CN116297956A - Method for evaluating release and transfer behaviors of acidic fragrant raw materials in cigarettes of different circumferences - Google Patents
Method for evaluating release and transfer behaviors of acidic fragrant raw materials in cigarettes of different circumferences Download PDFInfo
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- CN116297956A CN116297956A CN202310259838.1A CN202310259838A CN116297956A CN 116297956 A CN116297956 A CN 116297956A CN 202310259838 A CN202310259838 A CN 202310259838A CN 116297956 A CN116297956 A CN 116297956A
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- 235000019504 cigarettes Nutrition 0.000 title claims abstract description 119
- 230000002378 acidificating effect Effects 0.000 title claims abstract description 49
- 238000000034 method Methods 0.000 title claims abstract description 42
- 239000002994 raw material Substances 0.000 title claims abstract description 42
- 238000012546 transfer Methods 0.000 title claims abstract description 38
- 230000006399 behavior Effects 0.000 title claims abstract description 27
- 239000012086 standard solution Substances 0.000 claims abstract description 38
- 239000002304 perfume Substances 0.000 claims abstract description 34
- 239000002904 solvent Substances 0.000 claims abstract description 32
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- 238000002360 preparation method Methods 0.000 claims abstract description 11
- 238000004458 analytical method Methods 0.000 claims abstract description 9
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- 238000012360 testing method Methods 0.000 claims description 24
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- 239000000243 solution Substances 0.000 claims description 17
- 239000000796 flavoring agent Substances 0.000 claims description 13
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- NDJKXXJCMXVBJW-UHFFFAOYSA-N heptadecane Chemical compound CCCCCCCCCCCCCCCCC NDJKXXJCMXVBJW-UHFFFAOYSA-N 0.000 claims description 12
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- 239000000779 smoke Substances 0.000 claims description 12
- 239000011550 stock solution Substances 0.000 claims description 12
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 claims description 9
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- 235000013599 spices Nutrition 0.000 claims description 9
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- AFTLVCKDKPSOGG-UHFFFAOYSA-N o-methylhydroxylamine;pyridine;hydrochloride Chemical compound Cl.CON.C1=CC=NC=C1 AFTLVCKDKPSOGG-UHFFFAOYSA-N 0.000 claims description 4
- 238000004513 sizing Methods 0.000 claims description 4
- XCOBLONWWXQEBS-KPKJPENVSA-N N,O-bis(trimethylsilyl)trifluoroacetamide Chemical compound C[Si](C)(C)O\C(C(F)(F)F)=N\[Si](C)(C)C XCOBLONWWXQEBS-KPKJPENVSA-N 0.000 claims description 3
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- JOOXCMJARBKPKM-UHFFFAOYSA-N 4-oxopentanoic acid Chemical compound CC(=O)CCC(O)=O JOOXCMJARBKPKM-UHFFFAOYSA-N 0.000 description 10
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 10
- WBYWAXJHAXSJNI-VOTSOKGWSA-M .beta-Phenylacrylic acid Natural products [O-]C(=O)\C=C\C1=CC=CC=C1 WBYWAXJHAXSJNI-VOTSOKGWSA-M 0.000 description 6
- WBYWAXJHAXSJNI-SREVYHEPSA-N Cinnamic acid Chemical compound OC(=O)\C=C/C1=CC=CC=C1 WBYWAXJHAXSJNI-SREVYHEPSA-N 0.000 description 6
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- XYHKNCXZYYTLRG-UHFFFAOYSA-N 1h-imidazole-2-carbaldehyde Chemical compound O=CC1=NC=CN1 XYHKNCXZYYTLRG-UHFFFAOYSA-N 0.000 description 3
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- PRDIIROHTWNJDB-UHFFFAOYSA-N 3-caproyl propionic acid Chemical compound CCCCCC(=O)CCC(O)=O PRDIIROHTWNJDB-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 2
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- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
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- 235000007173 Abies balsamea Nutrition 0.000 description 1
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- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 150000001261 hydroxy acids Chemical class 0.000 description 1
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- 238000004811 liquid chromatography Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
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- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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Abstract
The invention provides a method for evaluating the release and transfer behaviors of acidic perfume raw materials in cigarettes with different circumferences, which comprises the following steps: (1) preparing a cigarette sample; (2) internal standard solution preparation; (3) matrix solvent preparation; (4) preparing a standard solution; (5) sample pretreatment; (6) mass spectrometry instrumentation analysis; (7) calculating the result. The evaluation method provided by the invention can effectively evaluate and analyze the release and transfer behaviors of the acidic perfume raw materials in cigarettes with different circumferences, and provides scientific basis and theoretical support for quantifying the perfuming and feeding of the cigarettes, strengthening the understanding of the perfuming effect and the perfume compensation technology of the fine cigarettes.
Description
Technical Field
The invention belongs to the technical field of detection of cigarette aroma raw materials, and particularly relates to a method for evaluating release and transfer behaviors of acidic aroma raw materials in cigarettes with different circumferences.
Background
The very important part of the technology of the essence and the spice for cigarettes is to determine the reasonable dosage of the spice monomer and the adding efficiency of the spice monomer, the transfer rate of the spice raw materials in the main stream smoke grain phase matters of cigarettes is directly reflected by the flavoring efficiency of the spice raw materials, and the higher the transfer rate of the spice raw materials in the main stream smoke grain phase is, the higher the corresponding flavoring efficiency is. Therefore, it is a key to improve the perfuming effect to increase the rate of transfer of the perfume raw material to the particulate phase of the mainstream smoke.
Sensory smoking experience shows that the appearance effects of flavoring raw materials and solvents commonly used in cigarette flavoring in fine cigarettes are different from those of coarse cigarettes and medium cigarettes due to the difference of the circumference and the length of the cigarettes. However, researches on the influence of cigarette circumferences on the transfer and release behaviors of the fragrance raw materials in cigarette smoke are reported recently.
The acidic organic matter can be derivatized to realize GC or GC/MS detection due to the polar or strong polar functional groups. Organic acids in tobacco can be classified as fatty acids and non-fatty acids. The volatile and semi-volatile fatty acids and their characteristic aroma and acidity can significantly affect the aroma quality of cigarettes, such as strength and irritation of cigarettes. But not fatty organic acids (hydroxy acids, oxo acids, aromatic acids, etc.), also have characteristic aroma and taste; for example, lactic acid has a milk flavor, which can make smoke more smooth and mellow; 4-oxo-nonanoic acid has pungent taste, and can increase smoke fullness; benzoic acid appears as a weak, light alcohol and fragrance; cinnamic acid has a mild, faint balsam fragrance, etc. Therefore, research on the type and content of organic acids in flavors is of great value and significance in understanding the sensory quality of tobacco and improving cigarette formulations. At present, the qualitative and quantitative methods of organic acid at home and abroad are more, and mainly include ion chromatography, capillary electrophoresis, liquid chromatography, gas chromatography and the like. Ion chromatography, capillary electrophoresis, liquid chromatography are basically used for the analysis of high content polyacids and polyhydroxy acids. In the gas chromatography, since derivative methods such as methyl esterification and silanization are applied in pretreatment, volatile acid and semi-volatile acid can be basically analyzed, but for volatile fatty acid and other non-fatty organic acid with low content in perfume, accurate quantification is difficult due to limitation of instrument sensitivity and influence of impurity interference.
Therefore, how to provide a method for evaluating the quantitative and release transfer behavior of low-content acidic perfume materials has become a problem to be solved.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a method for evaluating the release and transfer behaviors of acidic perfume raw materials in cigarettes with different circumferences. The evaluation method provided by the invention can effectively evaluate and analyze the release and transfer behaviors of the acidic perfume raw materials in cigarettes with different circumferences, and provides scientific basis and theoretical support for quantifying the perfuming and feeding of the cigarettes, strengthening the understanding of the perfuming effect and the perfume compensation technology of the fine cigarettes.
In order to achieve the aim of the invention, the invention adopts the following technical scheme:
the invention provides a method for evaluating the release and transfer behaviors of acidic perfume raw materials in cigarettes with different circumferences, which comprises the following steps:
(1) And (3) preparing cigarette samples: selecting tobacco shreds of the formula leaf group, and rolling an unflavoured feeding cigarette to serve as a blank cigarette; simultaneously selecting tobacco shreds with the same formula, respectively rolling cigarettes with different circumferences, and injecting and applying acidic fragrance raw material solution to serve as test cigarettes;
(2) And (3) preparing an internal standard solution: n-heptadecane is used as an internal standard substance, ethanol is used as a solvent, and an internal standard solution is prepared;
(3) Preparing a matrix solvent: smoking the blank cigarettes, and vibrating and extracting the collected filter discs by using ethanol as an extraction solvent, wherein the extraction liquid passes through an organic phase filter membrane to obtain a matrix solvent;
(4) Preparing a standard solution: taking acidic perfume raw materials as objects, adding an internal standard solution, and taking a matrix solvent as a dilution solvent to prepare standard solutions with different concentration gradients;
(5) Sample pretreatment: sucking test cigarettes, respectively collecting cigarette butts and filter discs, adding an internal standard solution, and treating and extracting acidic components in a sample by using an oximation and silanization derivatization method to obtain a sample solution to be tested;
(6) Mass spectrometry instrument analysis: detecting the sample solution to be detected and the standard solution by using a GC-MS instrument, collecting data, and quantitatively analyzing the content of the target object;
(7) And (3) calculating results: for cigarettes with different circumference samples, the retention rate and the transfer rate of the acidic perfume raw materials are calculated.
The steps (1), (2) and (3) do not distinguish the sequence.
The method can effectively evaluate the release and transfer behaviors of the acidic perfume raw materials in cigarettes with different circumferences, and provides scientific basis and theoretical support for quantifying the perfuming and feeding of the cigarettes, strengthening the understanding of the perfuming effect and the perfume compensation technology of the cigarettes.
Preferably, in the step (1), the cigarette sample manufacturing process is as follows: selecting a formula leaf group tobacco leaf, cutting into cut tobacco in a laboratory, and taking the rolled cigarettes as blank cigarettes without applying essence and spice; simultaneously selecting tobacco shreds with the same formula, respectively rolling cigarette samples with different circumferences, applying 15-25 mu L of acidic perfume raw material solution into the tobacco shreds with the formula by using a microinjector to obtain test cigarettes, and balancing for more than 48 hours at the temperature of 22 ℃ and relative humidity of 60+/-5%.
The volume of the acidic fragrant solution may be 15. Mu.L, 16. Mu.L, 17. Mu.L, 18. Mu.L, 19. Mu.L, 20. Mu.L, 21. Mu.L, 22. Mu.L, 23. Mu.L, 24. Mu.L, 25. Mu.L, etc., but is not limited to the above-listed values, and other values not listed in the above-listed value ranges are equally applicable.
Preferably, in the step (2), the internal standard solution is prepared by the following steps: accurately weighing 0.4-0.6g of n-heptadecane, transferring into a 100mL volumetric flask, dissolving with ethanol, shaking up and sizing to obtain an internal standard stock solution, accurately transferring 0.8-1.2mL of the internal standard stock solution into a 10mL volumetric flask, dissolving with ethanol, shaking up and sizing to obtain an internal standard solution.
The mass of n-heptadecane may be 0.4g, 0.45g, 0.5g, 0.55g or 0.6g, and the volume of the internal standard stock solution to be removed may be 0.8mL, 0.9mL, 1mL, 1.1mL or 1.2mL, but is not limited to the values listed above, and other values not listed in the above-mentioned numerical ranges are equally applicable.
Preferably, in the step (3), the matrix solvent is prepared by: selecting blank cigarettes, smoking according to GB19609 method, collecting filter discs after smoking, transferring to a bottle, adding ethanol, placing on a shaker, shaking and extracting at 140-180rpm for 30-50min, and filtering the extract with 0.22 μm organic phase filter membrane to obtain matrix solvent.
The speed of the shaking may be 140rpm, 150rpm, 160rpm, 170rpm, 180rpm, etc., and the time of the shaking may be 30min, 35min, 40min, 45min, 50min, etc., but the shaking is not limited to the above-listed values, and other values not listed in the above-listed value range are equally applicable.
Preferably, in the step (4), the standard solution preparation process is as follows: respectively weighing acidic perfume raw materials, and adding an internal standard solution and a matrix solvent as extraction solvents to serve as standard stock solution; and diluting the standard stock solution by using a matrix solvent as a diluent to prepare 6 concentration gradient standard solutions respectively.
Preferably, in step (5), the sample pretreatment process is: selecting test cigarettes, smoking the cigarettes according to a GB/T19609 method, collecting cigarette butts and Cambridge filter discs respectively after smoking, transferring the cigarettes into a bottle, adding 80-120 mu L of internal standard solution, 18-22mL of ethanol and 80-100 mu L of methoxyl ammonia hydrochloride-pyridine solution with the concentration of 20-30mg/mL, shaking and mixing uniformly, incubating for 30-60min at the temperature of 35-37 ℃, adding derivatization reagent N, O-bis (trimethylsilyl) trifluoroacetamide, and transferring the derivatized solution into a microscale sample injection device for on-machine test to obtain a sample solution to be tested.
The volume of the internal standard solution may be 80. Mu.L, 90. Mu.L, 100. Mu.L, 110. Mu.L, 120. Mu.L, etc., the volume of ethanol may be 18mL, 19mL, 20mL, 21mL, 22mL, etc., the volume of the methoxyammonia hydrochloride-pyridine solution may be 80. Mu.L, 85. Mu.L, 90. Mu.L, 95. Mu.L, 100. Mu.L, etc., the concentration may be 20mg/mL, 21mg/mL, 22mg/mL, 23mg/mL, 24mg/mL, 25mg/mL, 26mg/mL, 27mg/mL, 28mg/mL, 29mg/mL, 30mg/mL, etc., the temperature of incubation may be 35 ℃, 35.5 ℃, 36.5 ℃, 36 ℃, 37 ℃, etc., the time may be 30min, 35min, 40min, 45min, 50min, 55min, 60min, etc., but the above-mentioned values are not limited to the values, and the other values not listed above are equally applicable.
Preferably, in the step (6), the GC-MS is adopted to analyze the standard solutions with different concentration gradients, and a standard working curve is established; and quantitatively analyzing the sample solution to be detected.
Preferably, the analysis conditions are: the chromatographic column is DB-5MS, the specification is 30m multiplied by 0.25mm multiplied by 0.25 mu m; sample injection amount: 0.8-1.2. Mu.L; the flow rate is 0.8-1.2mL/min; heating program: heating to 200deg.C at 50deg.C/min, maintaining for 10min, heating to 280 deg.C at 20deg.C/min, and maintaining for 25min.
The sample amount may be 0.8. Mu.L, 0.9. Mu.L, 1. Mu.L, 1.1. Mu.L, 1.2. Mu.L, etc., and the flow rate may be 0.8mL/min, 0.9mL/min, 1mL/min, 1.1mL/min, 1.2mL/min, etc., but the present invention is not limited to the above-mentioned values, and other values not mentioned in the above-mentioned value ranges are equally applicable.
Preferably, in step (7), the result calculation process is:
retention = (target content in filter after test cigarette smoking-target content in filter after blank cigarette smoking)/target content in tobacco shred before test cigarette smoking x 100%.
Transfer rate = (target content in main stream smoke after test cigarette smoking-target content in main stream smoke after blank cigarette smoking)/target content in tobacco shred before test cigarette smoking x 100%.
Preferably, the acidic perfume raw material comprises any one or a combination of at least two of isovaleric acid, caproic acid, levulinic acid or cinnamic acid.
Compared with the prior art, the invention has the following beneficial effects:
the invention provides a method for evaluating the release and transfer behaviors of acidic perfume raw materials in cigarettes with different circumferences, which can effectively evaluate the release and transfer behaviors of the acidic perfume raw materials in the cigarettes with different circumferences and provides scientific basis and theoretical support for quantifying perfuming and feeding of the cigarettes, strengthening understanding of perfuming effect and perfume compensation technology of fine cigarettes.
Drawings
FIG. 1 is a GC-MS results for the standard solution of example 1;
FIG. 2 is a graph of GC-MS results for the sample solution of example 1.
Detailed Description
The technical scheme of the invention is further described by the following specific embodiments. It will be apparent to those skilled in the art that the examples are merely to aid in understanding the invention and are not to be construed as a specific limitation thereof.
Example 1
The embodiment provides a method for evaluating the release and transfer behaviors of acidic perfume raw materials in cigarettes with different circumferences, which takes isovaleric acid, caproic acid, levulinic acid and cinnamic acid as acidic perfume raw materials for perfuming the cigarettes as objects, and comprises the following specific steps:
(1) Cigarette sample preparation
Selecting a formula leaf group tobacco leaf, cutting into cut tobacco in a laboratory, and taking the rolled cigarettes as blank cigarettes without applying essence and spice; simultaneously selecting tobacco shreds with the same formula, respectively rolling cigarette samples (fine cigarettes, medium cigarettes and coarse cigarettes) with circumferences of 17mm, 20mm and 24mm, and applying 20 mu L of acidic essence solution with a certain concentration into the tobacco shreds with the same formula by using a microinjector to serve as test cigarettes. The equilibrium is carried out for 48 hours at a temperature of 22℃and a relative humidity of 60%.
Preparing an acidic essence solution: isovaleric acid, caproic acid, levulinic acid and cinnamic acid monomer flavors are respectively weighed into 0.1g of monomer flavors, transferred into a 50mL volumetric flask, added with ethanol for constant volume and uniformly shaken to obtain mixed acidic essence solution.
(2) Preparation of internal standard solution
Accurately weighing 0.5g of n-heptadecane (accurate to 0.1 mg), transferring into a 100mL volumetric flask, dissolving with ethanol, shaking up and fixing the volume to obtain an internal standard stock solution. Accurately transferring 1mL of internal standard stock solution into a 10mL volumetric flask, dissolving with ethanol, shaking, and fixing volume to obtain internal standard solution.
(3) Matrix solvent preparation
Selecting 20 blank cigarettes, smoking according to GB19609 method, collecting filter discs after smoking, transferring to a 100mL bread bottle, adding 20mL ethanol, placing on a shaker, shaking and extracting at 160rpm for 40min, and filtering the extract with 0.22 μm organic phase filter membrane to obtain matrix solvent.
(4) Standard solution preparation
Respectively weighing a certain amount of acidic perfume raw materials, adding 100 mu L of internal standard solution and 20mL of matrix solvent as extraction solvents, and taking the extraction solvents as standard stock solution; and then using a matrix solvent as a diluent to prepare 6 gradient standard solutions of 0.5, 2, 10, 50, 100 and 200 mug/mL respectively for GC-MS instrument analysis. A standard sample diagram of a typical target is shown in fig. 1.
(5) Sample pretreatment
Selecting 20 cigarettes added with an acidic essence solution, smoking the cigarettes according to a GB19609 method, respectively collecting cigarette butts and Cambridge filter discs after smoking, transferring the cigarettes into a 100mL bread bottle, adding 100 mu L of an internal standard solution and 20mL of ethanol, adding 90 mu L of a methoxyl ammonia hydrochloride-pyridine solution with the concentration of 25mg/mL, shaking and mixing uniformly, incubating for 50min at 36 ℃, adding a derivatization reagent N, O-bis (trimethylsilyl) trifluoroacetamide (BSTFA), reacting for 10min, transferring the derivatized solution into a microsyringe device, waiting for machine test, and obtaining a sample solution to be analyzed by a GC-MS instrument. A sample solution diagram of a typical target is shown in fig. 2. From the figure, it can be found that the chromatographic peak shows good performance after the target substance in the sample solution is derivatized as described above, and can be effectively separated and analyzed.
(6) Instrumental analysis
Chromatographic column: DB-5MS (30 m.times.0.25 mm.times.0.25 μm); sample injection amount: 1 μl; sample injection amount: 1 μl; the split flow mode is as follows: split sample introduction, wherein the split ratio is 5:1; sample port temperature: 260 ℃; carrier gas: helium, constant flow condition, 1.0mL/min; heating program: heating to 200deg.C at 8deg.C/min (holding for 10 min), heating to 280 deg.C at 20deg.C/min, and holding for 25min; transmission line temperature: 280 ℃; ionization mode: an EI source; ion source temperature: 230 ℃; ionization energy: 70eV; quadrupole temperature: 150 ℃; solvent delay: 3min; the detection mode is as follows: a SIM; mass spectral mass scan range: 30-450amu.
Quantitative results: compared with the conventional standard curve establishment method quantification method, the method can reduce interference of matrix effect, and remarkably improve accuracy of quantitative results of target components, wherein comparison results of typical sour and fragrant raw materials are shown in the table 1 below. As can be seen from the table, compared with the method for quantifying the target object by establishing the standard working curve under the conventional means, the method can remarkably improve the analysis accuracy of the target object by adopting the technical means of preparing the standard working solution by the matrix solvent.
TABLE 1 comparison of exemplary target component accuracy under different methods
(7) Result calculation
For cigarettes of different circumference samples, the retention rate and the transfer rate of the acidic perfume raw materials were calculated according to the following formulas, and the results are shown in the following table 2.
Retention = (target content in filter after test cigarette smoking-target content in filter after blank cigarette smoking)/target content in tobacco shred before test cigarette smoking x 100%;
transfer rate = (target content in main stream smoke after test cigarette smoking-target content in main stream smoke after blank cigarette smoking)/target content in tobacco shred before test cigarette smoking x 100%.
TABLE 2 release transfer results of target Components for cigarettes of different circumferences
According to the data, the method provided by the invention can be used for effectively evaluating the release and transfer behaviors of the acidic perfume raw materials in cigarettes with different circumferences.
Example 2
This example provides a method for evaluating the release transfer behavior of acidic flavor materials in cigarettes of different circumferences, in accordance with example 1, except that in step (5) the incubation is carried out at 36℃for 10 min.
The recovery rate of the final acidic perfume raw materials is as follows:
target component | Main aroma | Recovery (%) |
Isopentanoic acid | Sour incense | 91.45 |
Caproic acid | Sour incense | 90.24 |
Levulinic acid | Sour incense | 82.59 |
Cinnamic acid | Sour incense | 88.58 |
Example 3
This example provides a method for evaluating the release transfer behavior of acidic flavor materials in cigarettes of different circumferences, in accordance with example 1, except that in step (5) the incubation is carried out at 30℃for 50 min.
The recovery rate of the final acidic perfume raw materials is as follows:
target component | Main aroma | Recovery (%) |
Isopentanoic acid | Sour incense | 90.21 |
Caproic acid | Sour incense | 84.69 |
Levulinic acid | Sour incense | 85.14 |
Cinnamic acid | Sour incense | 87.45 |
From the data, the invention can further improve the recovery rate, the detection accuracy and the evaluation accuracy of the retention rate and the transfer rate by controlling the specific parameters.
The applicant states that the method of evaluating the release and transfer behavior of acidic perfume raw materials in cigarettes of different circumferences of the present invention is described by the above examples, but the present invention is not limited to the above examples, i.e. it does not mean that the present invention must be practiced by relying on the above examples. It should be apparent to those skilled in the art that any modification of the present invention, equivalent substitution of raw materials for the product of the present invention, addition of auxiliary components, selection of specific modes, etc., falls within the scope of the present invention and the scope of disclosure.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited to the specific details of the above embodiments, and various simple modifications can be made to the technical solution of the present invention within the scope of the technical concept of the present invention, and all the simple modifications belong to the protection scope of the present invention.
In addition, the specific features described in the above embodiments may be combined in any suitable manner, and in order to avoid unnecessary repetition, various possible combinations are not described further.
Claims (9)
1. A method for evaluating the release and transfer behavior of acidic flavor materials in cigarettes of different circumferences, comprising the steps of:
(1) And (3) preparing cigarette samples: selecting tobacco shreds of the formula leaf group, and rolling an unflavoured feeding cigarette to serve as a blank cigarette; simultaneously selecting tobacco shreds with the same formula, respectively rolling cigarettes with different circumferences, and injecting and applying acidic fragrance raw material solution to serve as test cigarettes;
(2) And (3) preparing an internal standard solution: n-heptadecane is used as an internal standard substance, ethanol is used as a solvent, and an internal standard solution is prepared;
(3) Preparing a matrix solvent: smoking the blank cigarettes, and vibrating and extracting the collected filter discs by using ethanol as an extraction solvent, wherein the extraction liquid passes through an organic phase filter membrane to obtain a matrix solvent;
(4) Preparing a standard solution: taking acidic perfume raw materials as objects, adding an internal standard solution, and taking a matrix solvent as a dilution solvent to prepare standard solutions with different concentration gradients;
(5) Sample pretreatment: sucking test cigarettes, respectively collecting cigarette butts and filter discs, adding an internal standard solution, and treating and extracting acidic components in a sample by using an oximation and silanization derivatization method to obtain a sample solution to be tested;
(6) Mass spectrometry instrument analysis: detecting the sample solution to be detected and the standard solution by using a GC-MS instrument, collecting data, and quantitatively analyzing the content of the target object;
(7) And (3) calculating results: for cigarettes with different circumference samples, calculating the retention rate and the transfer rate of the acidic perfume raw materials;
the steps (1), (2) and (3) do not distinguish the sequence.
2. The method for evaluating the release and transfer behavior of acidic perfume raw materials in cigarettes with different circumferences according to claim 1, wherein in the step (1), the preparation process of the cigarette sample is as follows: selecting a formula leaf group tobacco leaf, cutting into cut tobacco in a laboratory, and taking the rolled cigarettes as blank cigarettes without applying essence and spice; simultaneously selecting tobacco shreds with the same formula, respectively rolling cigarette samples with different circumferences, applying 15-25 mu L of acidic perfume raw material solution into the tobacco shreds with the formula by using a microinjector to obtain test cigarettes, and balancing for more than 48 hours at the temperature of 22 ℃ and relative humidity of 60+/-5%.
3. The method for evaluating the release and transfer behaviors of acidic flavor raw materials in cigarettes with different circumferences according to claim 1 or 2, wherein in the step (2), the preparation process of the internal standard solution is as follows: accurately weighing 0.4-0.6g of n-heptadecane, transferring into a 100mL volumetric flask, dissolving with ethanol, shaking up and sizing to obtain an internal standard stock solution, accurately transferring 0.8-1.2mL of the internal standard stock solution into a 10mL volumetric flask, dissolving with ethanol, shaking up and sizing to obtain an internal standard solution.
4. A method for evaluating the release and transfer behavior of acidic flavor materials in cigarettes of different circumferences according to any one of claims 1-3, wherein in step (3), the matrix solvent preparation process is as follows: selecting blank cigarettes, smoking according to GB19609 method, collecting filter discs after smoking, transferring to a bottle, adding ethanol, placing on a shaker, shaking and extracting at 140-180rpm for 30-50min, and filtering the extract with 0.22 μm organic phase filter membrane to obtain matrix solvent.
5. The method for evaluating the release and transfer behavior of acidic flavor materials on cigarettes of different circumferences according to any one of claims 1 to 4, wherein in step (4), the standard solution preparation process is as follows: respectively weighing acidic perfume raw materials, and adding an internal standard solution and a matrix solvent as extraction solvents to serve as standard stock solution; and diluting the standard stock solution by using a matrix solvent as a diluent to prepare 6 concentration gradient standard solutions respectively.
6. A method for evaluating the release and transfer behavior of acidic flavor materials on cigarettes of different circumferences according to any one of claims 1 to 5, wherein in step (5), the sample pretreatment process is as follows: selecting test cigarettes, smoking the cigarettes according to a GB/T19609 method, collecting cigarette butts and Cambridge filter discs respectively after smoking, transferring the cigarettes into a bottle, adding 80-120 mu L of internal standard solution, 18-22mL of ethanol and 80-100 mu L of methoxyl ammonia hydrochloride-pyridine solution with the concentration of 20-30mg/mL, shaking and mixing uniformly, incubating for 30-60min at the temperature of 35-37 ℃, adding derivatization reagent N, O-bis (trimethylsilyl) trifluoroacetamide, and transferring the derivatized solution into a microscale sample injection device for on-machine test to obtain a sample solution to be tested.
7. The method for evaluating the release and transfer behavior of acidic perfume raw materials in cigarettes with different circumferences according to any one of claims 1 to 6, wherein in the step (6), GC-MS is adopted to analyze standard solutions with different concentration gradients, and a standard working curve is established; and quantitatively analyzing the sample solution to be detected.
8. A method for evaluating the release and transfer behavior of an acidic flavor material in cigarettes of different circumferences according to claim 7, wherein the analysis conditions are: the chromatographic column is DB-5MS, the specification is 30m multiplied by 0.25mm multiplied by 0.25 mu m; sample injection amount: 0.8-1.2. Mu.L; the flow rate is 0.8-1.2mL/min; heating program: heating to 200deg.C at 50deg.C/min, maintaining for 10min, heating to 280 deg.C at 20deg.C/min, and maintaining for 25min.
9. The method for evaluating the release and transfer behavior of acidic flavor materials on cigarettes of different circumferences according to any one of claims 1 to 8, wherein in step (7), the result calculation process is as follows:
retention = (target content in filter after test cigarette smoking-target content in filter after blank cigarette smoking)/target content in tobacco shred before test cigarette smoking x 100%;
transfer rate = (target content in main stream smoke after test cigarette smoking-target content in main stream smoke after blank cigarette smoking)/target content in tobacco shred before test cigarette smoking x 100%.
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