filter, the ultrasonic time is as long as 40min, and meanwhile, the repeatability of a test result is influenced by the difference of different ultrasonic power, so that the problem to be solved is how to accurately and simultaneously determine the content of the phenolic compounds in the smoke which is not combusted during heating, and eliminate the influence of high moisture content on gas chromatography analysis.
The strength of cigarettes is related to the nicotine content in the mainstream smoke, and particularly has a closer relationship with free nicotine in the mainstream smoke. However, the salt formed by combining nicotine and organic acid is weak acid and weak base salt, and is easy to dissociate, so that the absolute content of free nicotine in smoke can be accurately measured with certain difficulty.
A heating non-combustion tobacco product (HNB) is composed of a tobacco rod (also called a heating rod) which is about half of a common cigarette in length, and chemical components in the tobacco rod are vaporized to generate smoke by sucking the heating non-combustion tobacco product, so that the smoking requirement of people is met. Because the tobacco product which is not burnt is heated and the substances of the cigarettes are vaporized or cracked only by heating, the main stream smoke of the tobacco product which is not burnt is less in harmful substances, and simultaneously, because the product contains a large amount of glycerol, the main stream smoke matrix of the tobacco product has larger difference with the conventional burning cigarette matrix and has higher water content. When the free nicotine in the mainstream smoke of the heating non-combustible tobacco product is measured, the substrate concentration is also improved when the detection sensitivity of the method is improved by simply increasing the smoking count of cigarettes, and the separation of the target object can be influenced. Therefore, the method for accurately measuring the content of free nicotine in the mainstream smoke of the tobacco product without burning has important theoretical significance and practical value for controlling the smoking quality of the tobacco product without burning.
At present, a Cambridge filter disc is generally adopted to capture nicotine in mainstream smoke of cigarettes for detection of free nicotine in the mainstream smoke of the cigarettes, then water and trichloromethane are added for extraction of nicotine on the filter disc, and as smoke particulate matters are enriched on the Cambridge filter disc, a target object cannot be completely extracted when water extraction is adopted, and detection data is higher when trichloromethane is adopted; in addition, the liquid-liquid extraction of water and trichloromethane consumes a long time, which is 2-4 hours, and the efficiency is not high, so that how to accurately measure the content of free nicotine in the heated non-combustible flue gas is a problem to be solved.
Disclosure of Invention
In order to solve the problem of simultaneously measuring the contents of propylene glycol, glycerol and menthol in the smoke which is not combusted during heating, the invention provides a method for simultaneously detecting main alcohol compounds (1, 2-propylene glycol, glycerol and menthol) in the main stream smoke of cigarettes by using a filter disc for trapping, solvent extraction and a gas chromatograph.
In order to accurately determine the main phenolic compounds in the main stream smoke of the heated non-burning cigarette, the invention provides the method for capturing the main phenolic compounds in the main stream smoke by using the capturing solution, so that the phenolic compounds in the main stream smoke of the heated non-burning cigarette can be rapidly, efficiently and accurately determined, and the efficiency and the accuracy of detecting the phenolic compounds are improved.
In order to accurately determine the free nicotine in the main stream smoke of the heated non-burning cigarette, the invention provides the method for capturing the main free nicotine in the main stream smoke by using the capturing solution, so that the free nicotine in the main stream smoke of the heated non-burning cigarette can be rapidly, efficiently and accurately determined, and the efficiency and the accuracy of detecting the free nicotine can be improved.
The method can accurately, efficiently and environmentally detect the content of the main alcohol compounds (1, 2-propylene glycol, glycerol and menthol) in the mainstream smoke of the cigarettes.
The purpose of the invention is realized by adopting the following technical scheme.
The invention provides a method for detecting alcohol compounds in mainstream smoke of a heated non-burning cigarette, which comprises the following steps:
(1) preparing a test solution comprising obtaining alcohol compounds from the total particulate matter of mainstream smoke of said heated non-burning cigarette;
(2) preparing a standard solution;
(3) measuring the content of alcohol compounds in the main stream smoke of the heated non-burning cigarette by adopting a gas chromatography; wherein the gas chromatography conditions comprise:
a chromatographic column: CP-1301 silica gel column capillary column;
preferably, the alcohol compounds are 1, 2-propanediol, glycerol and menthol.
Preferably, in the step (1), the preparing a test solution includes:
using a filter disc to capture the total particulate matters of the cigarettes in an ISO suction mode, then putting the filter disc into an organic solvent for oscillation and filtration;
preferably, the filter disc is a cambridge filter disc;
preferably, the number of cigarettes is 3-7, preferably 5;
preferably, the organic solvent is isopropanol;
preferably, the oscillation time is 20-35min, preferably 30 min;
preferably, the filtration is performed by using an anhydrous sodium sulfate needle filter;
preferably, in the step (1), the preparing a test solution includes:
using a Cambridge filter disc to collect total particulate matter of 5 cigarettes in an ISO suction mode, then placing the Cambridge filter disc into 20mL of isopropanol in a 100mL container, shaking for 30min at room temperature, transferring 2mL of extraction solution, and filtering through an anhydrous sodium sulfate needle filter.
Preferably, in the step (2), the preparing a standard solution includes: 1g of 1, 2-propylene glycol, glycerol and menthol are respectively taken, and the volume is determined by organic solvent;
preferably, the organic solvent is isopropanol;
preferably, in the step (2), the preparing a standard solution includes:
weighing 1g of 1, 2-propylene glycol, glycerol and menthol respectively into a 100mL container, fixing the volume by isopropanol, shaking up, and storing the obtained solution at 4 ℃; the solutions were transferred to 100mL containers at 0.2mL, 0.5mL, 2.5mL, 5mL, 7.5mL, 10mL, 15mL, and 20mL, respectively, to obtain standard solutions at concentrations of 0.02mg/mL, 0.05mg/mL, 0.25mg/mL, 0.50mg/mL, 0.75mg/mL, 1.00mg/mL, 1.50mg/mL, and 2.00mg/mL, respectively.
Preferably, the gas chromatography conditions further comprise:
the CP-1301 silica gel column capillary column has the column length of 30m, the inner diameter of the column of 0.32mm and the film thickness of 1 μm;
sample introduction temperature: 250 ℃;
detector temperature: 275 ℃;
the sample volume is 1 mu L;
the split ratio of split sample injection is as follows: 50: 1;
carrier gas: helium at a flow rate of 0.7 mL/min;
tail blowing: helium at a flow rate of 30 mL/min;
hydrogen gas: the flow rate is 40 mL/min;
air: the flow rate is 400 mL/min;
preferably, the initial temperature is 110 ℃ for 1min, increased from 110 ℃ to 150 ℃ at a rate of 10 ℃/min for 3min, and increased from 150 ℃ to 220 ℃ at a rate of 30 ℃/min for 5 min.
Preferably, the method for detecting alcohol compounds in mainstream smoke of the heated non-burning cigarette comprises the following steps:
(1) preparing a test solution:
collecting total particulate matter of 5 cigarettes by using a Cambridge filter disc under an ISO suction mode, then putting the Cambridge filter disc into a 100mL container, adding 20mL of isopropanol, oscillating for 30min at room temperature, transferring 2mL of solution, and filtering by using an anhydrous sodium sulfate syringe filter;
(2) preparation of standard solutions:
weighing 1g of 1, 2-propylene glycol, glycerol and menthol respectively into a 100mL container, fixing the volume by isopropanol, shaking up, and storing the obtained solution at 4 ℃; accurately transferring 0.2mL, 0.5mL, 2.5mL, 5mL, 7.5mL, 10mL, 15mL and 20mL of the above solutions into a 100mL container to obtain standard solutions with concentrations of 0.02mg/mL, 0.05mg/mL, 0.25mg/mL, 0.50mg/mL, 0.75mg/mL, 1.00mg/mL, 1.5.mg/mL and 2.00 mg/mL;
(3) determining the content of alcohol compounds in the main stream smoke of the heated non-burning cigarette by adopting a gas chromatography:
injecting the standard solution and the test solution into a gas chromatograph for determination, wherein the gas chromatograph conditions comprise:
a chromatographic column: CP-1301 silica gel column capillary column; preferably, the CP-1301 silica gel column capillary column has the column length of 30m, the inner diameter of the column of 0.32mm and the film thickness of 1 μm;
sample introduction temperature: 250 ℃;
detector temperature: 275 ℃;
the sample volume is 1 mu L;
the split ratio of split sample injection is as follows: 50: 1;
carrier gas: helium at a flow rate of 0.7 mL/min;
tail blowing: helium or nitrogen with a flow rate of 30 mL/min;
hydrogen gas: the flow rate is 40 mL/min;
air: the flow rate is 400 mL/min;
preferably, the initial temperature is 110 ℃ for 1min, increased from 110 ℃ to 150 ℃ at a rate of 10 ℃/min for 3min, and increased from 150 ℃ to 220 ℃ at a rate of 30 ℃/min for 5 min.
Compared with the prior art, the method for detecting the content of the alcohol compounds provided by the invention has the following beneficial effects:
(1) the method has high detection efficiency, and improves the working efficiency by trapping the main alcohol compounds (1, 2-propylene glycol, glycerol and menthol) in the main stream smoke at one time and simultaneously detecting the contents of three alcohols in a sample to be detected by using gas chromatography; the invention adopts the anhydrous sodium sulfate filter to achieve obvious effect, and eliminates the influence of high moisture in the sample on gas chromatography detection;
(2) the detection method provided by the invention saves the consumption of a large amount of organic reagents, reduces the cost and simultaneously reduces the harm of detection work on the environment and the health of detection personnel;
(3) the detection method has the advantages of high sensitivity, good repeatability and good recovery rate.
The invention provides a method for detecting phenolic compounds in mainstream smoke of a heated non-burning cigarette, which comprises the following steps:
(1) preparing a test solution; obtaining phenolic compounds from total particulate matter of mainstream smoke of the heated non-burning cigarette;
(2) preparing a standard solution;
(3) determining the content of alcohol compounds in the mainstream smoke of the cigarette which is not burnt by heating by adopting a high performance liquid chromatography; wherein the high performance liquid chromatography conditions comprise:
a chromatographic column:
explosive E2 column;
mobile phase: acetonitrile-water solution;
preferably, the phenolic compound is o-dihydroxybenzene, p-dihydroxybenzene, phenol, o-cresol, m-cresol, p-cresol, m-dihydroxybenzene.
Preferably, in the step (1), the preparing a test solution includes:
using a trapping solution to trap the total particulate matters of the cigarettes in an ISO suction mode, and then oscillating and filtering the obtained solution; wherein the concentration of the capture solution is 4%;
preferably, the number of cigarettes is 3-7, preferably 5;
preferably, the oscillation time is 2-7min, preferably 5 min;
preferably, the filtration is filtration with an aqueous phase filtration membrane, preferably with an aqueous phase filtration membrane of 0.22 μm;
preferably, in the step (1), the preparing a test solution includes:
collecting total particulate matters of 5 cigarettes in an ISO suction mode by using a collecting solution, oscillating the obtained solution at room temperature for 5min, and filtering by using a 0.22 mu m water-phase filter membrane;
preferably, the ratio of the number of cigarettes to the trapping solution is 5: 25 ml;
preferably, in the step (1), the preparing a test solution includes:
the total particulate matter of 5 cigarettes was trapped in two serial trap bottles containing 25mL of trapping solution in ISO suction mode, and then the solution in the two serial trap bottles was shaken at room temperature for 5min, and 2mL of the solution obtained above was removed and filtered through a 0.22 μm aqueous phase filter.
Preferably, in the step (2), the preparing a standard solution includes: respectively taking o-dihydroxybenzene, p-dihydroxybenzene, phenol, o-cresol, m-cresol, p-cresol and m-dihydroxybenzene, adding an organic solvent to completely dissolve, and then diluting by using the organic solvent;
preferably, the organic solvent is 4% acetic acid aqueous solution;
preferably, in the step (2), the preparing a standard solution includes:
respectively taking 100mg of o-dihydroxybenzene, 100mg of p-dihydroxybenzene, 100mg of phenol, 50mg of o-cresol, 50mg of m-cresol, 50mg of p-cresol and 20mg of m-dihydroxybenzene, adding 30mL of organic solvent into a 50mL container, completely dissolving, transferring into a 100mL container, and fixing the volume by the organic solvent;
preferably, in the step (2), the preparing a standard solution includes:
respectively adding 100mg of o-dihydroxybenzene, 100mg of p-dihydroxybenzene, 100mg of phenol, 50mg of o-cresol, 50mg of m-cresol, 50mg of p-cresol and 20mg of m-dihydroxybenzene into a 50mL container, adding 30mL of organic solvent until the o-cresol, the m-cresol, the p-cresol and the m-dihydroxybenzene are completely dissolved, transferring the mixture into the 100mL container, fixing the volume by the organic solvent, taking 10mL to 100mL of the obtained solution, and fixing the volume by the organic solvent to be used as a primary standard solution; then taking the primary standard solution in a container of 10mL to 100mL, and fixing the volume by using an organic solvent to obtain a secondary standard solution; respectively taking 1 mL, 2mL and 5mL of the obtained secondary standard solution and 1 mL, 2mL to 50mL of the obtained primary standard solution, and fixing the volume by using an organic solvent; respectively obtaining para-dihydroxybenzene standard solutions with the concentrations of 0.25 mug/mL, 0.50 mug/mL, 1.25 mug/mL, 2.51 mug/mL, 5.02 mug/mL and 12.54 mug/mL; m-dihydroxybenzene standard solution with concentration of 0.07. mu.g/mL, 0.13. mu.g/mL, 0.34. mu.g/mL, 0.67. mu.g/mL, 1.34. mu.g/mL, 3.35. mu.g/mL; ortho-diphenol standard solutions with concentrations of 0.36. mu.g/mL, 0.71. mu.g/mL, 1.78. mu.g/mL, 3.57. mu.g/mL, 7.13. mu.g/mL, 17.83. mu.g/mL; phenol standard solutions with concentrations of 0.26. mu.g/mL, 0.53. mu.g/mL, 1.32. mu.g/mL, 2.64. mu.g/mL, 5.28. mu.g/mL, 13.19. mu.g/mL; m-cresol standard solutions with concentrations of 0.14. mu.g/mL, 0.28. mu.g/mL, 0.71. mu.g/mL, 1.42. mu.g/mL, 2.83. mu.g/mL, 7.08. mu.g/mL; o-cresol standard solutions at concentrations of 0.24. mu.g/mL, 0.48. mu.g/mL, 1.21. mu.g/mL, 2.42. mu.g/mL, 4.85. mu.g/mL, 12.12. mu.g/mL.
Preferably, the high performance liquid chromatography conditions further comprise:
the inner diameter of the chromatographic column is 250mm × 4.6.6 mm,
preferably, the particle size of the filler is 5 μm;
preferably, the column temperature of the chromatographic column is: 20-40 ℃, preferably 30 ℃;
preferably, the flow rate of the chromatographic column is 1.0 ml/min;
preferably, the sample injection volume is: 10 mu L of the solution;
preferably, the volume ratio of water to acetonitrile is 50: 50.
Preferably, the method for detecting phenolic compounds in the mainstream smoke of the heated non-burning cigarette comprises the following steps:
(1) preparing a test solution:
collecting total particulate matters of 5 cigarettes in an ISO suction mode by using two serial collection bottles containing 25mL of collection solution, oscillating the solution in the two serial collection bottles for 5min at room temperature, transferring 2mL of the obtained solution, and filtering the solution by using a 0.22-micron water-phase filter membrane;
(2) preparation of standard solutions:
respectively adding 100mg of o-dihydroxybenzene, 100mg of p-dihydroxybenzene, 100mg of phenol, 50mg of o-cresol, 50mg of m-cresol, 50mg of p-cresol and 20mg of m-dihydroxybenzene into a 50mL container, adding 30mL of organic solvent until the o-cresol, the m-cresol, the p-cresol and the m-dihydroxybenzene are completely dissolved, transferring the mixture into the 100mL container, fixing the volume by the organic solvent, taking 10mL to 100mL of the obtained solution, and fixing the volume by the organic solvent to be used as a primary standard solution; then taking the primary standard solution in a container of 10mL to 100mL, and fixing the volume by using an organic solvent to obtain a secondary standard solution; respectively taking 1 mL, 2mL and 5mL of the obtained secondary standard solution and 1 mL, 2mL to 50mL of the obtained primary standard solution, and fixing the volume by using an organic solvent; respectively obtaining para-dihydroxybenzene standard solutions with the concentrations of 0.25 mug/mL, 0.50 mug/mL, 1.25 mug/mL, 2.51 mug/mL, 5.02 mug/mL and 12.54 mug/mL; m-dihydroxybenzene standard solution with concentration of 0.07. mu.g/mL, 0.13. mu.g/mL, 0.34. mu.g/mL, 0.67. mu.g/mL, 1.34. mu.g/mL, 3.35. mu.g/mL; ortho-diphenol standard solutions with concentrations of 0.36. mu.g/mL, 0.71. mu.g/mL, 1.78. mu.g/mL, 3.57. mu.g/mL, 7.13. mu.g/mL, 17.83. mu.g/mL; phenol standard solutions with concentrations of 0.26. mu.g/mL, 0.53. mu.g/mL, 1.32. mu.g/mL, 2.64. mu.g/mL, 5.28. mu.g/mL, 13.19. mu.g/mL; m-cresol standard solutions with concentrations of 0.14. mu.g/mL, 0.28. mu.g/mL, 0.71. mu.g/mL, 1.42. mu.g/mL, 2.83. mu.g/mL, 7.08. mu.g/mL; o-cresol standard solutions at concentrations of 0.24. mu.g/mL, 0.48. mu.g/mL, 1.21. mu.g/mL, 2.42. mu.g/mL, 4.85. mu.g/mL, 12.12. mu.g/mL;
(3) determining the content of alcohol compounds in the main stream smoke of the heated non-burning cigarette by adopting a high performance liquid chromatography:
injecting the standard solution and the test solution into a high performance liquid chromatograph for determination, wherein the conditions of the high performance liquid chromatograph comprise:
a chromatographic column:
explosive E2 column;
mobile phase: acetonitrile-water solution;
preferably, the inner diameter of the chromatographic column is 250mm × 4.6.6 mm,
preferably, the particle size of the filler is 5 μm;
preferably, the column temperature of the chromatographic column is: 20-40 ℃, preferably 30 ℃;
preferably, the flow rate of the chromatographic column is 1.0 ml/min;
preferably, the sample injection volume is: 10 mu L of the solution;
preferably, the volume ratio of the water to the acetonitrile solution is 50: 50.
Compared with the prior art, the method for detecting the content of phenols provided by the invention has the following beneficial effects:
(1) the method has short detection time, and the period for detecting the main phenolic compounds in the main stream smoke of the cigarette only needs about 10 minutes;
(2) compared with the existing method (YC/T255-2008), the method disclosed by the invention saves the consumption of a large amount of organic reagents, reduces the cost and simultaneously reduces the harm of detection work on the environment and the health of detection personnel;
(3) the method has the advantages of accurate operation, high sensitivity and good repeatability.
The invention provides a method for detecting free nicotine in mainstream smoke of a heated non-burning cigarette, which comprises the following steps:
(1) preparing a test solution; comprising obtaining free nicotine from total particulate matter of mainstream smoke of said heated non-burning cigarette;
(2) preparing a standard solution;
(3) measuring the content of free nicotine in the main stream smoke of the heated non-burning cigarette by adopting a gas chromatography; wherein the gas chromatography conditions comprise:
a chromatographic column: CP-1301 silica gel column capillary column;
column volume: 30 m.times.0.32 mm.times.1.0. mu.m.
Preferably, in the step (1), the preparing a test solution includes:
using a trapping solution to trap the total particulate matters of the cigarettes in an ISO suction mode, and then oscillating and filtering the obtained solution;
wherein the trapping solution is a mixed solution of water and trichloromethane, and the volume ratio of the water to the trichloromethane is 1: 1;
preferably, the number of cigarettes is 3-7, preferably 5;
preferably, the oscillation time is 2-7min, preferably 5 min;
preferably, the filtration is performed by using an anhydrous sodium sulfate needle filter;
preferably, in the step (1), the preparing a test solution includes:
trapping total particulate matters of 5 cigarettes in an ISO suction mode by using a trapping solution, oscillating the obtained solution at room temperature for 5min, and filtering by using an anhydrous sodium sulfate needle filter;
preferably, the ratio of the number of cigarettes to the trapping solution is 5: 25 ml;
preferably, in the step (1), the preparing a test solution includes:
and (3) trapping the total particulate matters of 5 cigarettes in an ISO suction mode by using two serial trapping bottles containing 25mL of trapping solution, then oscillating the solution in the two serial trapping bottles for 5min at room temperature, transferring 2mL of the obtained solution, and filtering by using an anhydrous sodium sulfate needle filter.
Preferably, in the step (2), the preparing a standard solution includes: taking 100mg of nicotine standard substance, and fixing the volume by using an organic solvent;
preferably, the organic solvent is chloroform;
preferably, in the step (2), the preparing a standard solution includes:
weighing 100mg of nicotine standard into a 50mL container, and metering the volume by using 100mL of trichloromethane; the solution was diluted with chloroform to give standard solutions of 0.05mg/mL, 0.10mg/mL, 0.50mg/mL, 1.00mg/mL, 2.00mg/mL, and 5.00mg/mL, respectively.
Preferably, the gas chromatography conditions further comprise:
sample introduction temperature: 250 ℃;
detector temperature: 275 ℃;
the sample volume is 1 mu L;
the split ratio of split sample injection is as follows: 20: 1;
carrier gas: helium, preferably at a flow rate of 1.2 mL/min;
preferably, the tail gas flow rate is 10 mL/min;
preferably, the septum purge flow rate is 10 mL/min;
preferably, the initial temperature is 100 ℃ for 0.5min, and is increased from 100 ℃ to 200 ℃ at a rate of 20 ℃/min for 1.5 min.
Preferably, the method for detecting free nicotine in mainstream smoke of the heated non-combustible cigarette comprises the following steps:
(1) preparing a test solution:
trapping total particulate matters of 5 cigarettes in an ISO suction mode by using two serial trapping bottles containing 25mL of trapping solution, oscillating the solution in the two serial trapping bottles for 5min at room temperature, transferring 2mL of the obtained solution, and filtering by using an anhydrous sodium sulfate needle filter;
(2) preparation of standard solutions:
weighing 100mg of nicotine standard into a 50mL container, and metering the volume by using 100mL of trichloromethane; diluting the solution with chloroform to obtain standard solutions with concentrations of 0.05mg/mL, 0.10mg/mL, 0.50mg/mL, 1.00mg/mL, 2.00mg/mL and 5.00mg/mL respectively;
(3) measuring the content of free nicotine in the main stream smoke of the heated non-burning cigarette by adopting a gas chromatography:
injecting the standard solution and the test solution into a gas chromatograph for determination, wherein the gas chromatograph conditions comprise:
a chromatographic column: CP-1301 silica gel column capillary column;
column volume: 30 m.times.0.32 mm.times.1.0 μm;
preferably, the injection temperature is: 250 ℃;
detector temperature: 275 ℃;
the sample volume is 1 mu L;
the split ratio of split sample injection is as follows: 20: 1;
carrier gas: helium at a flow rate of 1.2 mL/min;
preferably, the tail gas flow rate is 10 mL/min;
preferably, the septum purge flow rate is 10 mL/min;
preferably, the initial temperature is 100 ℃ for 0.5min, and is increased from 100 ℃ to 200 ℃ at a rate of 20 ℃/min for 1.5 min.
Compared with the prior art, the method for detecting the content of the free nicotine has the following beneficial effects:
(1) the detection method provided by the invention has short time, and the cycle of detecting the free nicotine in the main stream smoke of the cigarette which is not burnt needs only about 9 minutes;
(2) the detection method provided by the invention saves the processes of vibration extraction and liquid-liquid extraction after the filter disc is collected, and avoids the problems of incomplete extraction and poor liquid-liquid extraction repeatability of the filter disc method; the invention realizes the processes of smoke capture and free nicotine distribution in organic phase and water phase by one-step method, and the distribution process of the free nicotine is performed once every time the cigarette is smoked; the invention also saves the pretreatment time of the sample to be detected, the pretreatment process of the sample to be detected in the prior method needs 3 to 4 hours, and the invention only needs 10 min;
(3) the detection method has the advantages of accurate operation, high sensitivity and good repeatability.
Drawings
Embodiments of the invention are described in detail below with reference to the attached drawing figures, wherein:
FIG. 1 is a flow chart of the detection method of the present invention;
FIG. 2 is a chromatogram of a standard solution in the method for detecting alcohols according to the present invention;
FIG. 3 is a chromatogram of a test solution in the method for detecting alcohols according to the present invention;
FIG. 4 shows the selection of cigarette quantity in step (1) of the alcohol detection method according to the present invention;
FIG. 5 shows the selection of the amount of isopropyl alcohol used in step (1) of the method for detecting alcohols according to the present invention;
FIG. 6 shows the selection of the oscillation time in step (1) of the method for detecting alcohols according to the present invention;
FIG. 7 is a flow chart of a method for detecting phenols according to the present invention;
FIG. 8 is a chromatogram of a standard solution in the method for detecting phenols according to the present invention;
FIG. 9 is a chromatogram of a test solution in the method for detecting phenols according to the present invention;
FIG. 10 shows tandem trap bottles according to the method for detecting phenols of the present invention;
FIG. 11 shows the effect of two trap bottles in series in the method for detecting phenols of the present invention
FIG. 12 shows the effect of the filter and the absorption flask in series according to the method for detecting phenols of the present invention;
FIG. 13 is a flow chart of a method of detecting free nicotine according to the present invention;
FIG. 14 is a chromatogram of a standard solution in a method for detecting free nicotine according to the present invention;
FIG. 15 is a chromatogram of a test solution in a method for detecting free nicotine according to the present invention;
FIG. 16 shows tandem trap vials according to the method of the present invention for detecting free nicotine;
FIG. 17 shows the selection of cigarette quantity in step (1) of the method for detecting free nicotine according to the present invention;
FIG. 18 is a selection of trapping solution usage in step (1) of the method of detecting free nicotine according to the present invention.
Detailed Description
The present invention is described in further detail below with reference to specific embodiments, which are given for the purpose of illustration only and are not intended to limit the scope of the invention.
The experimental procedures in the following examples are conventional unless otherwise specified. The raw materials and reagents used in the following examples are all commercially available products unless otherwise specified.
Reagents and apparatus used in the following examples:
and (3) standard substance: 1, 2-propanediol, glycerol, menthol, dr. ehrenstorfer, germany;
reagent: isopropanol, chromatographic pure, Duksan pure chemicals, Korea;
the experimental water is deionized water of a Milli-Q pure water system;
the instrument comprises the following steps: gas chromatograph-FID detector, agilent;
SM450 linear smoking machines (Cerulean, uk);
electronic analytical balance, sensitivity: 0.0001g, Mettler, Switzerland;
an HY-6 double-layer adjustable-speed oscillator, Guohua electric appliances Limited;
anhydrous sodium sulfate needle filter, 13 mm. times.0.22 μm, Shanghai' an spectral science apparatus Co., Ltd.
O-dihydroxybenzene, p-dihydroxybenzene, phenol, o-cresol, m-cresol, p-cresol, m-dihydroxybenzene, DR company, Germany;
acetonitrile solution, HPLC pure, CNW, germany;
acetic acid solution, HPLC pure, merck, germany;
all the water for experiments is deionized water treated by an ultrapure water instrument;
the instrument comprises the following steps: SM450, 20-channel linear smoking machine;
high performance liquid chromatography, agilent;
fluorescence detector, FLD;
AE163 electronic balance, sensory 0.0001g, Mettler, Switzerland.
Example 1
(1) Preparing a test solution:
collecting total particulate matter of 5 cigarettes by using a Cambridge filter disc under an ISO suction mode, then putting the Cambridge filter disc into a 100mL container, adding 20mL of isopropanol, oscillating for 30min at room temperature, transferring 2mL of solution, and filtering by using an anhydrous sodium sulfate syringe filter;
(2) preparation of standard solutions:
weighing about 1g of 1, 2-propylene glycol, glycerol and menthol respectively into a 100mL container, accurately measuring to 0.0001g, metering volume by isopropanol, shaking up, and storing the obtained solution at 4 deg.C respectively; accurately transferring 0.2mL, 0.5mL, 2.5mL, 5mL, 7.5mL, 10mL, 15mL and 20mL of the above solutions into a 100mL container to obtain standard solutions with concentrations of 0.02mg/mL, 0.05mg/mL, 0.25mg/mL, 0.50mg/mL, 0.75mg/mL, 1.00mg/mL, 1.5mg/mL and 2.00 mg/mL; see table 1;
table 1: concentration of Standard solution (mg/mL) in the detection method of the present invention
(3) And (3) gas chromatograph determination:
the chromatographic conditions were as follows:
a chromatographic column: a fused silica gel column capillary column CP-1301, wherein the length of the column is 30m, the inner diameter of the column is 0.32mm, and the thickness of the membrane is 1 μm;
sample introduction temperature: 250 ℃;
detector temperature: 275 ℃;
the sample volume is 1 mu L;
the split ratio of split sample injection is as follows: 50: 1;
carrier gas: helium, preferably at a flow rate of 0.7 mL/min;
tail blowing: helium or nitrogen with a flow rate of 30 mL/min; hydrogen gas: the flow rate is 40 mL/min; air: the flow rate is 400 mL/min;
the initial temperature is 110 ℃, the temperature is kept for 1min, the temperature is increased from 110 ℃ to 150 ℃ at the speed of 10 ℃/min, the temperature is kept for 3min, and then the temperature is increased from 150 ℃ to 220 ℃ at the speed of 30 ℃/min, and the temperature is kept for 5 min.
(4) Establishment of a standard curve:
measuring the obtained standard solution by using a gas chromatograph to obtain an integrated peak area of the target compound (1, 2-propylene glycol, glycerol and menthol), and establishing a standard curve of the target compound by taking the integrated area of the target compound as a vertical coordinate and the concentration of the target compound as a horizontal coordinate. Using peak area quantification, using peak area (integral) to determine linear regression equation for mass concentration (mg/mL), verifying standard curve equation and correlation coefficient, R2Should not be less than 0.99. The standard curve and detection limit of each compound are shown in table 2;
table 2: standard curves and detection limits in the detection method of the invention
Note: the detection limit is calculated as a 3-fold signal-to-noise ratio (S/N-3)
(5) Methodological inspection of the detection methods described in the present invention
Carrying out standard solution standard addition recovery rate tests of low, medium and high concentration levels on the samples, respectively measuring each sample for 3 times, calculating the recovery rate of the main alcohol compounds (1, 2-propylene glycol, glycerol and menthol) in the detection method and the relative standard deviation of the measured value after adding the standard, and obtaining the results shown in table 3; it can be seen that, at 3 levels of spiking, the average recovery rate of the main alcohol compounds (1, 2-propanediol, glycerol and menthol) in the mainstream smoke detected by the detection method of the invention is 90.6-101.0%; the average relative deviation of the test results of the samples is less than 3.2 percent; the detection method has the advantages of high recovery rate and good repeatability.
Table 3: standard recovery rate investigation (n ═ 3)
(6) Detecting a sample to be tested
Measuring the sample solution of the obtained sample to be measured by using a gas chromatograph, measuring the chromatographic peak area of each compound (1, 2-propylene glycol, glycerol and menthol), substituting the chromatographic peak area into the standard curve, and respectively obtaining the content of the main alcohol compounds (1, 2-propylene glycol, glycerol and menthol) in the sample to be measured, wherein the content is shown in table 4;
table 4: detection results of propylene glycol, glycerol and menthol in mainstream smoke of heated non-burning cigarette
Example 2
(1) Preparing a test solution (same as example 1);
(2) preparation of standard solution (same as example 1);
(3) gas chromatograph (same as example 1);
(4) establishing a standard curve (same as the example 1);
(5) methodology investigation of the detection method of the invention (as in example 1);
(6) detecting a sample to be tested
Measuring the sample solution of the obtained sample to be measured by using a gas chromatograph, measuring the chromatographic peak area of each compound (1, 2-propylene glycol, glycerol and menthol), substituting the chromatographic peak area into the standard curve, and respectively obtaining the content of the main alcohol compounds (1, 2-propylene glycol, glycerol and menthol) in the sample to be measured, wherein the content is shown in table 5;
table 5: detection results of propylene glycol, glycerol and menthol in mainstream smoke of heated non-burning cigarette
Example 3
(1) Preparing a test solution (same as example 1);
(2) preparation of standard solution (same as example 1);
(3) gas chromatograph (same as example 1);
(4) establishing a standard curve (same as the example 1);
(5) methodology investigation of the detection method of the invention (as in example 1);
(6) detecting a sample to be tested
Measuring the sample solution of the obtained sample to be measured by using a gas chromatograph, measuring the chromatographic peak area of each compound (1, 2-propylene glycol, glycerol and menthol), substituting the chromatographic peak area into the standard curve, and respectively obtaining the content of the main alcohol compounds (1, 2-propylene glycol, glycerol and menthol) in the sample to be measured, wherein the content is shown in table 6;
table 6: detection results of propylene glycol, glycerol and menthol in mainstream smoke of heated non-burning cigarette
Example 4
(1) Preparing a test solution (same as example 1);
(2) preparation of standard solution (same as example 1);
(3) gas chromatograph (same as example 1);
(4) establishing a standard curve (same as the example 1);
(5) methodology investigation of the detection method of the invention (as in example 1);
(6) detecting a sample to be tested
Measuring the sample solution of the obtained sample to be measured by using a gas chromatograph, measuring the chromatographic peak area of each compound (1, 2-propylene glycol, glycerol and menthol), substituting the chromatographic peak area into the standard curve, and respectively obtaining the content of the main alcohol compounds (1, 2-propylene glycol, glycerol and menthol) in the sample to be measured, wherein the content is shown in table 7;
table 7: detection results of propylene glycol, glycerol and menthol in mainstream smoke of heated non-burning cigarette
Example 5: selection of cigarette quantity in the detection method of the invention
As can be seen from FIG. 4, the number of cigarettes in step (1) of the detection method of the present invention is 3-7, preferably 5.
Example 6: selection of the amount of isopropyl alcohol used in step (1) of the detection method of the present invention
As can be seen from FIG. 5, the amount of isopropyl alcohol used in step (1) of the detection method of the present invention was 20 ml.
Example 7: selection of oscillation time in step (1) of the detection method of the present invention
As can be seen from FIG. 6, the oscillation time in step (1) of the detection method of the present invention is 20 to 35min, preferably 30 min.
Example 8
(1) Preparing a test solution:
collecting total particulate matters of 5 cigarettes in an ISO suction mode by using two serial collection bottles containing 25mL of collection solution, oscillating the solution in the two serial collection bottles for 5min at room temperature, transferring 2mL of the obtained solution, and filtering the solution by using a 0.22-micron water-phase filter membrane;
FIG. 11 shows the effect of two trap bottles in tandem in the assay of the invention; FIG. 12 shows the effect of the filter and the absorption flask in series in the detection method of the present invention, and the results show that the effect of using two trapping flasks in series is better than the effect of using the filter to trap and add the absorption flasks.
(2) Preparation of standard solutions:
respectively adding 100mg of o-dihydroxybenzene, 100mg of p-dihydroxybenzene, 100mg of phenol, 50mg of o-cresol, 50mg of m-cresol, 50mg of p-cresol and 20mg of m-dihydroxybenzene into a 50mL container, adding 30mL of organic solvent until the o-cresol, the m-cresol, the p-cresol and the m-dihydroxybenzene are completely dissolved, transferring the mixture into the 100mL container, fixing the volume by the organic solvent, taking 10mL to 100mL of the obtained solution, and fixing the volume by the organic solvent to be used as a primary standard solution; then taking the primary standard solution in a container of 10mL to 100mL, and fixing the volume by using an organic solvent to obtain a secondary standard solution; respectively taking 1 mL, 2mL and 5mL of the obtained secondary standard solution and 1 mL, 2mL to 50mL of the obtained primary standard solution, and fixing the volume by using an organic solvent; respectively obtaining para-dihydroxybenzene standard solutions with the concentrations of 0.25 mug/mL, 0.50 mug/mL, 1.25 mug/mL, 2.51 mug/mL, 5.02 mug/mL and 12.54 mug/mL; m-dihydroxybenzene standard solution with concentration of 0.07. mu.g/mL, 0.13. mu.g/mL, 0.34. mu.g/mL, 0.67. mu.g/mL, 1.34. mu.g/mL, 3.35. mu.g/mL; ortho-diphenol standard solutions with concentrations of 0.36. mu.g/mL, 0.71. mu.g/mL, 1.78. mu.g/mL, 3.57. mu.g/mL, 7.13. mu.g/mL, 17.83. mu.g/mL; phenol standard solutions with concentrations of 0.26. mu.g/mL, 0.53. mu.g/mL, 1.32. mu.g/mL, 2.64. mu.g/mL, 5.28. mu.g/mL, 13.19. mu.g/mL; m-cresol standard solutions with concentrations of 0.14. mu.g/mL, 0.28. mu.g/mL, 0.71. mu.g/mL, 1.42. mu.g/mL, 2.83. mu.g/mL, 7.08. mu.g/mL; o-cresol standard solutions at concentrations of 0.24. mu.g/mL, 0.48. mu.g/mL, 1.21. mu.g/mL, 2.42. mu.g/mL, 4.85. mu.g/mL, 12.12. mu.g/mL;
(3) determining the content of phenolic compounds in the main stream smoke of the heated non-burning cigarette by adopting a high performance liquid chromatography:
injecting the standard solution and the test solution into a high performance liquid chromatograph for determination, wherein the conditions of the high performance liquid chromatograph comprise:
a chromatographic column:
explosive E2 column;
mobile phase: acetonitrile-water solution;
the inner diameter of the chromatographic column is 250mm × 4.6.6 mm,
the particle size of the filler is 5 mu m;
column temperature of the chromatographic column: 20-40 ℃, preferably 30 ℃;
the flow rate of the chromatographic column is 1.0 ml/min;
the sample introduction volume is as follows: 10 mu L of the solution;
the volume ratio of the water to the acetonitrile solution is 50: 50.
(4) Establishment of a standard curve:
the method comprises the steps of preparing 6 standard solutions of phenolic compounds by using o-dihydroxybenzene, p-dihydroxybenzene, phenol, o-cresol, m-cresol, p-cresol and m-dihydroxybenzene as detection indexes, carrying out high performance liquid chromatography analysis, carrying out regression analysis on corresponding concentrations of the phenolic compound target substances by using chromatographic peak areas of the phenolic compound target substances to obtain a standard curve, a regression equation and correlation coefficients of the standard curve, and calculating a detection limit by using the signal-to-noise ratio of the standard solution with the lowest concentration as 3. As can be seen from Table 8, the chromatographic conditions adopted lead the chromatographic peaks of the 6 phenolic compounds to be well separated and have good correlation, and the detection limit is between 0.005 mu g/cig and 0.021 mu g/cig.
Table 8: standard curve and limit of detection of said phenolic compounds
Note: the detection limit was calculated as 3 times the signal-to-noise ratio (S/N-3).
(5) Calculation of measurement results of phenolic compounds in mainstream smoke of heated non-burning cigarettes
And (3) carrying out quantitative analysis on the phenolic compound by an external standard method, namely carrying out regression analysis on the corresponding concentration of the target phenolic compound by using the chromatographic peak area of the phenolic compound to obtain a standard curve. And (3) measuring a sample to be detected, measuring the chromatographic peak area of the detected target phenolic compound, substituting the chromatographic peak area into the standard curve, and respectively obtaining the contents of o-dihydroxybenzene, p-dihydroxybenzene, phenol, o-cresol, m-cresol, p-cresol and m-dihydroxybenzene in the sample to be detected.
The m-cresol and the p-cresol can not be completely separated by the current technical means, and appear in a chromatogram map according to the situation of a chromatographic peak, so that the sum of the two compounds is measured without being measured independently.
And (3) calculating the result, wherein the formula for calculating phenolic compounds in the mainstream smoke of the cigarette is as follows:
in the formula:
m-the transmission quantity of the phenolic components in the main stream smoke of each cigarette, and the unit is microgram per cigarette (microgram/cig);
a-concentration of phenolic compounds in the extracted sample (. mu.g/mL);
50-volume of extraction solution (mL);
n-the number of cigarettes smoked per test (cig);
(6) methodological inspection of the detection methods described in the present invention
The samples of the invention are subjected to standard solution standard adding recovery rate tests with different concentration levels of high, medium and low (2 mug/cig, 1 mug/cig and 0.5 mug/cig), each sample is respectively measured for 5 times, the recovery rate of the main phenolic compounds in the main stream smoke of various cigarettes of the method and the relative standard deviation of the measured value after the standard adding are calculated, and the results are shown in a table 9; as can be seen from Table 9, the average recovery rate of the main phenolic compounds in the mainstream smoke of the cigarettes detected by the method is 91.5-103.9% at 3 standard adding levels; the average relative deviation of the test result is less than 3.2 percent, which shows that the method of the invention has higher recovery rate and better repeatability
Table 9: standard recovery rate investigation (n ═ 5)
(7) Detecting a sample to be tested
Carrying out regression analysis on the corresponding concentration of the phenolic compound target by using the chromatographic peak area of the phenolic compound target to obtain a standard curve; and (3) measuring the prepared sample to be detected, measuring the chromatographic peak area of the target substance of the detected phenolic compound, substituting the chromatographic peak area into the standard curve to respectively obtain the contents of the o-dihydroxybenzene, the p-dihydroxybenzene, the phenol, the o-cresol, the m-cresol, the p-cresol and the m-dihydroxybenzene in the sample to be detected, and the result is shown in the table 10.
Table 10: detection result of phenolic compounds in mainstream smoke of cigarette without burning during heating
Example 9
(1) Preparing a test solution (same as example 8);
(2) preparation of standard solution (same as example 8);
(3) high performance liquid chromatography (same as example 8);
(4) establishing a standard curve (same as the example 8);
(5) calculating the measurement result of the phenolic compounds in the mainstream smoke of the cigarette without burning (same as the example 8);
(6) methodology of the detection method of the present invention (same as example 8);
(7) detecting a sample to be tested
Carrying out regression analysis on the corresponding concentration of the phenolic compound target by using the chromatographic peak area of the phenolic compound target to obtain a standard curve; and (3) measuring the prepared sample to be detected, measuring the chromatographic peak area of the target substance of the detected phenolic compound, substituting the chromatographic peak area into the standard curve to respectively obtain the contents of the o-dihydroxybenzene, the p-dihydroxybenzene, the phenol, the o-cresol, the m-cresol, the p-cresol and the m-dihydroxybenzene in the sample to be detected, and the result is shown in the table 11.
Table 11: detection result of phenolic compounds in mainstream smoke of cigarette without burning during heating
Example 10
(1) Preparing a test solution (same as example 8);
(2) preparation of standard solution (same as example 8);
(3) gas chromatograph assay (same as example 8);
(4) establishing a standard curve (same as the example 8);
(5) calculating the measurement result of the phenolic compounds in the mainstream smoke of the cigarette without burning (same as the example 8);
(6) methodology of the detection method of the present invention (same as example 8);
(7) detecting a sample to be tested
Carrying out regression analysis on the corresponding concentration of the phenolic compound target by using the chromatographic peak area of the phenolic compound target to obtain a standard curve; and (3) measuring the prepared sample to be detected, measuring the chromatographic peak area of the target substance of the detected phenolic compound, substituting the chromatographic peak area into the standard curve to respectively obtain the contents of the o-dihydroxybenzene, the p-dihydroxybenzene, the phenol, the o-cresol, the m-cresol, the p-cresol and the m-dihydroxybenzene in the sample to be detected, and the result is shown in the table 12.
Table 12: detection result of phenolic compounds in mainstream smoke of cigarette without burning during heating
Example 11
(1) Preparing a test solution (same as example 8);
(2) preparation of standard solution (same as example 8);
(3) gas chromatograph assay (same as example 8);
(4) establishing a standard curve (same as the example 8);
(5) calculating the measurement result of the phenolic compounds in the mainstream smoke of the cigarette without burning (same as the example 8);
(6) methodology of the detection method of the present invention (same as example 8);
(7) detecting a sample to be tested
Carrying out regression analysis on the corresponding concentration of the phenolic compound target by using the chromatographic peak area of the phenolic compound target to obtain a standard curve; and (3) measuring the prepared sample to be detected, measuring the chromatographic peak area of the target substance of the detected phenolic compound, substituting the chromatographic peak area into the standard curve to respectively obtain the contents of the o-dihydroxybenzene, the p-dihydroxybenzene, the phenol, the o-cresol, the m-cresol, the p-cresol and the m-dihydroxybenzene in the sample to be detected, and obtaining the result shown in the table 13.
Table 13: detection result of phenolic compounds in mainstream smoke of cigarette without burning during heating
Example 12
(1) Preparing a test solution:
trapping total particulate matters of 5 cigarettes in an ISO suction mode by using two serial trapping bottles containing 25mL of trapping solution, oscillating the solution in the two serial trapping bottles for 5min at room temperature, transferring 2mL of the obtained solution, and filtering by using an anhydrous sodium sulfate needle filter;
(2) preparation of standard solutions:
weighing 100mg of nicotine standard substance into a 50mL container, and metering volume by trichloromethane; diluting the solution with chloroform to obtain standard solutions with concentrations of 0.05mg/mL, 0.10mg/mL, 0.50mg/mL, 1.00mg/mL, 2.00mg/mL and 5.00mg/mL respectively;
(3) measuring the content of free nicotine in the main stream smoke of the heated non-burning cigarette by adopting a gas chromatography:
injecting the standard solution and the test solution into a gas chromatograph for determination, wherein the gas chromatograph conditions comprise:
a chromatographic column: CP-1301 silica gel column capillary column;
column volume: 30 m.times.0.32 mm.times.1.0 μm;
sample introduction temperature: 250 ℃;
detector temperature: 275 ℃;
the sample volume is 1 mu L;
the split ratio of split sample injection is as follows: 20: 1;
carrier gas: helium at a flow rate of 1.2 mL/min;
the flow rate of the tail blowing gas is 10 mL/min;
the flow rate of purging the shock insulator is 10 mL/min;
the initial temperature was 100 deg.C, held for 0.5min, increased from 100 deg.C to 200 deg.C at a rate of 20 deg.C/min, and held for 1.5 min.
(4) Calculation of free nicotine determination results in mainstream smoke of heated non-burning cigarettes
And (3) carrying out quantitative analysis on the free nicotine by an external standard method, namely carrying out regression analysis on the corresponding concentration of the target free nicotine by using the chromatographic peak area of the target free nicotine to obtain a standard curve. And (3) measuring the prepared sample to be detected, detecting the chromatographic peak area of the detected target free nicotine, substituting the chromatographic peak area into the standard curve, and respectively obtaining the content of the free nicotine in the sample.
And (3) calculating results, wherein a calculation formula of free nicotine in the mainstream smoke of the heated non-combustible cigarette is as follows:
in the formula:
m-the content of free nicotine in the mainstream smoke of each cigarette, with the unit of microgram per cigarette (microgram/cig);
a-concentration of free nicotine in the extracted sample (. mu.g/mL);
50-volume of extraction solution (mL);
n-the number of cigarettes smoked per test (cig);
(4) establishment of a standard curve:
preparing a working standard solution by taking nicotine as a detection index, performing gas chromatography analysis, performing regression analysis on the corresponding concentration of the target by using the chromatographic peak area of the target to obtain a standard curve, a regression equation and a correlation coefficient of the standard curve, and calculating the detection limit by using the signal-to-noise ratio of the standard solution with the lowest concentration as 3. As can be seen from Table 14, the chromatographic conditions employed gave better separation of the free nicotine chromatographic peaks and a better correlation, with a detection limit of 5. mu.g/cig.
Table 14: standard curves and detection limits in the detection method of the invention
Note: the detection limit is calculated as a 3-fold signal-to-noise ratio (S/N-3)
(5) Calculation of free nicotine determination results in mainstream smoke of heated non-burning cigarettes
And (3) carrying out quantitative analysis on the free nicotine by an external standard method, namely carrying out regression analysis on the corresponding concentration of the target free nicotine by using the chromatographic peak area of the target free nicotine to obtain a standard curve. And (3) measuring the prepared sample to be detected, detecting the chromatographic peak area of the detected target free nicotine, substituting the chromatographic peak area into the standard curve, and respectively obtaining the content of the free nicotine in the sample.
And (3) calculating results, wherein a calculation formula of free nicotine in the mainstream smoke of the heated non-combustible cigarette is as follows:
in the formula:
m-the content of free nicotine in the mainstream smoke of each cigarette, with the unit of microgram per cigarette (microgram/cig);
a-concentration of free nicotine in the extracted sample (. mu.g/mL);
50-volume of extraction solution (mL);
n-the number of cigarettes smoked per test (cig);
(6) methodological inspection of the detection methods described in the present invention
The samples were subjected to standard solution spiking recovery tests of different concentration levels of high, medium and low (0.20mg/cig, 0.10mg/cig, 0.05mg/cig), each sample was measured 5 times, the recovery of free nicotine in the mainstream smoke of various cigarettes of the method and the relative standard deviation of the measured value after spiking were calculated, and the results are shown in table 15. As can be seen from Table 15, the average recovery rate of free nicotine in the mainstream smoke of cigarettes detected by the method is between 98.3% and 99.7% at 3 standard adding levels. The average relative deviation of the test results of the samples is less than 3.1%; the method has high recovery rate and good repeatability.
Table 15: standard recovery rate investigation (n ═ 5)
(7) Detecting a sample to be tested
And carrying out regression analysis on the corresponding concentration of the target compound according to the chromatographic peak area of the target compound to obtain a standard curve. Measuring the prepared sample A to be detected to obtain the chromatographic peak area of the detected target compound, substituting the chromatographic peak area into the standard curve to respectively obtain the content of free nicotine in the sample to be detected, and obtaining the result shown in Table 16
Table 16: detection result of free nicotine in mainstream smoke of heated non-combustible cigarette (sample A to be detected)
Example 13
(1) Preparing a test solution (same as example 12);
(2) preparation of standard solution (same as example 12);
(3) high performance liquid chromatography (same as example 12);
(4) establishing a standard curve (same as the example 12);
(5) calculating the measurement result of free nicotine in the main stream smoke of the cigarette without burning (same as example 12);
(6) methodology of the detection method of the present invention (same as example 12);
(7) detecting a sample to be tested
And carrying out regression analysis on the corresponding concentration of the target compound according to the chromatographic peak area of the target compound to obtain a standard curve. Measuring a sample B to be measured of another prepared brand of cigarette which is heated and does not burn, measuring the chromatographic peak area of the detected target compound, substituting the chromatographic peak area into a standard curve, and respectively obtaining the content of free nicotine in the sample to be measured, wherein the result is shown in a table 17;
table 17: detection result of free nicotine in mainstream smoke of heated non-combustible cigarette (sample B to be detected)
Example 14
(1) Preparing a test solution (same as example 12);
(2) preparation of standard solution (same as example 12);
(3) high performance liquid chromatography (same as example 12);
(4) establishing a standard curve (same as the example 12);
(5) calculating the measurement result of free nicotine in the main stream smoke of the cigarette without burning (same as example 12);
(6) methodology of the detection method of the present invention (same as example 12);
(7) detecting a sample to be tested
And carrying out regression analysis on the corresponding concentration of the target compound according to the chromatographic peak area of the target compound to obtain a standard curve. Measuring a sample C to be measured of another prepared brand of cigarette which is heated and does not burn, measuring the chromatographic peak area of the detected target compound, substituting the chromatographic peak area into a standard curve, and respectively obtaining the content of free nicotine in the sample to be measured, wherein the result is shown in a table 18;
table 18: detection result of free nicotine in mainstream smoke of heated non-burning cigarette (sample C to be detected)
Example 15
(1) Preparing a test solution (same as example 12);
(2) preparation of standard solution (same as example 12);
(3) high performance liquid chromatography (same as example 12);
(4) establishing a standard curve (same as the example 12);
(5) calculating the measurement result of free nicotine in the main stream smoke of the cigarette without burning (same as example 12);
(6) methodology of the detection method of the present invention (same as example 12);
(7) detecting a sample to be tested
And carrying out regression analysis on the corresponding concentration of the target compound according to the chromatographic peak area of the target compound to obtain a standard curve. Measuring a sample D to be measured of another prepared brand of cigarette which is not combusted by heating, measuring the chromatographic peak area of the detected target compound, substituting the chromatographic peak area into a standard curve, and respectively obtaining the content of free nicotine in the sample to be measured, wherein the result is shown in a table 19;
table 19: detection node for free nicotine in mainstream smoke of heated non-combustible cigarette (sample D to be detected)Fruit
Example 16: selection of cigarette quantity in the detection method of the invention
As can be seen from fig. 17, in the step (1) of the detection method of the present invention, the number of the cigarettes is 3 to 7, preferably 5.
Example 17: selection of the amount of trapping solution to be used in the detection method of the present invention in the step (1)
As can be seen from FIG. 18, the amount of the capturing solution used in the step (1) of the detection method of the present invention was 25 mL.
In conclusion, the above description of the embodiments of the present invention is not intended to limit the present invention, and those skilled in the art can make various changes or modifications according to the present invention without departing from the spirit of the present invention, which falls within the scope of the appended claims.
Claims (3)
1. A detection method of alcohol compounds in mainstream smoke of a heated non-burning cigarette comprises the following steps:
(1) preparing a test solution;
collecting total particulate matters of 5 cigarettes by using a Cambridge filter disc in an ISO suction mode, then putting the Cambridge filter disc into 20mL of isopropanol in a 100mL container, oscillating for 30min at room temperature, transferring 2mL of extraction solution, and filtering by using an anhydrous sodium sulfate needle filter to obtain an alcohol compound;
(2) preparing a standard solution;
(3) measuring the content of alcohol compounds in the main stream smoke of the heated non-burning cigarette by adopting a gas chromatography; wherein the gas chromatography conditions comprise:
a chromatographic column: the CP-1301 silica gel column capillary column has the column length of 30m, the column inner diameter of 0.32mm and the film thickness of 1 μm;
sample introduction temperature: 250 ℃;
detector temperature: 275 ℃;
the sample volume is 1 mu L;
the split ratio of split sample injection is as follows: 50: 1;
carrier gas: helium at a flow rate of 0.7 mL/min;
tail blowing: helium or nitrogen with a flow rate of 30 mL/min;
hydrogen gas: the flow rate is 40 mL/min;
air: the flow rate is 400 mL/min;
the initial temperature is 110 ℃, the temperature is kept for 1min, the temperature is increased from 110 ℃ to 150 ℃ at the speed of 10 ℃/min, the temperature is kept for 3min, and then the temperature is increased from 150 ℃ to 220 ℃ at the speed of 30 ℃/min, and the temperature is kept for 5 min;
the alcohol compounds are 1, 2-propylene glycol, glycerol and menthol.
2. The detection method according to claim 1, wherein in the step (2), the preparing of the standard solution comprises: 1g of 1, 2-propylene glycol, glycerol and menthol are respectively taken, and the volume is determined by an organic solvent which is isopropanol.
3. The detection method according to claim 1, wherein in the step (2), the preparing of the standard solution comprises:
weighing 1g of 1, 2-propylene glycol, glycerol and menthol respectively into a 100mL container, fixing the volume by isopropanol, shaking up, and storing the obtained solution at 4 ℃; the solutions were transferred into 100mL containers at a concentration of 0.2mL, 0.5mL, 2.5mL, 5mL, 7.5mL, 10mL, 15mL, or 20mL to give standard solutions at a concentration of 0.02mg/mL, 0.05mg/mL, 0.25mg/mL, 0.50mg/mL, 0.75mg/mL, 1.00mg/mL, 1.5.mg/mL, or 2.00mg/mL, respectively.
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| CN109557229A (en) * | 2018-11-20 | 2019-04-02 | 湖北中烟工业有限责任公司 | A kind of measuring method of cigarette menthol content in quick-fried pearl |
| CN109975452A (en) * | 2019-02-15 | 2019-07-05 | 云南中烟工业有限责任公司 | Heat the measuring method of menthol in the cigarette core substrate that do not burn |
| CN111122749B (en) * | 2020-01-07 | 2023-01-13 | 湖北中烟工业有限责任公司 | Separation method and detection method for aroma components in smoke of heated non-burning cigarette |
| CN112505227A (en) * | 2020-12-29 | 2021-03-16 | 广西中烟工业有限责任公司 | Analysis method for simultaneously determining 11 components in electronic cigarette liquid |
| CN113109472B (en) * | 2021-04-13 | 2023-03-14 | 中国烟草总公司郑州烟草研究院 | Novel method for simultaneously measuring main chemical components and phenolic harmful components in smoke exhaled by tobacco products |
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| CN101169397B (en) * | 2007-11-20 | 2012-02-01 | 川渝中烟工业公司 | Method for determining propane diols and glyceryl alcohol in cigarette main flue |
| CN102353736B (en) * | 2011-07-14 | 2013-05-15 | 浙江中烟工业有限责任公司 | Method for determining menthol in cigarette filter rod |
| CN103698431B (en) * | 2013-12-27 | 2015-09-09 | 云南烟草科学研究院 | The assay method of glycerine, 1,2-PD in a kind of cigarette, electronic cigarette and low temperature cigarette |
| CN104634914A (en) * | 2015-02-16 | 2015-05-20 | 国家烟草质量监督检验中心 | Method for determining content of 1,2-propanediol, propanetriol and triethylene glycol in suction aerosol of electronic cigarette |
| CN104698117B (en) * | 2015-03-20 | 2016-08-31 | 中国烟草总公司郑州烟草研究院 | Assay method while nicotine, 1,2-propylene glycol and glycerol in a kind of electronic cigarette flue gas |
| CN107490636B (en) * | 2017-08-09 | 2020-05-15 | 国家烟草质量监督检验中心 | Method for measuring 8 carbonyl compounds in mainstream smoke of heated non-combustible cigarette |
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