CN113109483A - Analysis method for pyrolysis aroma components of potentially-fragrant raw material for cigarettes - Google Patents

Analysis method for pyrolysis aroma components of potentially-fragrant raw material for cigarettes Download PDF

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CN113109483A
CN113109483A CN202110496975.8A CN202110496975A CN113109483A CN 113109483 A CN113109483 A CN 113109483A CN 202110496975 A CN202110496975 A CN 202110496975A CN 113109483 A CN113109483 A CN 113109483A
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aroma
temperature
sample
chromatographic column
raw materials
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CN113109483B (en
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梁德民
王嘉乐
费婷
张玮
吴秉宇
罗辰
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Shanghai Tobacco Group Co Ltd
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Shanghai Tobacco Group Co Ltd
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    • G01N30/04—Preparation or injection of sample to be analysed
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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
    • G01N30/26—Conditioning of the fluid carrier; Flow patterns
    • G01N30/28—Control of physical parameters of the fluid carrier
    • G01N30/30—Control of physical parameters of the fluid carrier of temperature
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    • 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
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    • G01N30/26—Conditioning of the fluid carrier; Flow patterns
    • G01N30/38—Flow patterns
    • G01N30/46—Flow patterns using more than one column
    • G01N30/461—Flow patterns using more than one column with serial coupling of separation columns
    • G01N30/482—
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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
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    • G01N30/02—Column chromatography
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    • G01N30/02—Column chromatography
    • G01N30/26—Conditioning of the fluid carrier; Flow patterns
    • G01N30/28—Control of physical parameters of the fluid carrier
    • G01N30/32—Control of physical parameters of the fluid carrier of pressure or speed
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Abstract

The invention provides a method for analyzing pyrolysis aroma components of potentially fragrant raw materials for cigarettes, which comprises the steps of adding an aroma raw material sample into an organic solvent for dissolving, and then adopting a temperature rise program sample introduction and a gas chromatography-mass spectrometry/smell identification method of a sample inlet for determination; the method comprises the steps of obtaining integral aroma by pyrolyzing an aroma raw material sample through a first chromatographic column in gas chromatography, and determining the smell information of the integral aroma by adopting smell discrimination; and (3) pyrolyzing a fragrance raw material sample through a second chromatographic column in the gas chromatography to obtain a plurality of fragrance components, determining the fragrance components and the release content thereof by adopting a mass spectrum, and determining the odor information of the fragrance components by adopting olfactory discrimination. The invention further provides an analysis device for the pyrolysis aroma components of the potentially fragrant raw materials for cigarettes and application of the analysis device. The method for analyzing the pyrolysis aroma components of the potentially aromatic raw materials for cigarettes, provided by the invention, can be used for not only qualitatively cracking products, but also clarifying the aroma characteristics and the odor intensity of the products, and has the advantages of simplicity, accuracy, rapidness, reliability, high efficiency, high sensitivity and good stability.

Description

Analysis method for pyrolysis aroma components of potentially-fragrant raw material for cigarettes
Technical Field
The invention belongs to the technical field of tobacco essence and flavor analysis, and relates to an analysis method for pyrolysis aroma components of a potentially aromatic raw material for tobacco.
Background
The tobacco essence perfume is an essential component of the cigarette, can coordinate the formula of the cigarette leaf group, endows the cigarette with characteristic aroma style, and ensures the stability of the smoking quality of the cigarette. Many excellent flavors and fragrances have limited wide application in cigarettes due to problems of too strong volatility, poor stability, short fragrance retention time and the like, so in recent years, a novel flavor release technology becomes a hotspot for research and application of flavors and fragrances for cigarettes, such as potentially fragrant raw materials.
The latent odor type fragrance raw material is a substance which has no fragrance or no obvious fragrance, but can be cracked to generate a fragrance substance in the heating process and the like, and release a fragrance component which is increased or improved. The latent fragrant substance has the characteristics of weak volatility, stable chemical property and the like under natural conditions, and is in a tasteless or slightly flavored stable structure state when the latent fragrant substance is added into a cigarette and is not combusted, so that the latent fragrant substance is cracked at a lower pyrolysis temperature and releases a large amount of fragrance components capable of enhancing main stream smoke and side stream smoke when the cigarette is combusted, and the release amount of the fragrance is expected to be basically consistent in the combustion process of the cigarette, thereby achieving a stable smoke fragrance compensation effect. The pyrolysis temperature range of the potentially fragrant raw materials is generally 150-400 ℃.
The development and application process of the formula of the essence and spice for the cigarettes needs to master the information of the aroma characteristics, the types, the release amount, the strength and the like of various aroma raw materials in smoke, but as the latent aroma type aroma raw materials are stored at normal temperature and are in a basically odorless state, the aroma characteristics can not be identified as the conventional essence and spice, and the release amount can not be detected through the conventional gas chromatography or gas chromatography mass spectrometry. The thermal cracking-gas chromatography-mass spectrometry combined method can be used for thermal cracking analysis of the latent fragrant raw materials, but is only limited to qualitative analysis, the types of the cracking products can be clarified, and the fragrance characteristics and the intensity cannot be distinguished at the same time. Therefore, the prior art cannot meet the requirements of developing and applying latent fragrance raw materials.
Disclosure of Invention
In view of the above disadvantages of the prior art, an object of the present invention is to provide an analysis method for pyrolysis aroma components of latent odor type aroma raw materials for cigarettes, which can simulate pyrolysis of the latent odor type aroma raw materials to determine the overall aroma characteristics of the pyrolysis aroma of the latent odor type aroma raw materials and the aroma characteristics, the release amount of odorants, and the aroma intensity of pyrolysis products, and the method has the advantages of simplicity, accuracy, rapidness, reliability, high sensitivity, and good stability.
In order to achieve the above objects and other related objects, a first aspect of the present invention provides a method for analyzing pyrolytic aroma components of latent odor type aroma raw materials for cigarettes, comprising the steps of adding an aroma raw material sample into an organic solvent for dissolution, and then performing temperature-rise sample injection and gas chromatography-mass spectrometry/olfactory identification (GC-MS/O) measurement by using a sample injection port; the method comprises the steps of obtaining integral aroma by pyrolyzing an aroma raw material sample through a first chromatographic column in gas chromatography, and determining the smell information of the integral aroma by adopting smell discrimination; and (3) pyrolyzing a fragrance raw material sample through a second chromatographic column in the gas chromatography to obtain a plurality of fragrance components, determining the fragrance components and the release content thereof by adopting a mass spectrum, and determining the odor information of the fragrance components by adopting olfactory discrimination.
Preferably, the perfume raw material is latent aroma raw material for cigarettes.
More preferably, the latent odor type fragrance raw material for the cigarettes is glucoside or acetal.
Preferably, before the aroma raw material sample is added with the organic solvent for dissolution, a thermal weight loss method is adopted for analysis, and the pyrolysis temperature range and the temperature reaching the maximum weight loss speed in the pyrolysis temperature range are determined.
The determination of the pyrolysis temperature range and the temperature reaching the maximum weight loss speed in the pyrolysis temperature range is a conventional analysis result of a thermal weight loss method, and can be specifically determined by adopting a thermal weight loss diagram obtained by analysis of a thermal weight loss analyzer.
More preferably, in the thermal weight loss method, the aroma raw material sample is put into an aluminum crucible and analyzed by a thermal weight loss analyzer.
More preferably, in the thermogravimetric method, the analysis atmosphere is a nitrogen atmosphere.
More preferably, in the thermal weight loss method, the flow rate is 10-30 mL/min.
More preferably, in the thermogravimetric method, the temperature-increasing procedure is: the initial temperature is 30-80 ℃, and the temperature is increased to 300-500 ℃ at 10-50 ℃.
More preferably, in the thermogravimetric method, the temperature-raising procedure is: the initial temperature was 50 ℃ and was raised to 500 ℃ at 20 ℃.
Preferably, the organic solvent is selected from one or more of methanol, ethanol, isopropanol, ethyl acetate, diethyl ether, tert-butyl methyl ether and n-hexane.
Preferably, the ratio of the mass mg added to the fragrance raw material sample to the volume mL added of the organic solvent is 5: 5-15, preferably 5: 10.
preferably, the dissolving is ultrasonic dissolving, and the ultrasonic dissolving time is 2-10 min.
Preferably, the injection port is selected from one of a temperature programmed gasification injection Port (PTV) or a multimode injection port (MMI). The functions of low-temperature sample injection, rapid temperature rise, solvent evacuation and the like can be realized, and the maximum temperature of a sample injection port is more than 400 ℃.
Preferably, the temperature rise program of the sample inlet is that the temperature is kept for 0.1-5 min at 40-80 ℃, the temperature is raised to the temperature which reaches the maximum weight loss speed in the pyrolysis temperature range of the perfume raw material sample at 300-900 ℃/min and is kept for 5-30 min, and the temperature is 10-100 ℃.
More preferably, the temperature rise program of the sample inlet is to maintain the temperature at 60 ℃ for 0.2min, raise the temperature at 900 ℃/min to the temperature which reaches the maximum weight loss speed in the pyrolysis temperature range of the fragrance raw material sample and maintain the temperature for 10min, wherein the temperature reaches the maximum weight loss speed plus 10-100 ℃.
Further preferably, the temperature rise program of the injection port is that the temperature is kept for 0.2min at 60 ℃, the temperature is raised to the temperature which reaches the maximum weight loss speed in the pyrolysis temperature range of the fragrance raw material sample at 900 ℃/min and is kept for 10min, and the temperature is 55-61 ℃.
Preferably, in the determination conditions of the gas chromatography, the sample injection mode is a non-flow splitting mode or a solvent emptying mode.
Preferably, the flow rate in the measuring condition of the gas chromatography is 0.8-2 mL/min.
Preferably, in the determination conditions of the gas chromatography, the first chromatographic column is a deactivated stationary phase-free capillary chromatographic column.
Preferably, in the determination conditions of the gas chromatography, the second chromatographic column is selected from one of DB-5ms, DB-wax, DB-17, DB-624 or Supelco-VOCOL capillary chromatographic columns.
Preferably, in the measurement conditions of the gas chromatography, the operation temperature of the column oven is 205-215 ℃, preferably 210 ℃ when measuring the whole aroma.
Preferably, in the measurement conditions of the gas chromatography, when the aroma components are measured, the temperature raising program of the column oven is to maintain the temperature at 60 ℃ for 1min, raise the temperature at 4 ℃/min to 180 ℃, and then raise the temperature at 10 ℃/min to 230 ℃ for 10 min.
The column oven is used for placing a chromatographic column in a gas chromatograph.
Preferably, the determination conditions of the mass spectrum are: the ionization source energy is 70 eV; the ion source temperature is 230 ℃; the transmission line temperature is 250 ℃; the scanning mode is scan; the scanning range is 35-300 m/z, and the temperature of the auxiliary heating transmission line (ODP) is 240 ℃.
Preferably, the qualitative method for determining the pyrolysis product by mass spectrometry is selected from one or more of NIST mass library retrieval compound structural formula qualitative determination, Wieley mass library retrieval compound structural formula qualitative determination and retention index qualitative determination.
Preferably, the method for measuring the release content of the aroma components is selected from one or more of an internal standard method, an external standard method and a peak area normalization method.
The internal standard method is a standard curve method or a standard one-point method which is used conventionally in a gas chromatography-mass spectrometry combined method and is added with an internal standard. The external standard method is a standard curve method or a standard one-point method which is conventionally used in a gas chromatography-mass spectrometry combined method. The peak area normalization method is a peak area normalization method which is conventionally used in a gas chromatography-mass spectrometry combined method.
Preferably, the odour information comprises odour characteristics and odour intensity.
The olfactive method (Odor) is conventionally used in the tobacco field, and adopts artificial sensory olfactive in the olfactive mouth, namely, a olfactive group consisting of sniffing personnel trained by a system carries out olfactive analysis on aroma.
The invention provides an analysis device for pyrolyzing aroma components of latent odor type aroma raw materials for cigarettes, which comprises a gas chromatography part and a mass spectrum part, wherein the gas chromatography part comprises a column incubator, a first chromatographic column and a second chromatographic column are arranged in the column incubator, and the column incubator is provided with a sample inlet and a smell distinguishing port; the sample inlet end of the first chromatographic column is communicated with the sample inlet, and the sample outlet end of the first chromatographic column is respectively communicated with the sample inlet end and the smell identification port of the second chromatographic column; the sample outlet end of the second chromatographic column is respectively communicated with the sniffing port and the mass spectrum part.
Preferably, a liner tube is arranged in the sample inlet and is communicated with the sample inlet end of the first chromatographic column.
More preferably, the liner tube is a flow-dividing and flow-non-dividing liner tube with glass wool, and the inner diameter of the liner tube is 3-5 mm, preferably 4 mm; the volume is 0.8 to 0.9mL, preferably 0.87 mL.
Preferably, a first three-way connector is arranged at the sample outlet end of the first chromatographic column, and a second three-way connector is arranged at the sample outlet end of the second chromatographic column; the first interface of the first three-way connector is communicated with the sample outlet end of the first chromatographic column, the second interface of the first three-way connector is communicated with the sample inlet end of the second chromatographic column, and the third interface of the first three-way connector is communicated with the sniffing port through a pipeline; the first interface of the second three-way connector is communicated with the sample outlet end of the second chromatographic column, the second interface of the second three-way connector is communicated with the sniffing port through a pipeline, and the third interface of the second three-way connector is communicated with the mass spectrum part through a pipeline.
More preferably, be equipped with first control valve between the appearance end of first three way connection ware and second chromatographic column, be equipped with the second control valve on the pipeline between first three way connection ware and the smelling mouth.
The invention provides application of an analysis device for pyrolysis aroma components of potentially fragrant raw materials for cigarettes in analysis of the pyrolysis aroma components of the aroma raw materials.
As mentioned above, the method for analyzing the pyrolysis aroma components of the potentially fragrant raw material for the cigarettes provided by the invention has the following beneficial effects:
(1) the method for analyzing the pyrolysis aroma components of the latent aroma type raw materials for the cigarettes can simulate the pyrolysis of the aroma raw materials, particularly the latent aroma type aroma raw materials, and realize the measurement of the integral aroma information of the latent aroma type aroma raw materials and the aroma information of a plurality of aroma components. Compared with the traditional thermal cracking-gas chromatography-mass spectrometry combined method, the method not only can qualitatively crack the product, but also can clarify the fragrance characteristics and the odor intensity of the product.
(2) According to the analysis method for the pyrolysis aroma components of the potentially aromatic raw materials for the cigarettes, provided by the invention, the pyrolysis temperature interval and the maximum weight loss speed of the potentially aromatic raw materials are rapidly determined through thermogravimetric analysis, and a basis is provided for the pyrolysis temperature rise of a sample inlet.
(3) According to the method for analyzing the pyrolysis aroma components of the potentially fragrant raw materials for cigarettes, the defect that an online pyrolysis process cannot be simulated by a gas chromatography split-flow/non-split-flow sample inlet is overcome through a special gas chromatography sample inlet (a temperature programming sample inlet or a multi-mode sample inlet), and the defects of large investment, long analysis time consumption and the like of a thermal cracking instrument are overcome.
(4) The invention provides an analysis method of pyrolysis aroma components of latent aroma type raw materials for cigarettes, which adopts a gas chromatography-mass spectrometry/smell identification measurement technology (GC-MS/O) and can comprehensively grasp the overall odor characteristics of pyrolysis products of the latent aroma type raw materials, the odor characteristics, the odor intensity, the types of the pyrolysis products, the release content and other information of the pyrolysis products one by one through the adjustment of instrument parameters.
(5) The method for analyzing the pyrolysis aroma components of the potentially aromatic raw materials for cigarettes has the advantages of simplicity, accuracy, rapidness, reliability, high efficiency, high sensitivity and good stability, is suitable for rapid analysis and detection of a large batch of potentially aromatic raw materials, realizes rapid screening of the potentially aromatic raw materials, and is better applied to cigarette blending.
Drawings
FIG. 1 is a schematic structural diagram of an analysis device for pyrolysis aroma components of latent aroma raw materials for cigarettes in the invention.
Fig. 2 shows a thermogravimetric plot of glycoside in pyrolysis aroma of latent aroma raw material for cigarette in example 1 of the present invention, wherein curve 1 is a change curve of glycoside mass with temperature, and curve 2 is a change curve of glycoside mass change rate with temperature.
FIG. 3 shows the pyrolysis mass spectrum of glycoside in pyrolysis aroma of latent aroma raw material for cigarette in example 1 of the present invention.
Fig. 4 shows a thermogravimetric plot of acetal in pyrolysis aroma of potentially fragrant raw material for cigarette in example 2 of the present invention, wherein curve 1 is a change curve of acetal mass with temperature, and curve 2 is a change curve of acetal mass change rate with temperature.
FIG. 5 shows the mass spectrum of acetal pyrolysis in the pyrolysis of raw material of latent aroma for cigarette in example 2 of the present invention.
Reference numerals
1 liner tube
2 sample inlet
3 first control valve
4 first chromatographic column
5 second chromatography column
6 sniff mouth
7 Mass Spectrometry section
8 second three-way connector
81 first interface of second three-way connector
82 second interface of second three-way connector
83 third interface of second three-way connector
9 second control valve
10 first three-way connector
101 first interface of first three-way connector
102 second interface of the first three-way connector
103 third interface of the first three-way connector
11 column incubator
Detailed Description
The present invention is further illustrated below with reference to specific examples, which are intended to be illustrative only and not to limit the scope of the invention.
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention.
The invention provides an analysis device for pyrolysis aroma components of potentially fragrant raw materials for cigarettes, which comprises a gas chromatography part and a mass spectrum part, wherein the gas chromatography part comprises a column incubator, a first chromatographic column and a second chromatographic column are arranged in the column incubator, and the column incubator is provided with a sample inlet and a smell identification port; the sample inlet end of the first chromatographic column is communicated with the sample inlet, and the sample outlet end of the first chromatographic column is respectively communicated with the sample inlet end and the smell identification port of the second chromatographic column; the sample outlet end of the second chromatographic column is respectively communicated with the sniffing port and the mass spectrum part.
In the analysis device for the pyrolysis aroma components of the latent aroma raw materials for cigarettes, the gas chromatography part is a gas chromatograph which is used conventionally, and the mass spectrometry part is a mass spectrometer which is used conventionally. Such as 7890B/5977A GC-MS combined instrument.
In the analysis device for the pyrolysis aroma components of the potentially fragrant raw material for the cigarette, as shown in fig. 1, a liner tube is arranged in the sample inlet and is communicated with the sample inlet end of the first chromatographic column. For inputting the sample.
In a specific embodiment, the liner tube is a flow-dividing and flow-non-dividing liner tube with glass wool, and the inner diameter of the liner tube is 3-5 mm, preferably 4 mm; the volume is 0.8 to 0.9mL, preferably 0.87 mL.
In the analysis device for the pyrolysis aroma components of the potentially fragrant raw materials for cigarettes, as shown in fig. 1, a first three-way connector is arranged at the sample outlet end of the first chromatographic column, and a second three-way connector is arranged at the sample outlet end of the second chromatographic column; the first interface of the first three-way connector is communicated with the sample outlet end of the first chromatographic column, the second interface of the first three-way connector is communicated with the sample inlet end of the second chromatographic column, and the third interface of the first three-way connector is communicated with the sniffing port through a pipeline; the first interface of the second three-way connector is communicated with the sample outlet end of the second chromatographic column, the second interface of the second three-way connector is communicated with the sniffing port through a pipeline, and the third interface of the second three-way connector is communicated with the mass spectrum part through a pipeline.
In a specific embodiment, as shown in fig. 1, a first control valve is disposed between the first three-way connector and the sample inlet end of the second chromatographic column, and a second control valve is disposed on a pipeline between the first three-way connector and the sniffing port.
Example 1
1. Thermogravimetric analysis
5mg of glycoside sample # 1 with unknown composition was weighed, placed in an aluminum crucible with a volume of 100 microliters, and analyzed with a thermogravimetric analyzer. The flow rate is set to be 20.0mL/min, the initial temperature of the thermal weight loss instrument is 50 ℃, then the temperature is increased to 500 ℃ at 20 ℃/min, and the test is carried out under the nitrogen atmosphere. The results of the thermogravimetric tests of glycoside sample # 1 are shown in figure 2. As can be seen from FIG. 2, the pyrolysis temperature range of glycoside sample No. 1 is 245-278 deg.C, where the maximum weight loss rate is reached at 265 deg.C.
2. Sample pretreatment
Weighing 5mg of glucoside sample No. 1, adding 10mL of methanol, dissolving by ultrasonic wave for 10min, taking 2mL of sample, placing in a chromatographic analysis bottle, and performing sample loading determination by gas chromatography-mass spectrometry/olfactory discrimination method (GC-MS/O), wherein the specific analysis device is shown in figure 1.
3. Measurement of Whole fragrance
And (3) inputting the glucoside sample No. 1 into a gas chromatography part through a liner tube through a sample inlet, and injecting the sample through an Agilent multimode MMI sample inlet. The temperature rise program of the sample inlet is that the temperature is kept for 0.2min at 60 ℃, the temperature is raised to 320 ℃ at 900 ℃/min, the temperature is kept for 10min, and the mode of no shunt is adopted.
And closing the first control valve, opening the second control valve, and pyrolyzing the whole aroma obtained by the glucoside sample 1# through a first chromatographic column in the gas chromatography, wherein the first chromatographic column is a capillary chromatographic column without an active and stationary phase. The column oven was operated with 210 ℃ being maintained. And performing sniffing through a sniffing mouth to determine the smell information of the whole aroma. The overall aroma olfactory results for glycoside sample # 1 are: has fragrance of orange and lemon.
4. Measurement of aroma component
And (3) inputting the glucoside sample No. 1 into a gas chromatography part through a liner tube through a sample inlet, and injecting the sample through an Agilent multimode MMI sample inlet. The temperature rise program of the sample inlet is that the temperature is kept for 0.2min at 60 ℃, the temperature is raised to 320 ℃ at 900 ℃/min, the temperature is kept for 10min, and the mode of no shunt is adopted.
And opening the first control valve, closing the second control valve, and pyrolyzing a plurality of aroma components obtained by pyrolyzing the glycoside sample 1# through a second chromatographic column in the gas chromatography after the glycoside sample 1# flows through the first chromatographic column in the gas chromatography, wherein the second chromatographic column is a DB-wax chromatographic column. The temperature raising program of the column incubator is that the temperature is maintained at 60 ℃ for 1min, the temperature is raised to 180 ℃ at 4 ℃/min, and then the temperature is raised to 230 ℃ at 10 ℃/min and maintained for 10 min.
And determining the aroma components and the release content thereof by adopting a mass spectrum, wherein the determination conditions of the mass spectrum are as follows: the ionization source energy is 70 eV; the ion source temperature is 230 ℃; the transmission line temperature is 250 ℃; the scanning mode is scan; the scanning range is 35-300 m/z, and the temperature of the auxiliary heating transmission line (ODP) is 240 ℃. The cleavage mass spectrum of glycoside sample # 1 is shown in FIG. 3. As can be seen from fig. 3, glycoside sample No. 1 was pyrolyzed under the temperature programmed condition set at the injection port, and a plurality of small-molecule aroma components were produced.
The retention time, the material components and the content of the small molecules separated by the chromatographic column are determined by mass spectrometry, and the odor information of the aroma components, including odor characteristics and odor intensity, is determined by performing olfactory discrimination through an olfactory discrimination mouth. Specific analysis data are shown in table 1, and as can be seen from table 1, the main substance produced in glycoside sample No. 1 is dihydromyrcenol, which has a taste equal to the flavor of citrus fruits and a highest content, and is the most important contribution component in the whole flavor.
TABLE 1
Retention time Name of Compound Odor characteristics Strength of smell Peak area ratio Qualitative mode
5.146 Methylglyoxal Pungent smell 1 2％ MS，Odor
6.405 Glycolaldehyde —— 0 1％ MS
14.950 Methylcycloheptene Chemical smell 1 28％ MS，Odor
16.309 Citronellal alkene Fragrance 1 19％ MS，Odor
20.553 Dihydromyrcenol Citrus fruit incense 3 43％ MS，Odor
26.540 Allose —— 0 8 MS
Example 2
1. Thermogravimetric analysis
5mg of acetal sample 1 of unknown composition was weighed into an aluminum crucible having a volume of 100. mu.l and analyzed by a thermogravimetric analyzer. The flow rate is set to be 20.0mL/min, the initial temperature of the thermal weight loss instrument is 50 ℃, then the temperature is increased to 500 ℃ at 20 ℃/min, and the test is carried out under the nitrogen atmosphere. The results of the thermogravimetric tests of acetal sample 1 are shown in figure 4. As can be seen from FIG. 4, the pyrolysis temperature range of acetal sample 1 was 189 to 222 ℃ where the maximum weight loss rate was reached at 219 ℃.
2. Sample pretreatment
Weighing 5mg acetal sample 1, adding 10mL ethanol, dissolving with ultrasound for 2min, taking 2mL sample, placing in a chromatographic analysis bottle, and performing sample loading determination by gas chromatography-mass spectrometry/olfactory discrimination method (GC-MS/O), wherein the specific analysis device is shown in figure 1. Wherein, because acetal is in a liquid state at normal temperature, ethanol with low toxicity is selected.
3. Measurement of Whole fragrance
And inputting the acetal sample 1 into the gas chromatography part through a liner tube through a sample inlet, and sampling by adopting an Agilent multimode MMI sample inlet. The temperature rise program of the sample inlet is that the temperature is kept for 0.2min at 60 ℃, the temperature is raised to 280 ℃ at 900 ℃/min, the temperature is kept for 10min, and the mode of no shunt is adopted.
And closing the first control valve, opening the second control valve, and pyrolyzing the acetal sample 1 by using a first chromatographic column in the gas chromatography to obtain the integral aroma, wherein the first chromatographic column is a deactivated immobile phase capillary chromatographic column. The column oven was operated with 210 ℃ being maintained. And performing sniffing through a sniffing mouth to determine the smell information of the whole aroma. The overall aroma of acetal sample 1 was smelled as: has milk fragrance and cocoa fragrance.
4. Measurement of aroma component
And inputting the acetal sample 1 into the gas chromatography part through a liner tube through a sample inlet, and sampling by adopting an Agilent multimode MMI sample inlet. The temperature rise program of the sample inlet is that the temperature is kept for 0.2min at 60 ℃, the temperature is raised to 280 ℃ at 900 ℃/min, the temperature is kept for 10min, and the mode of no shunt is adopted.
Opening the first control valve, closing the second control valve, flowing acetal sample 1 through the first chromatographic column in the gas chromatograph, and pyrolyzing the acetal sample 1 through the second chromatographic column in the gas chromatograph to obtain a plurality of aroma components, wherein the second chromatographic column is a DB-5ms nonpolar chromatographic column. The temperature raising program of the column incubator is that the temperature is maintained at 60 ℃ for 1min, the temperature is raised to 180 ℃ at 4 ℃/min, and then the temperature is raised to 230 ℃ at 10 ℃/min and maintained for 10 min.
And determining the aroma components and the release content thereof by adopting a mass spectrum, wherein the determination conditions of the mass spectrum are as follows: the ionization source energy is 70 eV; the ion source temperature is 230 ℃; the transmission line temperature is 250 ℃; the scanning mode is scan; the scanning range is 35-300 m/z, and the temperature of the auxiliary heating transmission line (ODP) is 240 ℃. The cleavage mass spectrum of acetal sample 1 is shown in FIG. 5. As can be seen from fig. 5, the acetal sample 1 can be pyrolyzed under the temperature programmed condition set at the injection port to generate a plurality of small molecular aroma components.
The retention time, the material components and the content of the small molecules separated by the chromatographic column are determined by mass spectrometry, and the odor information of the aroma components, including odor characteristics and odor intensity, is determined by performing olfactory discrimination through an olfactory discrimination mouth. Specific analytical data are shown in table 2, and it can be seen from table 2 that most of acetal sample 1 volatilizes during the pyrolysis process, only a small part of acetal sample pyrolyzes to produce ethyl vanillin with milk fragrance, and the ethyl vanillin has a moderate content and is the main component of the odor contribution in the whole fragrance.
TABLE 2
Figure BDA0003054811950000091
In conclusion, the method for analyzing the pyrolysis aroma components of the potentially aromatic raw materials for the cigarettes, provided by the invention, not only can qualitatively crack the products, but also can clarify the aroma characteristics and the aroma intensity, and has the advantages of simplicity, accuracy, rapidness, reliability, high efficiency, high sensitivity and good stability. Therefore, the invention effectively overcomes various defects in the prior art and has high industrial utilization value.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.

Claims (12)

1. A method for analyzing pyrolytic aroma components of aroma raw materials comprises adding an aroma raw material sample into an organic solvent for dissolving, and measuring by adopting a temperature rise program sample injection of a sample injection port and a gas chromatography-mass spectrometry/smell identification method; the method comprises the steps of obtaining integral aroma by pyrolyzing an aroma raw material sample through a first chromatographic column in gas chromatography, and determining the smell information of the integral aroma by adopting smell discrimination; and (3) pyrolyzing a fragrance raw material sample through a second chromatographic column in the gas chromatography to obtain a plurality of fragrance components, determining the fragrance components and the release content thereof by adopting a mass spectrum, and determining the odor information of the fragrance components by adopting olfactory discrimination.
2. The method for analyzing the pyrolytic aroma components of the incense raw materials according to claim 1, wherein the samples of the incense raw materials are analyzed by a thermogravimetric method before being added with an organic solvent for dissolution, and the pyrolysis temperature range and the temperature reaching the maximum weight loss speed in the pyrolysis temperature range are determined.
3. The method for analyzing the pyrolytic aroma components of the raw materials of the incense according to claim 2, wherein the conditions of the thermal weight loss method comprise any one or more of the following conditions:
A1) the analysis atmosphere is a nitrogen atmosphere;
A2) the flow rate is 10-30 mL/min;
A3) the temperature raising procedure is as follows: the initial temperature is 30-80 ℃, and the temperature is increased to 300-500 ℃ at 10-50 ℃.
4. The method for analyzing pyrolytic aroma components of raw materials for cigarettes according to claim 1, wherein the raw materials for aroma are latent aroma raw materials for cigarettes; the organic solvent is selected from one or more of methanol, ethanol, isopropanol, ethyl acetate, diethyl ether, tert-butyl methyl ether and n-hexane; the ratio of the mass of the fragrance raw material sample to the volume of the organic solvent is 5: 5-15 mg/mL.
5. The method for analyzing the pyrolytic aroma components of the aroma raw materials according to claim 1, wherein the temperature rise program of the sample inlet is 40-80 ℃ for 0.1-5 min, and the temperature is raised to the temperature which reaches the maximum weight loss rate in the pyrolysis temperature range of the aroma raw material sample at 300-900 ℃/min and is + 10-100 ℃ for 5-30 min.
6. The method for analyzing pyrolytic aroma components of raw materials according to claim 1, wherein the measurement conditions of the gas chromatography comprise any one or more of the following:
B1) the flow rate is 0.8-2 mL/min;
B2) the first chromatographic column is a deactivated non-stationary phase capillary chromatographic column;
B3) the second chromatographic column is one selected from DB-5ms, DB-wax, DB-17, DB-624 or Supelco-VOCOL capillary chromatographic columns;
B4) when the overall aroma is measured, the operation temperature of the column temperature box is 205-215 ℃;
B5) when the aroma components are measured, the temperature rise program of the column incubator is to keep the temperature at 60 ℃ for 1min, raise the temperature to 180 ℃ at 4 ℃/min, and then raise the temperature to 230 ℃ at 10 ℃/min and keep the temperature for 10 min.
7. The method for analyzing pyrolytic aroma components of raw materials of claim 1, wherein the mass spectrometry is performed under the following conditions: the ionization source energy is 70 eV; the ion source temperature is 230 ℃; the transmission line temperature is 250 ℃; the scanning mode is scan; the scanning range is 35-300 m/z, and the temperature of the auxiliary heating transmission line is 240 ℃.
8. The device for analyzing the pyrolysis aroma components of the aroma raw materials is characterized by comprising a gas chromatography part and a mass spectrum part (7), wherein the gas chromatography part comprises a column temperature box (11), a first chromatographic column (4) and a second chromatographic column (5) are arranged in the column temperature box (11), and a sample inlet (2) and a smell identification port (6) are arranged on the column temperature box (11); the sample introduction end of the first chromatographic column (4) is communicated with the sample introduction port (2), and the sample outlet end of the first chromatographic column (4) is respectively communicated with the sample introduction end of the second chromatographic column (5) and the sniffing port (6); the sample outlet end of the second chromatographic column (5) is respectively communicated with the sniffing port (6) and the mass spectrum part (7).
9. The analysis device for the pyrolytic aroma components of the raw materials according to claim 8, wherein a liner tube (1) is arranged in the sample inlet (2), and the liner tube (1) is communicated with the sample inlet end of the first chromatographic column (4).
10. The analysis device for the pyrolytic aroma components of raw materials according to claim 8, wherein the sample outlet end of the first chromatographic column (4) is provided with a first three-way connector (10), and the sample outlet end of the second chromatographic column (5) is provided with a second three-way connector (8); a first interface (101) of the first three-way connector is communicated with a sample outlet end of the first chromatographic column (4), a second interface (102) of the first three-way connector is communicated with a sample inlet end of the second chromatographic column (5), and a third interface (103) of the first three-way connector is communicated with the sniffing port (6) through a pipeline; the first interface (81) of the second three-way connector is communicated with the sample outlet end of the second chromatographic column (5), the second interface (82) of the second three-way connector is communicated with the sniffing port (6) through a pipeline, and the third interface (83) of the second three-way connector is communicated with the mass spectrum part (7) through a pipeline.
11. The analyzing device for the pyrolytic aroma components of the raw materials according to claim 10, wherein a first control valve (3) is arranged between the first three-way connector (10) and the sample inlet end of the second chromatographic column (5), and a second control valve (9) is arranged on a pipeline between the first three-way connector (10) and the smell distinguishing port (6).
12. Use of an apparatus for analysis of a pyrolysis aroma composition of a fragrance raw material according to any one of claims 8-11 in the analysis of a pyrolysis aroma composition of a fragrance raw material.
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