CN111289677A - Method for measuring spicy components in main stream smoke of cigarette - Google Patents
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Abstract
The invention relates to a method for measuring spicy components in main stream smoke of cigarettes, belonging to the technical field of aroma component detection. The method for measuring the spicy components in the mainstream smoke of the cigarettes comprises the following steps: (1) extraction: collecting cigarette mainstream smoke particulate matters, extracting the cigarette mainstream smoke particulate matters by using acetone, and taking supernate as a sample to be detected; (2) detecting the content by an internal standard method: and (3) carrying out gas chromatography-mass spectrometry combined analysis on the sample to be detected obtained in the step (1), and detecting the content of the spicy component by an internal standard method. The method has the advantages of rapid detection, high sensitivity, good selectivity and high accuracy, and can simultaneously determine 24 spicy components in the main stream smoke of the cigarette.
Description
Technical Field
The invention relates to a method for measuring spicy components in main stream smoke of cigarettes, belonging to the technical field of aroma component detection.
Background
In the industry standard YCT 497 and 2014 Chinese style sensory evaluation method, the spicy flavor is used as a component of the cigarette aroma style and is one of the important aroma notes of the cigarette. The spicy components in the cigarette smoke can be the inherent components of tobacco leaves, and can also be energy sources in the burning or artificial addition of the tobacco leaves. The composition modes of the spicy components in the smoke of different cigarettes may be different, which is an important material basis that various cigarette products may have different spicy expressions. The method inspects the key component composition with the spicy characteristic in the smoke of various cigarettes, is favorable for deepening the understanding of the substance basis of the spicy characteristic of the smoke, and can provide basic support for pertinently improving the spicy feeling of the cigarettes; and only by focusing the research object on the smoke components with the spicy characteristics, a good analysis effect can be obtained aiming at the spicy characteristic substance basis.
More than 6000 components exist in cigarette smoke, and the relation between aroma characteristics and chemical structures is not predicted by a generally effective theoretical model, so that the acquisition of spicy characteristic components existing in the cigarette smoke can be completed only by scientific screening and systematic component aroma characteristic evaluation. At present, reports specially aiming at an analysis method of spicy components in cigarette smoke are rarely seen, and the quantity of the spicy components related in related smoke aroma component analysis documents is generally less. Therefore, it is necessary to develop a new method for measuring the spicy components in the cigarette smoke more comprehensively.
Disclosure of Invention
The invention aims to provide a method for measuring spicy components in main stream smoke of cigarettes, which has the advantages of quick detection, high sensitivity, good selectivity and high accuracy and can simultaneously measure 24 spicy components in the main stream smoke of the cigarettes.
The technical scheme of the invention is as follows:
a method for measuring spicy components in main stream smoke of cigarettes comprises the following steps:
(1) extraction of
Collecting cigarette mainstream smoke particulate matters, extracting the cigarette mainstream smoke particulate matters by using acetone, and taking supernate as a sample to be detected;
(2) content detection by internal standard method
Carrying out gas chromatography-mass spectrometry combined analysis on the sample to be detected obtained in the step (1), and detecting the content of the spicy components by an internal standard method;
the spice component is one or more of anisole, 2-methylanisole, 6-methyl-3, 5-pentadiene-2-ketone, 2-methylbenzofuran, 4-allyl anisole, α -terpineol, p-xylylene ether, carvone, 4-isopropylbenzaldehyde, 4- (2-furyl) -3-butene-2-ketone, methyl eugenol, p-methoxybenzaldehyde, cinnamaldehyde, dihydroeugenol, eugenol, thymol, isoeugenol methyl ether, carvacrol, cinnamyl alcohol, p-allylphenol, isoeugenol, 4-allyl-2, 6-dimethoxyphenol, syringaldehyde and nipagin propyl ester.
The method for measuring the spicy components in the main stream smoke of the cigarettes can simultaneously measure the content of 24 spicy components in the main stream smoke of the cigarettes by extracting particulate matters of the main stream smoke of the cigarettes by using acetone and combining a gas chromatography-mass spectrometry combined method, has the advantages of quick detection, high sensitivity, good selectivity and high accuracy, can simultaneously measure 24 spicy components in the main stream smoke of the cigarettes, and is suitable for detecting the spicy components in the main stream smoke of the cigarettes, such as anisole, 2-methyl anisole, 6-methyl-3, 5-pentadiene-2-one, 2-methyl benzofuran, 4-allyl anisole, α -terpineol, p-dimethyl ether, carvone, 4-isopropyl benzaldehyde, 4- (2-furyl) -3-butene-2-one, methyl eugenol, p-methoxybenzaldehyde, cinnamaldehyde, dihydroeugenol, eugenol, thymol, isoeugenol methyl ether, carvacrol, cinnamyl alcohol, p-allyl phenol, isoeugenol, 4-allyl phenol, 4-2, 6-dimethoxyphenol, eugenol and propylparaben.
It should be understood that the method for determining the spicy component in the mainstream smoke of the cigarette of the invention can detect one or more of 24 spicy components means that for a particulate matter containing the 24 spicy components, the method can simultaneously detect 24 spicy components such as anisole, 2-methylanisole, 6-methyl-3, 5-pentadiene-2-one, 2-methylbenzofuran, 4-allylanisole, α -terpineol, p-xylylene ether, carvone, 4-isopropylbenzaldehyde, 4- (2-furyl) -3-buten-2-one, methyl eugenol, p-methoxybenzaldehyde, cinnamaldehyde, dihydroeugenol, eugenol, thymol, iso-eugenol methyl ether, carvacrol, cinnamyl alcohol, p-allylphenol, iso-eugenol, 4-allyl-2, 6-dimethoxyphenol, syringaldehyde and nipagin propyl paraben, however, if the spicy component in the particulate matter only contains some of the 24 spicy components, the method can detect only some of the spicy components in the mainstream smoke of the cigarette, the cigarette if the spicy components are detected, the method can detect only the spicy components such as 2-methylanisole, 3-octylphenol, and the cigarette mainstream smoke of the particulate matter, the cigarette can detect only such as p-methoxybenzaldehyde, and the octoxybenzaldehyde.
The collection mode of the particulate matters in the mainstream smoke of the cigarettes is not limited, and the conventional collection mode in the field can be adopted. Preferably, in the step (1), the collection of the particulate matters in the mainstream smoke of the cigarette is realized by the following steps: and (3) trapping particulate matters in the main stream smoke of the cigarettes by using a Cambridge filter. Every two Cambridge filter sheets can trap particulate matters of the main stream smoke of 10 cigarettes.
The extraction method is not limited, and can be a conventional extraction method in the field, preferably, in the step (1), the extraction is performed at room temperature by shaking, and the shaking extraction time is 20-40 min.
The room temperature refers to indoor temperature, such as 20-30 ℃.
Preferably, the internal standard used in the internal standard method is styrofoam propionate. The styrallyl propionate is used as an internal standard substance, and the accuracy of a detection result is improved.
For the internal standard method, the internal standard substance is added into the sample to be detected before detection, the specific time for adding the internal standard substance is not limited, and preferably, in the step (1), the acetone solution containing the internal standard substance is used for extracting the particulate matters of the mainstream smoke of the cigarettes to obtain the sample to be detected; or extracting the cigarette mainstream smoke particulate matter by using acetone, and then adding an internal standard substance to obtain the sample to be detected.
Preferably, the concentration of the internal standard in the extract is 0.1-0.2. mu.g/mL. The concentration of the internal standard substance is 0.1-0.2 mug/mL, so that the concentration is between the highest concentration and the lowest concentration of the measured spicy component, and the quantitative result is accurate.
Preferably, in the step (1), the amount of acetone is: and each 10 cigarettes of main stream smoke particle phase substances are collected to correspond to 10-50 mL of acetone.
Preferably, in the step (2), the gas chromatography conditions in the gas chromatography-mass spectrometry are as follows: a chromatographic column: DB-WAXETR, specification 60m × 0.25mm × 0.25 μm; carrier gas: he; column flow rate: 1 mL/min; sample inlet temperature: 250 ℃; temperature programming: keeping the temperature at 50 ℃ for 0min, heating to 100 ℃ at the heating rate of 10 ℃/min, keeping the temperature for 0min, heating to 250 ℃ at the heating rate of 3 ℃/min, and keeping the temperature for 20 min; no split mode.
Preferably, in the step (2), the conditions of mass spectrum in the gas chromatography-mass spectrometry are as follows: GC/MS transmission line temperature: 250 ℃, EI ion source temperature: 230 ℃, quadrupole temperature: 150 ℃; EI ionization energy: 70 eV; scanning mode: an ion scan is selected.
It is understood that the quantitative ion information and corresponding retention times for the spice components anisole, 2-methylanisole, 6-methyl-3, 5-pentadiene-2-one, 2-methylbenzofuran, 4-allylanisole, α -terpineol, p-xylylene ether, carvone, 4-isopropylbenzaldehyde, 4- (2-furyl) -3-buten-2-one, methyl eugenol, p-methoxybenzaldehyde, cinnamaldehyde, dihydroeugenol, eugenol, thymol, iso-eugenol methyl ether, carvacrol, cinnamyl alcohol, p-allylphenol, iso-eugenol, 4-allyl-2, 6-dimethoxyphenol, syringaldehyde, propylparaben, and the internal standard styrofoam propionate are shown in table 1.
Quantitative ion information of 124 spicy components and internal standard styrofoam propionate in table
It should be understood that, in the method for determining a spicy component in mainstream smoke of a cigarette, a gas chromatography-mass spectrometry combined analysis is used for detecting by an internal standard quantitative method, an internal standard substance (styrofoam propionate) with a known concentration and each spicy component with a known gradient concentration are mixed to prepare a standard working solution, then, internal standard method quantification is adopted, the ratio of the peak areas of the spicy component in the standard working solution and the quantitative ion peak area of the internal standard substance is taken as a horizontal coordinate, the ratio of the spicy component in the standard working solution and the internal standard substance concentration is taken as a horizontal coordinate, a regression equation is drawn, and when a sample to be determined with an unknown concentration is determined, the concentration of each spicy component in the sample to be determined can be obtained by combining the regression equation according to the relative peak areas of the sample to be determined and the internal standard substance with the known concentration.
Specifically, in the internal standard quantitative method detection, the concentration of 24 octyl components and 1 internal standard substance in the used standard working solution is acetone, the concentration of the internal standard substance styrofol in all the standard working solutions is 0.1 mu g/mL, the concentration of the anisole and the tereptadiol in the standard working solutions is 0.0008 mu g/mL, 0.004 mu g/mL, 0.016 mu g/mL, 0.08 mu g/mL and 0.4 mu g/mL in the standard working solutions, the concentration of the 2 octyl components in each concentration level is equal to each other, the concentration of the 2-methylanisole, 4-allylanisole, thymol and the concentration of the isoeugenol in each standard working solution is 0.0025 mu g/mL, 0.005 mu g/mL, 0.012 mu g/mL, 0.025 mu g/mL, and 0.05 mu g/mL in each concentration level, the concentration of the 4-allylanisole is equal to each other, the concentration of the methyl ether, the 0.0025 mu g/mL, 0.005 mu g/mL, 0.012 mu g/mL, 0.025 mu g/mL, 0.8-24 mu g/mL, the concentration of the eugenol in each standard working solution is equal to each concentration of cinnamyl aldehyde, the concentration of the upper working solution is 0.05 mu g/mL, the concentration of the upper octophenol, the lower standard working solution is equal to each concentration of the 2-24 mu g/mL, the lower standard working solution is 0.05 mu g/mL, the concentration of the upper benzaldehyde, the lower standard working solution is 0.8 mu g/mL, the concentration of the upper benzaldehyde, the concentration of the upper working solution is equal to 2-isopropyl benzaldehyde, the lower standard working solution, the concentration of the lower standard working solution is 0.8 mu g/mL, the concentration of the lower solution, the lower standard working solution, the concentration of the upper working solution is equal to each level, the concentration of the lower solution, the upper standard working solution is 0.8 mu g/mL, the lower solution, the lower concentration of the upper concentration of the lower concentration of the upper concentration of the lower solution is 0.8 mu g/mL, the lower concentration of the upper concentration of the lower concentration of.
The SIM diagrams of the solutions containing the internal standard substance and the standard samples of 24 kinds of spicy components (each spicy component concentration corresponds to the standard solution with the lowest concentration level) are shown in fig. 1 and 2, and as can be seen from fig. 1 and 2, the analysis method of the present invention can better separate 24 kinds of spicy components and has better peak shape. In these, 21-1 and 21-2 are peaks corresponding to the cis-trans isomer of sample No. 21.
Table 224 linear ranges and regression equations for spicy ingredients
Drawings
FIG. 1 is a SIM diagram of the standard numbered 1-19 spice components of the present invention;
FIG. 2 is a SIM chart of the numbered 20-24 spice component standard of the present invention;
FIG. 3 is a SIM chart of the spicy components of cigarette mainstream smoke numbers 1-12 of example 1;
FIG. 4 is a SIM chart of the spicy components of cigarette mainstream smoke numbers 13-19 of example 1;
figure 5 is a SIM map of the spicy components of cigarette mainstream smoke numbers 20-24 of example 1.
Detailed Description
The present invention will be further described with reference to the following embodiments.
The specific embodiment of the method for determining the spicy components in the mainstream smoke of the cigarettes comprises the following steps:
example 1
The method for measuring the spicy components in the mainstream smoke of the cigarette comprises the following steps:
(1) smoking the cigarette with the brand number 1 after balancing and screening according to the standard smoking condition specified in YC/T29-1496, trapping 10 cigarette mainstream smoke particulate matters by using two Cambridge filters, placing the Cambridge filters in a 50mL conical flask with a plug and flatly laying the conical flask at the bottom, adding 20mL acetone solution containing 0.1 mug/mL internal standard substance styrallyl propionate, oscillating for 30min at room temperature, and taking 2mL supernatant, namely the sample to be detected.
(2) Detecting the sample to be detected obtained in the step (1) by adopting GC-MS to obtain a selective ion scanning result in a detection time period, wherein a total ion flow diagram is shown in a figure 3, a figure 4 and a figure 5, and as can be seen from the figure 3, the figure 4 and the figure 5, by using the analysis method disclosed by the invention, 24 spicy substances in the sample to be detected can be identified, meanwhile, the ratio of the quantitative ion peak area and the internal standard substance peak area of each detected spicy substance in the figures 3, 4 and 5 can be obtained by integration, the content of the corresponding spicy substance is obtained by combining the ratio with the regression curve in the table 2, the content is multiplied by the volume of the extraction liquid, the volume is divided by the number of cigarettes of the extracted particulate substances to obtain the content of the spicy substance in each cigarette particulate substance, and the cigarette detection result of the brand number 1 is shown in the table 3.
The chromatographic conditions are as follows: a chromatographic column: DB-WAXETR (60m × 0.25mm × 0.25 μm); carrier gas: he; column flow rate: 1 mL/min; sample inlet temperature: 250 ℃; temperature programming: 50 deg.C (0min), 10 deg.C/min → 100 deg.C (0min), 3 deg.C/min → 250 deg.C (20 min); no split mode.
The mass spectrum conditions are as follows: GC/MS transmission line temperature: 250 ℃, EI ion source temperature: 230 ℃, quadrupole temperature: 150 ℃; EI ionization energy: 70 eV; scanning mode: an ion scan is selected, and the time segments are divided according to retention time.
Example 2
The method for measuring the spicy components in the mainstream smoke of the cigarette comprises the following steps:
(1) smoking the cigarette with the brand number 2 after balancing and screening according to the standard smoking condition specified in YC/T29-1496, trapping 10 cigarette mainstream smoke particulate matters by using two Cambridge filters, placing the Cambridge filters in a 50mL conical flask with a plug and flatly laying the conical flask at the bottom, adding 20mL acetone solution containing 0.1 mug/mL internal standard substance styrallyl propionate, oscillating for 30min at room temperature, and taking 2mL supernatant, namely the sample to be detected.
(2) And (3) detecting the sample to be detected obtained in the step (1) by adopting GC-MS, and detecting the content of the spicy component by an internal standard method. The cigarette test results for brand 2 are shown in table 3.
The chromatographic conditions are as follows: a chromatographic column: DB-WAXETR (60m × 0.25mm × 0.25 μm); carrier gas: he; column flow rate: 1 mL/min; sample inlet temperature: 250 ℃; temperature programming: 50 deg.C (0min), 10 deg.C/min → 100 deg.C (0min), 3 deg.C/min → 250 deg.C (20 min); no split mode.
The mass spectrum conditions are as follows: GC/MS transmission line temperature: 250 ℃, EI ion source temperature: 230 ℃, quadrupole temperature: 150 ℃; EI ionization energy: 70 eV; scanning mode: an ion scan is selected, and the time segments are divided according to retention time.
Example 3
The method for measuring the spicy components in the mainstream smoke of the cigarette comprises the following steps:
(1) smoking the cigarette with the brand number 3 after balancing and screening according to the standard smoking condition specified in YC/T29-1496, trapping 10 cigarette mainstream smoke particulate matters by using two Cambridge filters, placing the Cambridge filters in a 50mL conical flask with a plug and flatly laying the conical flask at the bottom, adding 20mL acetone solution containing 0.15 mug/mL internal standard substance styrallyl propionate, oscillating for 30min at room temperature, and taking 2mL supernatant, namely the sample to be detected.
(2) And (3) detecting the sample to be detected obtained in the step (1) by adopting GC-MS, and detecting the content of the spicy component by an internal standard method. The cigarette test results for brand 3 are shown in table 3.
The chromatographic conditions are as follows: a chromatographic column: DB-WAXETR (60m × 0.25mm × 0.25 μm); carrier gas: he; column flow rate: 1 mL/min; sample inlet temperature: 250 ℃; temperature programming: 50 deg.C (0min), 10 deg.C/min → 100 deg.C (0min), 3 deg.C/min → 250 deg.C (20 min); no split mode.
The mass spectrum conditions are as follows: GC/MS transmission line temperature: 250 ℃, EI ion source temperature: 230 ℃, quadrupole temperature: 150 ℃; EI ionization energy: 70 eV; scanning mode: an ion scan is selected, and the time segments are divided according to retention time.
Table 3 detection results of spicy components in cigarette mainstream smoke by methods for measuring spicy components in examples 1 to 3
Note: "-" indicates no detection.
Claims (9)
1. A method for measuring spicy components in main stream smoke of cigarettes is characterized by comprising the following steps:
(1) extraction of
Collecting cigarette mainstream smoke particulate matters, extracting the cigarette mainstream smoke particulate matters by using acetone, and taking supernate as a sample to be detected;
(2) content detection by internal standard method
Carrying out gas chromatography-mass spectrometry combined analysis on the sample to be detected obtained in the step (1), and detecting the content of the spicy components by an internal standard method;
the spice component is one or more of anisole, 2-methylanisole, 6-methyl-3, 5-pentadiene-2-ketone, 2-methylbenzofuran, 4-allyl anisole, α -terpineol, p-xylylene ether, carvone, 4-isopropylbenzaldehyde, 4- (2-furyl) -3-butene-2-ketone, methyl eugenol, p-methoxybenzaldehyde, cinnamaldehyde, dihydroeugenol, eugenol, thymol, isoeugenol methyl ether, carvacrol, cinnamyl alcohol, p-allylphenol, isoeugenol, 4-allyl-2, 6-dimethoxyphenol, syringaldehyde and nipagin propyl ester.
2. The method for determining the spicy component in the mainstream smoke of cigarettes according to claim 1, wherein the internal standard used in the internal standard method is styrofoam propionate.
3. The method for determining the spicy components in the mainstream smoke of the cigarettes according to claim 1, wherein in the step (1), the acetone solution containing the internal standard substance is used for extracting the particulate matters of the mainstream smoke of the cigarettes to obtain the sample to be detected;
or extracting the cigarette mainstream smoke particulate matter by using acetone, and then adding an internal standard substance to obtain the sample to be detected.
4. The method for determining the spicy component in the mainstream smoke of cigarettes according to claim 3, wherein the concentration of the internal standard substance in the extracting solution is 0.1-0.2 μ g/mL.
5. The method for determining the spicy component in the mainstream smoke of cigarettes according to claim 1, wherein in the step (1), the amount of acetone is as follows: and each 10 cigarettes of main stream smoke particle phase substances are collected to correspond to 10-50 mL of acetone.
6. The method for determining the spicy components in the mainstream smoke of the cigarettes according to claim 1, wherein in the step (1), the extraction is performed at room temperature by shaking, and the shaking extraction time is 20-40 min.
7. The method for determining the spicy component in the mainstream smoke of the cigarette according to claim 1, wherein in the step (1), the collection of the particulate matters in the mainstream smoke of the cigarette is realized by the following steps: and (3) trapping particulate matters in the main stream smoke of the cigarettes by using a Cambridge filter.
8. The method for determining the spicy components in the mainstream smoke of the cigarettes according to any one of claims 1 to 7, wherein in the step (2), the conditions of gas chromatography in the gas chromatography-mass spectrometry are as follows:
a chromatographic column: DB-WAXETR, specification 60m × 0.25mm × 0.25 μm; carrier gas: he; column flow rate: 1 mL/min; sample inlet temperature: 250 ℃; temperature programming: keeping the temperature at 50 ℃ for 0min, heating to 100 ℃ at the heating rate of 10 ℃/min, keeping the temperature for 0min, heating to 250 ℃ at the heating rate of 3 ℃/min, and keeping the temperature for 20 min; no split mode.
9. The method for determining the spicy components in the mainstream smoke of the cigarettes according to any one of claims 1 to 7, wherein in the step (2), the conditions of mass spectrum in the gas chromatography-mass spectrometry are as follows:
GC/MS transmission line temperature: 250 ℃, EI ion source temperature: 230 ℃, quadrupole temperature: 150 ℃; EI ionization energy: 70 eV; scanning mode: an ion scan is selected.
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