CN111307961B - Method for simultaneously measuring 10 acid aroma components in main stream smoke of cigarette - Google Patents
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Abstract
The invention discloses a method for simultaneously measuring 10 acid aroma components in main stream smoke of cigarettes. Extracting particulate matters of main stream smoke of cigarettes by using an extracting agent, derivatizing and heating supernate by using a derivatizing agent, detecting a smoke sample by using a gas chromatography-tandem mass spectrum (GC-MS/MS), and simultaneously detecting the contents of 10 acid aroma substances such as formic acid, acetic acid, isovaleric acid, n-valeric acid, 3-methyl-2-butenoic acid, 3-methylvaleric acid, 4-methylvaleric acid, n-hexanoic acid, n-heptanoic acid, benzoic acid and the like by using an internal standard quantitative method. The method focuses on the component with the unique sensory characteristic of acid aroma in the cigarette smoke, eliminates the interference of non-acid aroma organic acid components, has the advantages of quick detection, high sensitivity, good selectivity, high accuracy and the like, and can effectively reflect the composition condition of the main material basis of the acid aroma characteristic of the smoke of different cigarette products.
Description
Technical Field
The invention relates to the technical field of aroma component detection, in particular to a method for simultaneously determining 10 acid aroma components in main stream smoke of cigarettes.
Background
Sour aroma is an aroma characteristic that is widely found in nature, and the taste profile of many fruits, vegetables, pastries, and brewed foods includes a perception of sour aroma. The complex flavor profile provided by cigarette smoke also includes a sour taste sensation. The proper acid aroma can improve the flavor quality of the system and even bring unforgettable characteristics, and excessive acid aroma can cause sense impression such as putrefaction, acid odor and the like, thereby reducing the acceptance of the product. Therefore, the analytical method for reasonably evaluating and monitoring the basic composition of the acid aroma characteristic substances in the flavor system has important significance.
Although the acid component is essentially all organic acids, not all organic acids are acid components. This has not received sufficient attention in many reports. In fact, molecules that interact with olfactory receptors to produce aroma need themselves to have relatively low molecular weights, and all aroma substances currently found have molecular weights below 350[ chemistry ] biological sensitivity, 2004,1 (12): 1957-1974], so that organic acids with molecular weights above 350 do not have an acid aroma contribution. Secondly, from the perspective of evolution, the normal height of the human nasal cavity is 1.5-2 m above the ground, and the human olfactory behavioral pattern determines that the human olfactory system mainly detects substances with strong volatility; in contrast, animals such as boars or beagles can inhale less volatile chemicals into the nasal cavity by bringing the nose close to the ground and inhaling them quickly, and thus have evolved the ability to detect low-volatile molecules [ Predator-pre Dynamics: the Role of ozone new York, CRC Press,2007], so that The less volatile organic acids have essentially no acid fragrance contribution. Thirdly, the relationship between aroma characteristics and chemical structures is not predicted by an effective theoretical model at present [ Angew. Chem. Int. Ed.,2006, 45.
At present, most of the methods are to use various organic acids with different aroma or taste characteristics in the smoke as analysis objects. Therefore, it is necessary to develop a rapid, sensitive and focused quantitative analysis method for important acid and aroma components in cigarette smoke.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, and provides a method for simultaneously measuring 10 acid aroma components in the mainstream smoke of cigarettes, which has the advantages of quick detection, high sensitivity, good selectivity and high accuracy and is suitable for measuring the content of the acid aroma components in the cigarette smoke.
In order to solve the technical problems, the invention adopts the following specific technical scheme:
s1, sample extraction and derivatization:
after particulate matters of mainstream smoke of the cigarettes are captured by using a Cambridge filter, transferring the Cambridge filter into an extraction container, adding a dichloromethane solution, adding an internal standard substance solution for oscillation extraction, taking supernate, adding a derivatization reagent, and heating to obtain a smoke sample;
the internal standard substance is trans-3-hexenoic acid;
s2, detecting a sample by gas chromatography-tandem mass spectrometry:
detecting a smoke sample by adopting GC-MS/MS, and detecting the content of 10 acid and fragrance components by an internal standard quantitative method;
the gas chromatography conditions for the detection are as follows: and (3) chromatographic column: DB-5MS (60 m 0.25mm 0.25 μm); carrier gas: he; column flow rate: 1mL/min; sample inlet temperature: 250 ℃; temperature programming: 50 deg.C (1 min), 5 deg.C/min → 200 deg.C (0 min); the split ratio is as follows: 5:1.
In the invention, the acid aroma components in the mainstream smoke of the cigarette are formic acid, acetic acid, isovaleric acid, n-valeric acid, 3-methyl-2-butenoic acid, 3-methylvaleric acid, 4-methylvaleric acid, n-hexanoic acid, n-heptanoic acid and benzoic acid.
Preferably, the amount of the internal standard substance solution is 10 to 100 μ L, the amount of the dichloromethane is 10 to 50mL, the derivatization reagent is N, O-bis (trimethylsilyl) trifluoroacetamide or N-methyl-N- (trimethylsilyl) trifluoroacetamide, and the amount of the derivatization reagent is 50 to 100 μ L.
Preferably, in S1, the concentration of the internal standard substance is 2mg/mL.
Preferably, the shaking extraction time is 20-50 min.
Preferably, in S1, the heating temperature is 20-100 ℃, and the heating time is 50-100 min.
Preferably, the mass spectrometry conditions for the detection in s2. Are: GC/MS transmission line temperature: 250 ℃, EI ion source temperature: 230 ℃, quadrupole temperature: 150 ℃; EI ionization energy: 70eV; scanning mode: an ion scan is selected, and the time segments are divided according to retention time.
Preferably, in s2, the standard working solution adopted by the internal standard quantitative method contains 10 acid-fragrance components and 1 internal standard substance, and the solvent is dichloromethane; the concentration of the internal standard substance trans-3-hexenoic acid in all the standard working solutions is 2mg/mL, and the concentration magnitude of formic acid in the standard working solutions is 0.645, 1.29, 3.225, 6.45 and 12.9 mu g/mL from low to high in sequence; the concentration magnitude of the acetic acid is 4.708, 9.416, 23.54, 47.08 and 94.16 mu g/mL from low to high in sequence; the concentration magnitude of the isovaleric acid is 0.187, 0.374, 0.935, 1.87 and 3.74 mu g/mL from low to high in sequence; the concentration magnitude of the n-valeric acid is 0.051, 0.102, 0.255, 0.51 and 1.02 mu g/mL from low to high in sequence; the concentration levels of the 3-methyl-2-butenoic acid are 0.011, 0.022, 0.055, 0.11 and 0.22 mu g/mL from low to high in sequence; the concentration levels of the 3-methylvaleric acid are 0.029, 0.058, 0.145, 0.29 and 0.58 mu g/mL from low to high in sequence; the concentration levels of the 4-methylvaleric acid are 0.047, 0.094, 0.235, 0.47 and 0.94 mu g/mL from low to high in sequence; the concentration magnitude of the n-hexanoic acid is 0.05, 0.1, 0.25, 0.5 and 1 mu g/mL from low to high in sequence; the concentration levels of the n-heptanoic acid are 0.094, 0.188, 0.47, 0.94 and 1.88 mu g/mL from low to high in sequence; the concentration of the benzoic acid is 0.94, 1.88, 4.7, 9.4 and 18.8 mu g/mL from low to high in sequence.
Compared with the prior art, the invention has the following beneficial effects:
the method fills the blank of the prior art, and adopts a GC-MS/MS method to simultaneously determine the content of 10 acid aroma components in the mainstream smoke of the cigarette, wherein the 10 acid aroma components specifically comprise formic acid, acetic acid, isovaleric acid, n-valeric acid, 3-methyl-2-butenoic acid, 3-methylvaleric acid, 4-methylvaleric acid, n-hexanoic acid, n-heptanoic acid and benzoic acid. Wherein the content of the components such as 3-methyl-2-butenoic acid and the like can be quantitatively detected in the tobacco products for the first time. The method has the advantages of focusing important acid aroma components in the smoke, quick detection, high sensitivity, good selectivity and high accuracy, and is suitable for measuring the content of the acid aroma components in the cigarette smoke.
Drawings
FIG. 1 is a graph of SIM obtained by GC-MS detection of 10 kinds of acid aroma component standard samples.
FIG. 2 is a SIM chart of the GC-MS detection of the acid components in the mainstream smoke sample of the cigarette of example 1.
Wherein, 1: formic acid; 2: acetic acid; 3: isovaleric acid; 4: n-pentanoic acid; 5: 3-methyl-2-butenoic acid; 6: 3-methylvaleric acid; 7: 4-methylvaleric acid; 8: n-hexanoic acid; 9: n-heptanoic acid; 10: benzoic acid.
FIG. 3 is a schematic diagram of the overall process of the method of the present invention.
Detailed Description
The present invention will be further described with reference to the following embodiments.
The invention adopts a standard addition method to compare retention time, and then carries out quantification through an internal standard curve method. The names and quantitative ion information of 10 types of acid components and internal standards are shown in table 1:
TABLE 1 10 acid aroma components, internal standard names, and quantitative ion information
Under the detection conditions of the present invention, the quantitative curve, linear range, detection limit, and quantitative limit of 10 kinds of acid components are shown in table 2.
TABLE 2 quantitative curves, linear ranges, detection limits, quantitative limits of the 10 acid components
Example 1
The method for simultaneously measuring 10 types of acid aroma components in the mainstream smoke of the cigarette comprises the following steps:
s1, smoking the cigarette with the trade mark 1 after balancing and screening according to the standard smoking condition specified in YC/T29-1996, using two Cambridge filter discs to collect particulate matters of the mainstream smoke of 5 cigarettes, placing the filter discs in a 50mL conical flask with a plug, adding 25mL of dichloromethane solution, vibrating for 20min on an oscillator at room temperature, adding 30 μ L of trans-3-hexenoic acid internal standard solution, mixing uniformly, taking 1.5mL of supernatant, adding 60 μ L of derivatization reagent N, O-bis (trimethylsilyl) trifluoroacetamide (BSTFA), and placing the supernatant in a water bath at 60 ℃ to heat for 50min to obtain a cigarette smoke sample.
S2, detecting the flue gas sample obtained in the step S1 by adopting GC-MS (gas chromatography-Mass spectrometer)
The chromatographic conditions are as follows: a chromatographic column: DB-5MS (60 m 0.25mm 0.25 μm); carrier gas: he; column flow rate: 1mL/min; sample inlet temperature: 250 ℃; temperature programming: 50 deg.C (0 min), 5 deg.C/min → 200 deg.C (0 min); the split ratio is as follows: 5:1.
the mass spectrum conditions are as follows: GC/MS transmission line temperature: 250 ℃, EI ion source temperature: 230 ℃, quadrupole temperature: 150 ℃; EI ionization energy: 70eV; scanning mode: an ion scan is selected, and the time segments are divided according to retention time.
The results of the cigarette test of the method for simultaneously measuring 10 acid-flavor components in the mainstream smoke of the cigarette under the brand number 1 are shown in table 3.
Example 2
The method for simultaneously measuring 10 types of acid aroma components in the mainstream smoke of the cigarette comprises the following steps:
s1, smoking the cigarette with the trade name 2 after balancing and screening according to standard smoking conditions specified in YC/T29-1996, using two Cambridge filter discs to collect particulate matters of main stream smoke of 8 cigarettes, placing the cigarettes in a 50mL conical flask with a plug, adding 40mL of dichloromethane solution, vibrating for 30min on an oscillator at room temperature, adding 20 μ L of trans-3-hexenoic acid internal standard solution, mixing uniformly, taking 1mL of supernatant, adding 70 μ L of derivatization reagent BSTFA, and placing the mixture in a water bath at 60 ℃ for heating for 70min to obtain a cigarette smoke sample.
S2, detecting the flue gas sample obtained in the step S1 by adopting GC-MS;
the chromatographic conditions are as follows: and (3) chromatographic column: DB-5MS (60 m 0.25mm 0.25 μm); carrier gas: he; column flow rate: 1mL/min; sample inlet temperature: 250 ℃; temperature programming: 50 deg.C (0 min), 5 deg.C/min → 200 deg.C (0 min); the split ratio is as follows: 5:1.
the mass spectrum conditions are as follows: GC/MS transmission line temperature: 250 ℃, EI ion source temperature: 230 ℃, quadrupole temperature: 150 ℃; EI ionization energy: 70eV; scanning mode: an ion scan is selected, and the time segments are divided according to retention time.
The results of the cigarette test of the brand 2 by the method for simultaneously measuring 10 acid-flavor components in the mainstream smoke of the cigarette in this embodiment are shown in table 3.
Example 3
The method for simultaneously measuring 10 types of acid aroma components in the mainstream smoke of the cigarette comprises the following steps:
s1, smoking the cigarette with the mark 3 after balancing and screening according to standard smoking conditions specified in YC/T29-1996, using two Cambridge filter discs to collect particulate matters of main stream smoke of 8 cigarettes, placing the cigarettes in a 50mL conical flask with a plug, adding 50mL of dichloromethane solution, vibrating for 40min on an oscillator at room temperature, adding 60 mu L of trans-3-hexenoic acid internal standard solution, mixing uniformly, taking 1mL of supernatant, adding 90 mu L of derivatization reagent BSTFA, and placing the mixture in a water bath at 50 ℃ to heat for 90min to obtain a cigarette smoke sample.
S2, detecting the flue gas sample obtained in the step S1 by adopting GC-MS;
the spectral conditions were: and (3) chromatographic column: DB-5MS (60 m 0.25mm 0.25 μm); carrier gas: he; column flow rate: 1mL/min; sample inlet temperature: 250 ℃; temperature programming: 50 deg.C (0 min), 5 deg.C/min → 200 deg.C (0 min); the split ratio is as follows: 5:1.
the mass spectrum conditions are as follows: GC/MS transmission line temperature: 250 ℃, EI ion source temperature: 230 ℃, quadrupole temperature: 150 ℃; EI ionization energy: 70eV; scanning mode: an ion scan is selected, and the time segments are divided according to retention time.
The results of the cigarette test of the brand 3 by the method for simultaneously measuring 10 acid-flavor components in the mainstream smoke of the cigarette in this embodiment are shown in table 3.
Example 4
The method for simultaneously measuring 10 acid aroma components in the mainstream smoke of the cigarette in the embodiment comprises the following steps:
s1, smoking the cigarette with the mark 4 after balancing and screening according to standard smoking conditions specified in YC/T29-1996, using two Cambridge filter discs to collect particulate matters of main stream smoke of 8 cigarettes, placing the cigarettes in a 50mL conical flask with a plug, adding 50mL of dichloromethane solution, vibrating for 30min on an oscillator at room temperature, adding 100 mu L of trans-3-hexenoic acid internal standard solution, mixing uniformly, taking 1mL of supernatant, adding 100 mu L of derivatization reagent BSTFA, and placing the mixture in a water bath at 60 ℃ to heat for 100min to obtain a cigarette smoke sample.
S2, detecting the flue gas sample obtained in the step S1 by adopting GC-MS;
the spectral conditions were: a chromatographic column: DB-5MS (60 m 0.25mm 0.25 μm); carrier gas: he; column flow rate: 1mL/min; sample inlet temperature: 250 ℃; temperature programming: 50 deg.C (0 min), 5 deg.C/min → 200 deg.C (0 min); the split ratio is as follows: 5:1.
the mass spectrum conditions are as follows: GC/MS transmission line temperature: 250 ℃, EI ion source temperature: 230 ℃, quadrupole temperature: 150 ℃; EI ionization energy: 70eV; scanning mode: an ion scan is selected, and the time segments are divided according to retention time.
The cigarette test results of the method for simultaneously measuring 10 acid-flavor components in the mainstream smoke of the cigarette under the brand number 4 are shown in table 3.
Example 5
The method for simultaneously measuring 10 types of acid aroma components in the mainstream smoke of the cigarette comprises the following steps:
s1, smoking the balanced and screened cigarette with the brand 5 according to standard smoking conditions specified in YC/T29-1996, trapping 8 cigarette mainstream smoke particulate matters by using two Cambridge filter discs, placing the cigarette in a 50mL conical flask with a plug, adding 35mL of dichloromethane solution, vibrating for 40min on an oscillator at room temperature, adding 70 mu L of trans-3-hexenoic acid internal standard solution, uniformly mixing, taking 1mL of supernatant, adding 80 mu L of derivatization reagent BSTFA, and placing the mixture in a 70 ℃ water bath for heating for 60min to obtain a cigarette smoke sample.
S2, detecting the flue gas sample obtained in the step S1 by adopting GC-MS;
the spectral conditions were: and (3) chromatographic column: DB-5MS (60 m 0.25mm 0.25 μm); carrier gas: he; column flow rate: 1mL/min; sample inlet temperature: 250 ℃; temperature programming: 50 deg.C (0 min), 5 deg.C/min → 200 deg.C (0 min); the split ratio is as follows: 5:1.
the mass spectrum conditions are as follows: GC/MS transmission line temperature: 250 ℃, EI ion source temperature: 230 ℃, quadrupole temperature: 150 ℃; EI ionization energy: 70eV; scanning mode: ion scanning is selected, and the time segments are divided according to retention time.
The cigarette test results of the method for simultaneously measuring 10 acid-flavor components in the mainstream smoke of the cigarette under the brand number 5 are shown in table 3.
TABLE 3 test results of contents of acid-flavor components in cigarette samples of examples 1 to 5
The balanced and screened cigarettes are smoked according to the standard smoking conditions specified in YC/T29-1996, and 8 cigarette smoke particulate matters are collected by 2 Cambridge filter discs. The RSD value of 6 parallel measurements of 6 groups and 10 acid components measured according to the method of example 1 is between 3% and 8% (see Table 4), which proves that the method of the invention has higher precision and good repeatability.
TABLE 4 precision of solvent extraction-gas chromatography-mass spectrometry combination
It should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the present invention and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.
Claims (5)
1. A method for simultaneously measuring the contents of 10 acid aroma components in the mainstream smoke of cigarettes is characterized by comprising the following steps: the method comprises the following steps:
s1, sample extraction and derivatization:
after particulate matters of mainstream smoke of the cigarettes are trapped by using a Cambridge filter disc, transferring the Cambridge filter disc into an extraction container, adding a dichloromethane solution, then adding an internal standard substance solution for oscillation extraction, taking supernate, adding a derivatization reagent, and heating to obtain a smoke sample;
the internal standard substance is trans-3-hexenoic acid;
s2, detecting a sample by gas chromatography-tandem mass spectrometry:
detecting a smoke sample by adopting GC-MS/MS, and detecting the content of 10 acid and fragrance components by an internal standard quantitative method;
the gas chromatography conditions for detection are as follows: and (3) chromatographic column: DB-5MS specification 60m × 0.25mm × 0.25 μm; carrier gas: he; column flow rate: 1mL/min; sample inlet temperature: 250 ℃; temperature programming: 0min at 50 ℃,5 ℃/min → 0min at 200 ℃; the split ratio is as follows: 5, 1;
the 10 kinds of acid components comprise formic acid, acetic acid, isovaleric acid, n-pentanoic acid, 3-methyl-2-butenoic acid, 3-methylpentanoic acid, 4-methylpentanoic acid, n-hexanoic acid, n-heptanoic acid and benzoic acid;
s2, in the internal standard quantitative method, a standard working solution contains 10 acid fragrance components and 1 internal standard substance, and a solvent is dichloromethane; the concentration of the internal standard substance trans-3-hexenoic acid in all the standard working solutions is 2mg/mL, and the concentration magnitude of formic acid in the standard working solutions is 0.645, 1.29, 3.225, 6.45 and 12.9 mu g/mL from low to high in sequence; the concentration magnitude of the acetic acid is 4.708, 9.416, 23.54, 47.08 and 94.16 mu g/mL from low to high in sequence; the concentration magnitude of the isovaleric acid is 0.187, 0.374, 0.935, 1.87 and 3.74 mu g/mL from low to high in sequence; the concentration magnitude of the n-valeric acid is 0.051, 0.102, 0.255, 0.51 and 1.02 mu g/mL from low to high in sequence; the concentration magnitude of the 3-methyl-2-butenoic acid is 0.011, 0.022, 0.055, 0.11 and 0.22 mu g/mL in sequence from low to high; the concentration magnitude of the 3-methyl pentanoic acid is 0.029, 0.058, 0.145, 0.29 and 0.58 mu g/mL from low to high in sequence; the concentration levels of the 4-methylvaleric acid are 0.047, 0.094, 0.235, 0.47 and 0.94 mu g/mL from low to high in sequence; the concentration magnitude of the n-hexanoic acid is 0.05, 0.1, 0.25, 0.5 and 1 mu g/mL from low to high in sequence; the concentration magnitude of the n-heptanoic acid is 0.094, 0.188, 0.47, 0.94 and 1.88 mu g/mL from low to high in sequence; the concentration magnitude of the benzoic acid is 0.94, 1.88, 4.7, 9.4 and 18.8 mu g/mL from low to high in sequence;
the using amount of the internal standard substance solution is 10-100 mu L, the using amount of the dichloromethane is 10-50 mL, the derivatization reagent is N, O-bis (trimethylsilyl) trifluoroacetamide or N-methyl-N- (trimethylsilyl) trifluoroacetamide, and the using amount of the derivatization reagent is 50-100 mu L.
2. The method for simultaneously determining the contents of 10 acid-flavor components in the mainstream smoke of cigarettes according to claim 1, wherein the method comprises the following steps: s1, the concentration of the internal standard substance is 2mg/mL.
3. The method for simultaneously determining the contents of 10 acid-flavor components in the mainstream smoke of the cigarette according to claim 1, wherein in S1, the oscillation extraction time is 20-50 min.
4. The method for simultaneously determining the contents of 10 acid-flavor components in the mainstream smoke of the cigarette according to claim 1, wherein in S1, the heating temperature is 20-100 ℃, and the heating time is 50-100 min.
5. The method for simultaneously determining the contents of 10 acid-flavor components in the mainstream smoke of cigarettes according to claim 1, wherein the method comprises the following steps: s2, the mass spectrum conditions of the detection are as follows: GC/MS transmission line temperature: 250 ℃, EI ion source temperature: 230 ℃, quadrupole temperature: 150 ℃; EI ionization energy: 70eV; scanning mode: an ion scan is selected, and the time segments are divided according to retention time.
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| 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 |
| CN114034787B (en) * | 2021-10-29 | 2024-05-03 | 中国烟草总公司郑州烟草研究院 | Method for measuring sensory related amide compounds in main stream smoke of cigarettes |
| CN116297956B (en) * | 2023-03-17 | 2024-01-30 | 江苏中烟工业有限责任公司 | Method for evaluating release and transfer behaviors of acidic fragrant raw materials in cigarettes of different circumferences |
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