CN113156013A - GC-MS-based heated cigarette aroma-carrying particle evaluation method - Google Patents
GC-MS-based heated cigarette aroma-carrying particle evaluation method Download PDFInfo
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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
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
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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
- G01N30/02—Column chromatography
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- 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
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/72—Mass spectrometers
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- 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
- G01N30/02—Column chromatography
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Abstract
The invention discloses a heated cigarette aroma-carrying particle evaluation method based on GC-MS, which comprises the following steps: s1, compounding essence and spice with solvent; s2, spraying the essence and spice compounded in the step S1 into the aroma-carrying particles to be evaluated for perfuming, weighing the perfumed particles after fully and uniformly mixing, and placing the weighed perfumed particles into a headspace bottle; s3, placing the headspace bottle containing the flavored particles in the step S2 in a headspace sample injector, heating to a certain temperature, balancing for a period of time, and injecting headspace gas into a sample inlet of a gas chromatograph-mass spectrometer for analysis; s4, reading the response value of each fragrance component in the headspace gas by a gas chromatograph-mass spectrometer, and quantifying by using a standard curve. According to the method, aroma substances volatilized by heating aroma-carrying particles are extracted through a headspace sample injector, and then the extracted gas phase substances are rapidly analyzed through a gas chromatography-mass spectrometry combination method, so that the release amount of aroma components carried by different aroma-carrying particles under the same condition is judged, and the aroma-carrying particles most suitable for heating cigarettes are determined.
Description
Technical Field
The invention relates to the technical field of heated cigarette aroma-carrying particle analysis, in particular to a GC-MS-based heated cigarette aroma-carrying particle evaluation method.
Background
The heating cigarette is also called as a heating non-combustion cigarette, belongs to one of novel tobaccos, and is the novel tobacco which is developed most rapidly and with the greatest prospect at present. The heated cigarette is characterized by heating tobacco shreds instead of burning the tobacco shreds. The tobacco material for cigarette heating is mostly used in the form of tobacco sheet (reconstituted tobacco), which is a core material of cigarette products that are not burned. Due to the characteristics of 'heating without burning' and low heating temperature (about 300 ℃), the release of volatile aroma substances in the smoke of the tobacco sheets of the heated cigarettes is inferior to that of the traditional cigarettes, and the characteristic aroma of the tobacco sheets is generally required to be modified and improved or compensated by adding external fragrance. Therefore, the utilization of the blending technology and the blending means to make up for the flavor deficiency of the heated cigarette has become a hot point in the development of the heated cigarette. The three-section cigarette structure for heating cigarette is composed of core section, multifunctional cavity fixing section and cellulose acetate section. The multifunctional cavity fixing section can be filled with aroma particle substances, the cigarette is eluted through the temperature of smoke during smoking, and the aroma substances are released to realize aroma supplementation, and in order to improve the release amount of aroma during smoking, volatile aroma components are often added to the aroma particle substances, so that the aroma components on the aroma particle substances are fully volatilized during smoking. However, the fragrance-carrying particulate matter has a different structure, and the volatilization speed and the appropriate temperature of the fragrance component attached to the fragrance-carrying particulate matter are also different, so that the volatilization amount is different during smoking. Therefore, the aroma-laden particles also have a large influence on the smoking quality of the heated cigarette.
At present, scientific and technical tobacco workers in China have less research on relevant aspects such as preparation processes, storage conditions and the like of the aroma-carrying particles, and the evaluation method of the aroma-carrying particles for heating cigarettes is not reported and recorded. In the prior art, the aroma substances in the tobacco products can be analyzed by adopting a gas chromatography-mass spectrometry (GC-MS) method, and the methods for extracting the aroma substances mainly comprise a distillation extraction method, a supercritical extraction method, a solvent extraction method, a solid phase micro-extraction method and the like. The method for extracting the fragrant substances has the advantages of more complicated operation steps and long extraction time, and needs an organic solvent in the detection process, so that the method is not favorable for the rapid nondestructive analysis of a conventional laboratory and does not accord with the development concept of green and environmental protection.
Disclosure of Invention
In order to solve the problems, the invention provides a heated cigarette aroma-carrying particle evaluation method based on GC-MS, which comprises the steps of extracting aroma substances volatilized by heating aroma-carrying particles through a headspace sample injector, and then rapidly analyzing the extracted gas phase substances through a gas chromatography-mass spectrometry combined method, so that the release amounts of aroma components carried by different types of aroma-carrying particles under the same condition are judged, and the aroma-carrying particles most suitable for heating cigarettes are determined. The method does not relate to the pretreatment process of an organic reagent, does not need to roll the aroma-carrying particles into the heated cigarette and then analyze the release amount of aroma components in the mainstream smoke of the cigarette, and is simple to operate and convenient to popularize.
In order to achieve the purpose, the technical scheme provided by the invention is as follows: a heated cigarette aroma-carrying particle evaluation method based on GC-MS is characterized by comprising the following steps:
s1, compounding essence and spice with a solvent, wherein the mass ratio of the solvent to the essence and spice is 370-: 1;
s2, spraying the essence and spice compounded in the step S1 into the aroma-carrying particles to be evaluated for perfuming, weighing the perfumed particles after fully and uniformly mixing, and placing the weighed perfumed particles into a headspace bottle;
s3, placing the headspace bottle containing the flavored particles in the step S2 in a headspace sample injector, heating to a certain temperature, balancing for a period of time, and injecting headspace gas into a sample inlet of a gas chromatograph-mass spectrometer for analysis;
s4, reading the response value of each fragrance component in the headspace gas through a gas chromatograph-mass spectrometer, quantifying by using a standard curve, and determining the concentration of each fragrance component in the headspace gas so as to determine the volatilization amount of each fragrance component in the flavoring particles;
the manufacturing method of the standard curve comprises the following steps: weighing 100 mu L of mixed essence and spice standard samples with different concentrations in a 20mL headspace bottle, setting the heating temperature to 160 ℃, heating and balancing for 30min, injecting 1mL headspace gas into a gas chromatograph-mass spectrometer sample inlet for analysis, and drawing by using the peak area of each fragrance component and the corresponding concentration of the mixed essence and spice standard samples to obtain a standard curve of the headspace GC-MS.
Further, the solvent in step S1 is ethanol.
Further, the essence and flavor in the step S1 includes at least one of alcohol essence and flavor, aldehyde essence and flavor, ketone essence and flavor, ester/lactone essence and flavor, acid essence and flavor, and phenol essence and flavor.
Further, the mass ratio of the essence and the flavor to the flavor-carrying particles in the step S2 is 0.01-0.3: 1.
Further, in step S2, 0.3-0.4g of the flavored granules are weighed and placed in a 20mL headspace bottle.
Further, in step S3, the headspace bottle containing the flavored particles is placed in a headspace sampler and heated to 40-160 ℃.
Further, after the heating in the step S3 is completed, balancing for 5-30min, and injecting headspace gas into a sample inlet of a gas chromatograph-mass spectrometer for analysis.
Further, in the step S3, 1mL or 3mL of headspace gas is injected into the sample inlet of the gas chromatograph-mass spectrometer for analysis.
The static headspace analysis method is a method that a sample is placed in a headspace bottle, after the sample is heated, volatile and semi-volatile substances in the sample reach thermal equilibrium in a solid (liquid) phase and a gas phase, and then a certain amount of gas above the headspace bottle is directly sucked for qualitative and quantitative analysis. The headspace analysis method only takes a gas phase part for analysis, so that the interference of a sample matrix on the analysis is greatly reduced, and if the headspace analysis method is used for extracting the fragrant substances, the interference of impurities brought by an organic solvent in the traditional extraction method on the analysis can be avoided.
The aroma substance extracted by headspace analysis is a gas substance, and the gas substance can be analyzed by gas chromatography-mass spectrometry. The gas chromatograph-mass spectrometer is used in medicine and physics, and has inert gas as the mobile phase and fixed phase of adsorbent with great surface area and certain activity. After a multi-component mixed sample enters a chromatographic column, due to the different adsorption force of the adsorbent to each component, the running speed of each component in the chromatographic column is different after a certain time. The less strongly adsorbed component is readily desorbed first from the column and enters the detector, whereas the most strongly adsorbed component is least readily desorbed and therefore leaves the column. In this way, the components are separated from each other in the column and sequentially detected and recorded in the detector.
The invention has the beneficial effects that:
1. the invention provides a heated cigarette aroma-carrying particle evaluation method based on GC-MS, which comprises the steps of extracting aroma substances volatilized by heating aroma-carrying particles through a headspace sample injector, and then rapidly analyzing the release amount of aroma components carried by the aroma-carrying particles through a gas chromatography-mass spectrometry combined method, thereby determining the aroma-carrying particles most suitable for heating cigarettes. The method does not relate to the pretreatment process of an organic reagent, does not need to roll the aroma-carrying particles into the heated cigarette and then analyze the release amount of aroma components in the mainstream smoke of the cigarette, and is simple to operate and convenient to popularize.
2. According to the heating cigarette aroma-carrying particle evaluation method based on GC-MS, after the standard curve is made, the standard curve can be used and compared for multiple times, the response value of each aroma component in the headspace gas is read through a gas chromatograph-mass spectrometer and compared with the response value of the standard curve, so that the content of each aroma component in the headspace gas is obtained, the accuracy is high, the repeatability is good, the subjectivity of artificial sensory evaluation is avoided, and the judgment result is more objective.
Drawings
FIG. 1 is a flow chart of a method for evaluating aroma-carrying particles of a heated cigarette based on GC-MS in an embodiment of the invention.
Detailed Description
In order to more clearly illustrate the embodiments of the present invention and the technical solutions in the prior art, the following will describe the specific embodiments of the present invention with reference to the accompanying drawings.
It is obvious that the drawings in the following description are only some examples of the invention, and it is obvious to a person skilled in the art that other drawings and other embodiments can be obtained from these drawings without inventive effort, and the invention is not limited to this example.
In the examples of the present invention, the chromatographic conditions were: HP-Innowax chromatography column (30 m 0.25 mm, 0.25 μm); carrier gas: high purity helium gas; carrier gas flow: 1.0 mL/min; sample introduction amount: 1 mu L of the solution; sample inlet temperature: 230 ℃; the split ratio is as follows: 10: 1; temperature programming: the starting temperature was 70 deg.C (held for 5 min) and increased to 230 deg.C (held for 8 min) at 5 deg.C/min.
Mass spectrum conditions: an Electron Impact (EI) ion source; electron energy 70 eV; ion source temperature: 230 ℃; transmission line temperature: 230 ℃; the mass range is as follows: m/z 33-300 amu.
The specific embodiment of the invention is as follows:
preliminary screening of conditions:
example 1
S1, preparing fragrance-carrying particles A for laboratories, and compounding essence and spice with ethanol, wherein the essence and spice comprises six fragrance components of citral, tea ketone, citronellol, heptanoic acid, cinnamaldehyde and methyl dihydrojasmonate, and the mass ratio of the citral, the tea ketone, the citronellol, the heptanoic acid, the cinnamaldehyde, the methyl dihydrojasmonate to the ethanol is 1: 1: 1: 1: 1: 1: 370;
s2, spraying the essence standard sample compounded in the step S1 into the aroma-carrying particles A to be evaluated for perfuming, wherein the mass ratio of the essence standard sample to the aroma-carrying particles A is 1:100, and after fully and uniformly mixing, weighing two parts of 0.3g of perfumed particles A and respectively placing the weighed parts into two 20mL headspace bottles;
s3, respectively placing the two headspace bottles containing the perfumed particles A in the step S2 into two headspace sample injectors, respectively balancing for 15 min at 60 ℃ and 120 ℃, respectively injecting 1mL of headspace gas into sample injection ports of a gas chromatograph-mass spectrometer for analysis, and reading peak areas of six perfume components in the perfumed particles A.
Example 2
S1, preparing fragrance-carrying particles A for laboratories, and compounding essence and spice with ethanol, wherein the essence and spice comprises six fragrance components of citral, tea ketone, citronellol, heptanoic acid, cinnamaldehyde and methyl dihydrojasmonate, and the mass ratio of the citral, the tea ketone, the citronellol, the heptanoic acid, the cinnamaldehyde, the methyl dihydrojasmonate to the ethanol is 1: 1: 1: 1: 1: 1: 370;
s2, spraying the essence standard sample compounded in the step S1 into the aroma-carrying particles A to be evaluated for perfuming, wherein the mass ratio of the essence standard sample to the aroma-carrying particles A is 1:10, and after fully and uniformly mixing, weighing two parts of 0.3g of perfumed particles A and respectively placing the weighed two parts into two 20mL headspace bottles;
s3, respectively placing the two headspace bottles containing the perfumed particles A in the step S2 into two headspace sample injectors, respectively balancing for 15 min at 60 ℃ and 120 ℃, respectively injecting 1mL of headspace gas into sample injection ports of a gas chromatograph-mass spectrometer for analysis, and reading peak areas of six perfume components in the perfumed particles A.
Example 3
S1, preparing fragrance-carrying particles A for laboratories, and compounding essence and spice with ethanol, wherein the essence and spice comprises six fragrance components of citral, tea ketone, citronellol, heptanoic acid, cinnamaldehyde and methyl dihydrojasmonate, and the mass ratio of the citral, the tea ketone, the citronellol, the heptanoic acid, the cinnamaldehyde, the methyl dihydrojasmonate to the ethanol is 1: 1: 1: 1: 1: 1: 370;
s2, spraying the essence standard sample compounded in the step S1 into the aroma-carrying particles A to be evaluated for perfuming, wherein the mass ratio of the essence standard sample to the aroma-carrying particles A is 3:10, and after fully and uniformly mixing, weighing two parts of 0.4g of perfumed particles A and respectively placing the weighed two parts into two 20mL headspace bottles;
s3, respectively placing the two headspace bottles containing the perfumed particles A in the step S2 into two headspace sample injectors, respectively balancing for 15 min at 60 ℃ and 120 ℃, respectively injecting 1mL of headspace gas into sample injection ports of a gas chromatograph-mass spectrometer for analysis, and reading peak areas of six perfume components in the perfumed particles A.
The result shows that the peak areas of the six flavor components in the flavoring particle A are read to be smaller due to the lower content of the flavors and fragrances in the example 1, and the flavoring particle A is not suitable for cigarette making. The content of the essence and the spice in example 3 is high, and the peak areas of the six aroma components in the read flavoring particles A are high, so that the method is not suitable for cigarette manufacture. Therefore, the conditions of example 2 were selected as the conditions for preparing the calibration curve in the present invention.
And (3) preparing a standard curve:
example 4
S1, compounding essence and spice with ethanol, and compounding essence and spice standard samples with seven concentrations of 10 mug/g, 20 mug/g, 40 mug/g, 80 mug/g, 160 mug/g, 320 mug/g and 640 mug/g respectively by compounding essence and spice with different masses with ethanol solvent;
the essence is any one of six fragrance components of citral, tea ketone, citronellol, heptanoic acid, cinnamaldehyde and methyl dihydrojasmonate, namely seven essence standard samples with different concentrations are contained in the six fragrance components;
s2, adding the essence and spice standard samples with different concentrations compounded in the 100 mu L step S1 into corresponding 20mL headspace bottles respectively, wherein each concentration is a group, namely seven concentrations of six aroma components, namely 10 microgram/g, 20 microgram/g, 40 microgram/g, 80 microgram/g, 160 microgram/g, 320 microgram/g and 640 microgram/g are grouped, and forty two groups are provided in the embodiment of the invention;
s3, heating forty two groups in the step S2 to 160 ℃ respectively, balancing for 30min, injecting 1mL of headspace gas into a sample inlet of a gas chromatograph-mass spectrometer respectively, and analyzing to obtain peak areas corresponding to six kinds of aroma components at seven concentrations of 10 mug/g, 20 mug/g, 40 mug/g, 80 mug/g, 160 mug/g, 320 mug/g and 640 mug/g. And then, drawing the peak area of each fragrance component and the concentration of each fragrance component in the corresponding mixed essence standard sample to obtain six linear equations. Wherein y is a peak area, and x is the concentration of the fragrance component in the standard sample of the mixed essence and spice. The results are shown in Table 1.
TABLE 1 Linear equation and correlation coefficient of fragrance composition under static headspace GC/MS analysis method
As can be seen from Table 1, the linear relationship between the peak area and the concentration of the standard curve is good in the measured content range, and the correlation coefficient range of the regression equation is between 0.995 and 0.999. The correlation coefficient is close to 1, the error is small, and the concentration of the fragrance component in the gas can be directly obtained by introducing the peak area through a linear equation in the later period, so that the volatilization quantity of the essence and the spice in the fragrant particles is determined.
And (3) judging different aroma-carrying particles:
example 5
S1, preparing fragrance-carrying particles A for laboratories, and compounding essence and spice with ethanol, wherein the essence and spice comprises six fragrance components of citral, tea ketone, citronellol, heptanoic acid, cinnamaldehyde and methyl dihydrojasmonate, and the mass ratio of the citral, the tea ketone, the citronellol, the heptanoic acid, the cinnamaldehyde, the methyl dihydrojasmonate to the ethanol is 1: 1: 1: 1: 1: 1: 370;
s2, spraying the essence standard sample compounded in the step S1 into the aroma-carrying particles A to be evaluated for perfuming, wherein the mass ratio of the essence standard sample to the aroma-carrying particles A is 1:10, and after fully and uniformly mixing, weighing two parts of 0.3g of perfumed particles A and respectively placing the weighed two parts into two 20mL headspace bottles;
s3, placing the two headspace bottles containing the perfumed particles A in the step S2 into two headspace sample injectors respectively, balancing at 60 ℃ and 120 ℃ for 15 min respectively, then injecting 1mL of headspace gas into sample injection ports of a gas chromatograph-mass spectrometer respectively for analysis, reading peak areas of six fragrance components in the perfumed particles A, and respectively substituting the peak areas into linear equations corresponding to the example 1 to obtain respective concentrations of the six fragrance components in the gas released by the perfumed particles A.
Example 6
S1, preparing fragrance-carrying particles B for laboratories, and compounding essence and spice with ethanol, wherein the essence and spice comprises six fragrance components of citral, tea ketone, citronellol, heptanoic acid, cinnamaldehyde and methyl dihydrojasmonate, and the mass ratio of the citral, the tea ketone, the citronellol, the heptanoic acid, the cinnamaldehyde, the methyl dihydrojasmonate to the ethanol is 1: 1: 1: 1: 1: 1: 370;
s2, spraying the essence standard sample compounded in the step S1 into the aroma-carrying particles B to be evaluated for perfuming, wherein the mass ratio of the essence standard sample to the aroma-carrying particles B is 1:10, and after fully and uniformly mixing, weighing two parts of 0.3g of perfumed particles B and respectively placing the weighed two parts into two 20mL headspace bottles;
s3, placing the two headspace bottles containing the perfumed particles B in the step S2 into two headspace sample injectors respectively, balancing for 15 min at 60 ℃ and 120 ℃, then injecting 1mL of headspace gas into sample injection ports of a gas chromatograph-mass spectrometer respectively for analysis, reading peak areas of six fragrance components in the perfumed particles B, and respectively substituting the peak areas into linear equations corresponding to example 1 to obtain respective concentrations of the six fragrance components in the gas released by the perfumed particles B.
Example 7
S1, preparing fragrance-carrying particles C for laboratories, and compounding essence and spice with ethanol, wherein the essence and spice comprises six fragrance components of citral, tea ketone, citronellol, heptanoic acid, cinnamaldehyde and methyl dihydrojasmonate, and the mass ratio of the citral, the tea ketone, the citronellol, the heptanoic acid, the cinnamaldehyde, the methyl dihydrojasmonate to the ethanol is 1: 1: 1: 1: 1: 1: 370;
s2, spraying the essence standard sample compounded in the step S1 into the aroma-carrying particles C to be evaluated for perfuming, wherein the mass ratio of the essence standard sample to the aroma-carrying particles C is 1:10, and after fully and uniformly mixing, weighing two parts of 0.3g of perfumed particles C and respectively placing the weighed two parts into two 20mL headspace bottles;
s3, placing the two headspace bottles containing the perfumed particles C in the step S2 into two headspace sample injectors respectively, balancing at 60 ℃ and 120 ℃ for 15 min respectively, then injecting 3mL of headspace gas into sample injection ports of a gas chromatograph-mass spectrometer respectively for analysis, reading peak areas of six fragrance components in the perfumed particles C, and respectively substituting the peak areas into linear equations corresponding to the example 1 to obtain respective concentrations of the six fragrance components in the gas released by the perfumed particles C.
Analysis of the results of examples 5 to 7:
taking two temperatures of 60 ℃ and 120 ℃ as measurement standards, taking the sum of the concentration of the fragrance component in the gas released by the perfuming particle at the temperature of 60 ℃ and the concentration of the fragrance component in the gas released by the perfuming particle at the temperature of 120 ℃ as a comprehensive evaluation index of the release amount at different temperatures, wherein the higher the evaluation index is, the larger the total release amount of the perfuming particles at the two temperatures is.
The total release at 60 ℃ and 120 ℃ of the fragrance-loaded granules of examples 5 to 7, respectively, was calculated and tabulated below.
TABLE 2 Total fragrance ingredient Release from perfuming granules at 60 ℃ and 120 ℃
As can be seen from Table 2, the total release amounts of the six flavor components in flavor-bearing particle A at 60 ℃ and 120 ℃ were larger than those of flavor-bearing particle B and flavor-bearing particle C. Namely, the aroma-carrying particle A is the most suitable aroma-carrying particle for heating cigarettes in the three types of particles, and the aroma component amount released in the smoking process is the largest.
In order to verify the actual application effect of the three types of flavoring particles in the embodiment 5-7 of the invention in heating cigarettes, the experimental cigarette A, the experimental cigarette B and the experimental cigarette C are sequentially prepared by using three types of flavoring particles on a machine, a unified test sheet is adopted when the cigarettes are rolled, parameters of other auxiliary materials are kept consistent except for different flavoring particles, and the content of the flavor components in the main stream smoke of the experimental cigarettes is analyzed according to the following method.
The suction method comprises the following steps: adopting an IQOS smoking set according to ISO/FDIS 20768: 2018 aerosol conventional analysis smoking using electronic cigarette smoking machine definition and standard conditions. 8 cigarettes are prepared for each of the three experimental cigarettes for smoking, and mainstream smoke of every 4 cigarettes is captured on one 44 mm Cambridge filter, namely smoke generated by smoking of each experimental cigarette is captured on two corresponding filters.
The extraction method comprises the following steps: after pumping, placing two filter discs of each of the three samples in a 100 mL conical flask, adding dichloromethane solution containing an internal standard, performing oscillation extraction for 30min at the rotating speed of 160 r/min, transferring extract liquor into a concentration flask, concentrating the extract liquor to about 0.8 mL at normal pressure through a rotary evaporator, filtering the extract liquor through a 0.22 mu m organic filter membrane, detecting the extract liquor by using a gas chromatograph-mass spectrometer, and analyzing the flavor components in the mainstream smoke by using GC/MS, wherein the chromatographic conditions and the mass spectrum conditions are the same as those in the embodiments 2-4 of the invention.
Table 3 reflects the release amounts of six flavor components in the mainstream smoke of three experimental cigarettes, and as can be seen from Table 3, the release amounts of 6 flavor components in the mainstream smoke of the heated cigarette made of the flavoring particles A are all the highest, which is completely consistent with the result of directly analyzing the flavoring particles by a static headspace GC/MS method. Thus, the evaluation of three fragrance-loaded particles is fully feasible in inventive examples 5-7.
The results of the release amount of the flavor components in the mainstream smoke of the experimental cigarettes prepared by the three types of flavoring particles are shown in table 3.
TABLE 3-release amount of flavor components in mainstream smoke of experimental cigarettes prepared from three kinds of flavoring particles
The above-described aspects may be implemented individually or in various combinations, and such variations are within the scope of the present invention.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
The foregoing is a more detailed description of the invention in connection with specific preferred embodiments and it is not intended that the specific embodiments of the invention be limited to these descriptions. For those skilled in the art to which the invention pertains, several simple deductions or substitutions can be made without departing from the spirit of the invention, and all shall be considered as belonging to the protection scope of the invention.
Claims (8)
1. A heated cigarette aroma-carrying particle evaluation method based on GC-MS is characterized by comprising the following steps:
s1, compounding essence and spice with a solvent, wherein the mass ratio of the solvent to the essence and spice is 370-: 1;
s2, spraying the essence and spice compounded in the step S1 into the aroma-carrying particles to be evaluated for perfuming, weighing the perfumed particles after fully and uniformly mixing, and placing the weighed perfumed particles into a headspace bottle;
s3, placing the headspace bottle containing the flavored particles in the step S2 in a headspace sample injector, heating and balancing for a period of time, and injecting headspace gas into a sample inlet of a gas chromatograph-mass spectrometer for analysis;
s4, reading the response value of each fragrance component in the headspace gas through a gas chromatograph-mass spectrometer, quantifying by using a standard curve, and determining the concentration of each fragrance component in the headspace gas so as to determine the volatilization amount of each fragrance component in the flavoring particles;
the manufacturing method of the standard curve comprises the following steps: weighing 100 mu L of mixed essence and spice standard samples with different concentrations in a 20mL headspace bottle, setting the heating temperature to 160 ℃, heating and balancing for 30min, injecting 1mL headspace gas into a gas chromatograph-mass spectrometer sample inlet for analysis, and drawing by using the peak area of each fragrance component and the corresponding concentration of the mixed essence and spice standard samples to obtain a standard curve of the headspace GC-MS.
2. The method for evaluating the aroma-carrying particles of the heated cigarette based on GC-MS as claimed in claim 1, wherein the solvent in step S1 is ethanol.
3. The method for evaluating the aroma-carrying particles of the heated cigarette based on the GC-MS as claimed in claim 1, wherein the flavors and fragrances in the step S1 include at least one of alcohol flavors and fragrances, aldehyde flavors and fragrances, ketone flavors and fragrances, ester/lactone flavors and fragrances, acid flavors and phenol flavors and fragrances.
4. The method for evaluating the aroma-carrying particles of the heated cigarette based on the GC-MS as claimed in claim 1, wherein the mass ratio of the flavors and fragrances to the aroma-carrying particles in the step S2 is 0.01-0.3: 1.
5. The method for evaluating the flavor-loaded particles of the heated cigarettes based on the GC-MS as claimed in claim 1, wherein 0.3-0.4g of the flavored particles are weighed in a 20mL headspace bottle in the step S2.
6. The method for evaluating the aroma-carrying particles of the heated cigarettes based on GC-MS as claimed in claim 1, wherein the headspace bottle containing the flavored particles is placed in a headspace sampler and heated to 40-160 ℃ in step S3.
7. The method for evaluating the aroma-carrying particles of the heated cigarettes based on the GC-MS as claimed in claim 7, wherein the headspace gas is taken out and injected into a sample inlet of a gas chromatograph-mass spectrometer for analysis after the heating in the step S3 is completed and the balance is 5-30 min.
8. The method for evaluating the aroma-carrying particles of the heated cigarette based on the GC-MS as claimed in claim 1, wherein 1mL or 3mL of headspace gas is taken in the step S3 and injected into a sample inlet of a gas chromatograph-mass spectrometer for analysis.
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