CN113777201A - Method for analyzing aroma components in tobacco - Google Patents
Method for analyzing aroma components in tobacco Download PDFInfo
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- CN113777201A CN113777201A CN202111068542.9A CN202111068542A CN113777201A CN 113777201 A CN113777201 A CN 113777201A CN 202111068542 A CN202111068542 A CN 202111068542A CN 113777201 A CN113777201 A CN 113777201A
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/08—Preparation using an enricher
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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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
Abstract
The invention provides a method for analyzing aroma components in tobacco, which comprises the following steps: continuously heating a tobacco sample to be detected, simultaneously adopting a closed loop gas stripping method to enrich aroma components in the tobacco, then thermally desorbing, and adopting a gas chromatography-mass spectrometer for qualitative and quantitative analysis. The method in the application can effectively avoid the problem that the adsorption effect of the adsorbent is poor in the enrichment process, and has a good adsorption effect on the tobacco sample to be tested with higher moisture content, so that the test of the aroma components in the tobacco is more accurate and effective.
Description
Technical Field
The invention relates to the field of tobacco, in particular to an analysis method of aroma components in tobacco.
Background
The analysis of the aroma components in the tobacco has important significance for analyzing the style and the characteristics of the tobacco leaves and researching the quality and the style of the cigarettes. Analytical methods conventionally employed in the prior art include solvent extraction, solid phase extraction, and headspace-solid phase microextraction. The sensitivity of the method is still insufficient aiming at trace aroma components in tobacco leaves and smoke.
In a Closed-Loop air-lift method (CLSA), a certain volume of gas circulates between a sample bottle and an enrichment tube through an air pump and a pipeline system, and volatile and semi-volatile components to be detected in a sample are continuously extracted and adsorbed in the enrichment tube by airflow. At present, the technology is applied to analysis and preparation of volatile and semi-volatile components in natural products and tobacco products. For example, the invention patent with the domestic application number of 2016101345446 discloses an analysis method for volatile and semi-volatile components in tobacco based on CLSA, and the application number of 2020102391931 also discloses a preparation method and a device for volatile aroma components in natural products based on CLSA.
Disclosure of Invention
In view of the above-mentioned drawbacks of the prior art, it is an object of the present invention to provide a solution to the problems of the prior art.
To achieve the above objects and other related objects, the present invention is achieved by the following technical solutions.
The invention provides a method for analyzing aroma components in tobacco, which comprises the following steps:
continuously heating a tobacco sample to be detected, simultaneously adopting a closed loop gas stripping method to enrich aroma components in the tobacco, then thermally desorbing, and adopting a gas chromatography-mass spectrometer for qualitative and quantitative analysis.
Preferably, the tobacco sample to be tested is equilibrated prior to heating. More preferably, the balancing treatment is to put the tobacco sample to be measured into a sample bottle for heating balancing, wherein the heating balancing temperature is 40-90 ℃, and the heating balancing time is 10-30 minutes.
Preferably, the temperature for heating the tobacco sample to be detected is 40-90 ℃.
Preferably, the closed loop gas stripping method is to circulate the gas generated by heating the tobacco sample to be tested in a closed loop so as to enrich the aroma components in the adsorbent; along the circulation direction of the gas, the gas is sequentially subjected to heating, condensation, heating, adsorbent adsorption and heating.
Preferably, the tobacco sample to be detected comprises tobacco leaves, cut tobacco or a cambridge filter sheet for trapping cigarette mainstream smoke.
Preferably, the tobacco sample to be tested is equilibrated and heated in a flask.
More preferably, the temperature of the heating equilibrium is 65-70 ℃.
More preferably, the time for the heating equilibration is 15 min.
More preferably, the temperature for heating the tobacco sample to be detected is 65-70 ℃.
Preferably, the flow rate of gas in the closed loop is 500-1000 mL/min.
More preferably, the gas flow rate in the closed loop is 800 mL/min.
Preferably, the circulation flow time is 5-24 h.
More preferably, the circulation flow time is 18 h.
Preferably, the adsorbent is one or more selected from Tenax, activated carbon, and molecular sieves. More preferably, the adsorbent is Tenax, which is hydrophobic relative to the other adsorbents.
Preferably, the amount of the adsorbent used is 20-200 mg.
More preferably, the adsorbent is Tenax, used in an amount of 200 mg.
More preferably, the condensation is carried out at the neck of the flask. More preferably, the condensation provides a temperature of 0-5 ℃.
More preferably, the condensation provides a temperature of 4 ℃.
Preferably, in the closed path, the heating provides a temperature of 40-90 ℃.
More preferably, in the closed path, the heating provides a temperature of 70 ℃.
Preferably, the thermal desorption conditions are: the first-stage desorption temperature is 250 ℃ and 280 ℃, and the desorption time is 5-10 min; the secondary desorption temperature is 260-290 ℃, and the desorption time is 3-8 min; the split ratio is 9:1-99: 1.
More preferably, the thermal desorption conditions are: the first-stage desorption temperature is 270 ℃, and the desorption time is 10 min; the secondary desorption temperature is 280 ℃, and the desorption time is 8 min; the split ratio was 99: 1.
Preferably, the gas chromatography adopts DB-WAX capillary column, the carrier gas adopts high-purity helium, and the flow rate of the carrier gas is 1-5 ml/min.
More preferably, the gas chromatography is performed by using a DB-WAX capillary column, the carrier gas is high-purity helium, and the flow rate of the carrier gas is 2 ml/min. The carrier gas in the gas chromatography adopts high-purity helium, and the purity of the helium is more than or equal to 99.999 percent.
Preferably, the initial temperature in the gas chromatography heating procedure is 30-50 ℃ and is kept for 2-5 minutes, the heating speed is 2-5 ℃/min, and the temperature is increased to 220-240 ℃ and is kept for 10-20 minutes.
More preferably, the initial temperature in the gas chromatography heating program is 40 ℃ and kept for 5 minutes, the heating speed is 4 ℃/min, and the temperature is raised to 23 ℃ and kept for 10 minutes.
Preferably, the mass spectrometry conditions are: the temperature of the transmission line is 230-250 ℃, the temperature of the ion source is 220-240 ℃, and the temperature of the four-level rod is 140-160 ℃.
More preferably, the mass spectrometry conditions are: transmission line temperature: 230 ℃; ion source temperature: 230 ℃; quadrupole temperature: 150 ℃; an ionization mode: an EI source; ionization energy: 70 eV; the scanning mode is as follows: full scan and selective ion monitoring.
Preferably, the closed loop gas stripping process is carried out in a closed loop gas stripping device comprising a flask, a heating assembly, a condensing assembly, and a closed loop channel; the air inlet end of the closed-loop channel is communicated with the air outlet of the flask, the air outlet end of the closed-loop channel is communicated with the flask, and the closed-loop channel is sequentially provided with a heating module, an adsorbent and an air pump along the air flowing direction; the heating component is used for supplying heat to the flask so as to heat the tobacco sample to be measured and the gas in the flask; the condensation assembly acts on the neck of the flask for cooling the gas passing through the neck.
Preferably, the air pump is an electrically diaphragm air pump.
Preferably, the condensation assembly comprises a condenser and a spiral condensation pipe, and the spiral condensation pipe is sleeved on the bottleneck of the flask.
More preferably, the air outlet end of the flask is provided at the top of the flask.
More preferably, the air outlet end of the closed-loop channel is arranged at the bottom of the flask.
Most preferably, the distance from the air outlet end of the closed-loop channel to the bottom surface of the flask is 0.5-1 cm. Preferably, the long-necked sample bottle is a glass bottle which is conventionally used. The volume of the long-neck sample bottle is 1-10L.
Preferably, condensed water is arranged in the spiral condenser pipe. The spiral condensing tube condenses circulating water through cold condensed water.
Preferably, the spiral condenser tube is made of a metal copper tube, and the spiral condenser tube can be sleeved outside the flask in size.
Preferably, the heating assembly is a water bath kettle which is a conventionally used temperature-controlled water bath heating kettle.
As described above, the method for analyzing aroma components in tobacco provided by the present invention has the following advantages:
1) the method for analyzing the aroma components in the tobacco has a good enriching effect on the aroma components in the tobacco, is high in concentration multiple and strong in adsorption efficiency, and can be used for analyzing trace and trace components.
2) According to the method for analyzing the aroma components in the tobacco, provided by the invention, the closed-loop channel before adsorption is sequentially designed for condensation, dehydration and heating, so that the defect that the adsorption performance is influenced by the condensation of water vapor on an adsorbent due to long-time purging is avoided, and the method also has a good enrichment effect on the tobacco sample to be tested with higher moisture content, so that more comprehensive and abundant aroma components are obtained.
3) The method for analyzing the aroma components in the tobacco provided by the invention is proved by methodology to have good repeatability and high analysis sensitivity, and can meet the analysis requirements of the aroma components in the tobacco.
4) The method for analyzing the aroma components in the tobacco is simple to operate, and related equipment is convenient to assemble and low in cost.
The method for analyzing the aroma components in the tobacco disclosed by the invention overcomes various defects in the prior art and is creative.
Drawings
FIG. 1 is a schematic diagram of a closed loop stripper apparatus provided in an embodiment of the present disclosure.
FIG. 2 shows the results obtained from the analysis of the method of example 1 using the combined technique of thermal desorption and gas chromatography-mass spectrometry.
Wherein the reference numerals in fig. 1 are as follows:
1 air pump
2 air inlet pipe
21 first air intake section
22 second air intake section
3 air outlet pipe
31 first air outlet section
32 second air outlet section
4 heating module
5 adsorption liner tube with adsorbent therein
6 spiral condenser pipe
7 condenser
8 long neck bottle
9 water bath heating device
Detailed Description
The following description of the embodiments of the present invention is provided for illustrative purposes, and other advantages and effects of the present invention will become apparent to those skilled in the art from the present disclosure.
Before the present embodiments are further described, it is to be understood that the scope of the invention is not limited to the particular embodiments described below; it is also to be understood that the terminology used in the examples is for the purpose of describing particular embodiments only, and is not intended to limit the scope of the present invention. Test methods in which specific conditions are not specified in the following examples are generally carried out under conventional conditions or under conditions recommended by the respective manufacturers.
When numerical ranges are given in the examples, it is understood that both endpoints of each of the numerical ranges and any value therebetween can be selected unless the invention otherwise indicated. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In addition to the specific methods, devices, and materials used in the examples, any methods, devices, and materials similar or equivalent to those described in the examples may be used in the practice of the invention in addition to the specific methods, devices, and materials used in the examples, in keeping with the knowledge of one skilled in the art and with the description of the invention.
In practical work, the applicant finds that during the process of enriching the target component in the gas, the adsorbent fails or is incompletely adsorbed due to the existence of moisture in the gas, so that the accuracy and the effectiveness of analyzing and testing the target component in the tobacco are influenced.
Accordingly, the applicant of the present application has found that based on the above technical problems, a novel method for analyzing aroma components in tobacco is provided, which comprises the following steps: continuously heating a tobacco sample to be detected, simultaneously adopting a closed loop gas stripping method to enrich aroma components in the tobacco, then thermally desorbing, and adopting a gas chromatography-mass spectrometer for qualitative and quantitative analysis.
In a preferred embodiment, the tobacco sample to be tested is equilibrated prior to heating. In a more preferred embodiment, the balancing treatment is to fill the tobacco sample to be tested into a sample bottle for heating balancing, wherein the heating balancing temperature is 40-90 ℃, and the heating balancing time is 10-30 minutes.
In a preferred embodiment, the temperature for heating the tobacco sample to be tested is 40-90 ℃.
In a preferred embodiment, the closed loop air stripping method is that gas generated by heating a tobacco sample to be tested circulates in a closed loop to enrich the aroma components in the adsorbent; along the circulation direction of the gas, the gas is sequentially subjected to heating, condensation, heating, adsorbent adsorption and heating.
In a preferred embodiment, the tobacco sample to be tested comprises tobacco leaves, cut tobacco or cambridge filter sheets trapping cigarette mainstream smoke.
In a preferred embodiment, the tobacco sample to be tested is equilibrated and heated in a flask.
In a more preferred embodiment, the temperature of the heating equilibrium is 65 to 70 ℃.
In a more preferred embodiment, the time for the heating to equilibrate is 15 min.
In a more preferred embodiment, the tobacco sample to be tested is heated to a temperature of 65 to 70 ℃.
In a preferred embodiment, the gas flow rate in the closed loop is 500 to 1000 mL/min.
In a more preferred embodiment, the gas flow rate in the closed loop is 800 mL/min.
In a preferred embodiment, the circulation flow time is from 5 to 24 h.
In a more preferred embodiment, the circulation flow time is 18 h.
In a preferred embodiment, the adsorbent is one or more selected from Tenax, activated carbon, and molecular sieves. In a more preferred embodiment, the adsorbent is Tenax, which is hydrophobic relative to the other adsorbents.
In a preferred embodiment, the adsorbent is used in an amount of 20-200 mg.
In a more preferred embodiment, the adsorbent is Tenax, used in an amount of 200 mg.
In a more preferred embodiment, the condensation is carried out at the neck of the flask. In a more preferred embodiment, the condensation provides a temperature of 0-5 ℃.
In a more preferred embodiment, the condensation provides a temperature of 4 ℃.
In a preferred embodiment, the heating provides a temperature of 40-90 ℃ in the closed path.
In a more preferred embodiment, in the closed path, the heating provides a temperature of 70 ℃.
In a preferred embodiment, the thermal desorption conditions are: the first-stage desorption temperature is 250 ℃ and 280 ℃, and the desorption time is 5-10 min; the secondary desorption temperature is 260-290 ℃, and the desorption time is 3-8 min; the split ratio is 9:1-99: 1.
In a more preferred embodiment, the thermal desorption conditions are: the first-stage desorption temperature is 270 ℃, and the desorption time is 10 min; the secondary desorption temperature is 280 ℃, and the desorption time is 8 min; the split ratio was 99: 1.
In a preferred embodiment, the gas chromatography is performed using a DB-WAX capillary column, high purity helium is used as the carrier gas, and the carrier gas flow rate is 1-5 ml/min.
In a more preferred embodiment, the gas chromatography is performed using a DB-WAX capillary column, high purity helium is used as the carrier gas, and the carrier gas flow rate is 2 ml/min. The carrier gas in the gas chromatography adopts high-purity helium, and the purity of the helium is more than or equal to 99.999 percent.
In a preferred embodiment, the initial temperature in the gas chromatography heating procedure is 30-50 ℃ and is kept for 2-5 minutes, the heating speed is 2-5 ℃/min, and the temperature is raised to 220-240 ℃ and is kept for 10-20 minutes.
In a more preferred embodiment, the initial temperature in the gas chromatography temperature-increasing program is 40 ℃ and kept for 5 minutes, the temperature-increasing speed is 4 ℃/min, and the temperature is increased to 23 ℃ and kept for 10 minutes.
In a preferred embodiment, the mass spectrometry conditions are: the temperature of the transmission line is 230-250 ℃, the temperature of the ion source is 220-240 ℃, and the temperature of the four-level rod is 140-160 ℃.
In a more preferred embodiment, the mass spectrometry conditions are: transmission line temperature: 230 ℃; ion source temperature: 230 ℃; quadrupole temperature: 150 ℃; an ionization mode: an EI source; ionization energy: 70 eV; the scanning mode is as follows: full scan and selective ion monitoring.
In a preferred embodiment, the closed loop stripping process is carried out in a closed loop stripping apparatus comprising a flask, a heating assembly, a condensing assembly, and a closed loop passage; the air inlet end of the closed-loop channel is communicated with the air outlet of the flask, the air outlet end of the closed-loop channel is communicated with the flask, and the closed-loop channel is sequentially provided with a heating module, an adsorbent and an air pump along the air flowing direction; the heating component is used for supplying heat to the flask so as to heat the tobacco sample to be measured and the gas in the flask; the condensation assembly acts on the neck of the flask for cooling the gas passing through the neck.
According to the closed loop air lifting device, the closed loop is composed of a long-neck bottle and a closed loop channel, wherein the two ends of the head and the tail of the closed loop channel are communicated with the long-neck bottle. In the closed loop, the tobacco sample to be measured in the flask generates gas after being heated by the heating component, the gas is condensed at the neck of the flask by the condensing component, and then is heated by the heating module in the closed channel, adsorbed by the adsorbent, condensed by the condensing component, and enters the flask to be heated again. Therefore, the gas continuously and circularly flows in the closed loop gas stripping device, so that the aroma components in the gas are continuously adsorbed by the adsorbent, and the completeness and sufficiency of adsorption are ensured.
In the technical scheme, the neck of the flask is provided with the condensing assembly for condensing water vapor in the gas, so that the water vapor is liquefied as much as possible and stays in the flask without entering the adsorbent along with the gas circulating flow; and a heating module is arranged after condensation, and the heating module is positioned at the upstream of the adsorbent and is used for keeping uncondensed water vapor at a certain temperature and not condensing in the adsorbent or the adsorption liner pipe.
The aforesaid in this application closed loop air stripping device can be among the effectual solution prior art at the target composition enrichment in-process that awaits measuring, because cycle time is longer, the problem of adsorbent adsorption effect variation, to the higher tobacco sample that awaits measuring of moisture content very much, adopt above-mentioned device it also can reach good adsorption effect.
In a preferred embodiment, the air pump is an electrically diaphragm air pump.
In a preferred embodiment, the condensing assembly comprises a condenser and a spiral condenser tube, and the spiral condenser tube is sleeved on the bottleneck of the flask.
In a more preferred embodiment, the gas outlet end of the flask is provided at the top of the flask.
In a more preferred embodiment, the gas outlet end of the closed-loop channel is arranged at the bottom of the flask.
In a more preferred embodiment, the distance from the gas outlet end of the closed-loop channel to the bottom surface of the flask is 0.5-1 cm. In a preferred embodiment, the long-necked sample vial is a conventionally used glass vial. The volume of the long-neck sample bottle is 1-10L.
In a more preferred embodiment, the neck of the flask has a length of 10 to 15cm and a diameter of 35 to 45 mm. The length and the diameter are matched, so that the circulating circulation of the gas can be ensured, and the higher condensation efficiency of the water vapor in the gas can be ensured.
In a preferred embodiment, the spiral condenser pipe is provided with condensed water therein. The spiral condensing tube condenses circulating water through cold condensed water.
In a preferred embodiment, the spiral condenser tube is made of a metal copper tube and is sized to fit outside the flask.
In a preferred embodiment, the heating assembly is a water bath, which is a conventionally used temperature-controlled water bath heating pan.
In a preferred embodiment, the heating module comprises a temperature-controlled heating element sleeved outside the closed-loop channel.
The technical solution and technical effects of the present application are further explained and explained by the following detailed description and the implementation effect data.
The closed loop stripper apparatus employed in the following examples of the present application is illustrated in FIG. 1. The closed loop gas stripping device comprises a flask 8, a heating component, a condensing component and a closed loop channel; the air inlet end of the closed-loop channel is communicated with the air outlet of the flask 8, the air outlet end of the closed-loop channel is communicated with the flask 8, and the closed-loop channel is sequentially provided with a heating module 4, an adsorbent and an air pump 1 along the air flowing direction; the heating component is used for supplying heat to the flask 8 so as to heat the tobacco sample to be measured in the flask 8; the condensation assembly acts on the neck of the flask 8 for cooling the gas passing through the neck.
In fig. 1, the heating assembly is a water bath heating device 9, the condensing assembly comprises a condenser 7 and a spiral condensing pipe 6, and the neck of the flask 8 is sleeved with the spiral condensing pipe 6.
As shown in fig. 1, the closed-loop channel includes an outlet pipe 3, an adsorption liner pipe 5 with an adsorbent disposed therein, and an inlet pipe 2 along a gas flowing direction, wherein the outlet pipe 3 includes a first outlet section 31 and a second outlet section 32, and the adsorption liner pipe 5 with the adsorbent disposed therein is disposed between the first outlet section 31 and the second outlet section 32. The intake pipe 2 includes a first intake section 21 and a second intake section 22. The second air inlet section 22 is arranged in the flask 8. An air pump 1 is arranged between the air inlet pipe 2 and the air outlet pipe 3. As shown in fig. 1, the heating module 4 is provided upstream of the adsorption liner 5.
When the closed loop gas stripping method is carried out by adopting the specific closed loop gas stripping device shown in fig. 1, the water bath heating device 9 heats the tobacco component to be detected in the flask 8, the generated gas is condensed by the spiral condenser pipe 6 when reaching the neck of the flask 8, the water vapor is liquefied and kept in the flask, then the gas enters the second gas outlet section 32, the gas is heated by the heating module 4 to avoid condensation when passing through the adsorbent, and then the gas enters the bottom in the flask through the adsorption liner pipe 5 in which the adsorbent is arranged, the second gas outlet section 32, the first gas inlet section 21 and the second gas inlet section 22, and then the gas continues to enter the next cycle.
Example 1
The method for analyzing the aroma components in the tobacco comprises the following steps:
1) smoking the cigarettes by using a smoking machine, trapping mainstream smoke by using a Cambridge filter disc, putting the Cambridge filter disc into a flask, and putting the flask into a temperature-controlled water bath heating pot to heat and balance for 15 minutes at 70 ℃;
2) after balancing, continuously heating the sample bottle through a temperature-controlled water bath heating pot at the temperature of 70 ℃, preparing air by using an electric diaphragm air pump, wherein the outlet flow rate of the electric diaphragm air pump is 800mL/min, and purging the sample in the sample bottle for 18 hours;
3) the resulting air sweep was enriched using an adsorption liner (0.25 inch diameter and 3.5 inches in length) packed with 200mg of Tenax adsorbent. The adsorption liner tube is connected with the long-neck bottle, the spiral condenser tube, the heating module and the circulating stripping pump to form a closed loop, wherein the spiral condenser tube is coiled on the neck of the long-neck sample bottle, and the temperature is 4 ℃; the heating module is arranged at the front end of the adsorption liner tube, and the temperature is 70 ℃.
4) After the enrichment is completed, the adsorption liner tube is taken down and analyzed by adopting a thermal desorption-gas chromatography-mass spectrometry combined technology, and the result is shown in fig. 2.
Wherein the detection conditions of the thermal desorption-gas chromatography-mass spectrometer (GC-MS) are as follows:
the thermal desorption conditions were: first-order desorption temperature: desorbing at 270 deg.C for 10 min; secondary desorption temperature: at 280 ℃, the desorption time is 8 min; the valve temperature is 250 ℃; transmission line temperature: 250 ℃; the split ratio was 99: 1.
The gas chromatography conditions were: a chromatographic column: DB-WAX capillary column (60m × 0.32mm × 0.25 μm); carrier gas: helium (more than or equal to 99.999%); constant flow mode flow rate: 2.0 mL/min; temperature rising procedure: the temperature was maintained at 40 ℃ for 5min and then increased to 230 ℃ at a rate of 4 ℃/min for 10 min.
The mass spectrum conditions are as follows: transmission line temperature: 230 ℃; electron energy: 70 eV; EI source temperature: 230 ℃; temperature of the quadrupole rods: 150 ℃; the scanning mode is as follows: full Scan (Scan) and Selective Ion Monitoring (SIM); mass scan range: 33 to 300 amu.
And quantitatively analyzing the detection result by adopting a peak area normalization method, and qualitatively analyzing the detection result by adopting a map database retrieval, wherein the map database is an NIST database, and the matching degree is more than or equal to 90 according to component judgment selection.
The analysis method in the application adopts the closed loop gas stripping device, can effectively enrich the chemical components of the aroma, and has simple operation and good repeatability. The method is used for analyzing the aroma components in the main stream smoke of the cigarette, and can detect 254 different components, wherein 49 nitrogen heterocycles, 28 micromolecule aldones, 27 phenols, 26 oxa heterocycles, 23 aromatics, 19 cyclopentenones (alcohol ketones), 13 acids, 12 olefins, 8 alcohols and 8 neutral aroma components. The partially detected substances are shown in table 1. The specific detection effect is shown in fig. 2, and it can be seen from fig. 2 that: aiming at the main stream smoke of the cigarette, the established method has the advantages of lower chromatographic baseline, better peak type, high sensitivity and rich detected peaks, and substances such as limonene, 2, 3-dimethylcyclopentenone, 5-methylfurfural, 2-isohexyl-6-methyl-1-heptene, nicotine, neophytadiene, glyceryl triacetate, 4-vinyl guaiacol, 2, 6-dimethoxyphenol, isonicotinine, 5-hydroxymethyl furfural, myristic acid, palmitic acid and the like have higher response.
TABLE 1
Example 2
The method of the invention is examined repeatedly. The results show that the RSD of typical aroma components in mainstream smoke are less than 10% each, as shown in table 2. Compared with the smoke data obtained by the conventional solvent extraction method (using 50mL of organic reagent to extract Cambridge filter discs and injecting sample at 1 uL), the response of the typical aroma components obtained by the method is remarkably increased and is about 500 times of that of the conventional solvent extraction method. The method provided by the invention has the advantages that the extracted components are comprehensive and typical, the relative content of each component is high, and the repeatability is good.
TABLE 2
Example 3
100g of tobacco shreds are selected and put into a long-neck sample bottle, and the long-neck sample bottle is heated and balanced for 15 minutes in a water bath kettle at the temperature of 40 ℃. And then, continuously heating the balanced tobacco shreds at 40 ℃, inputting air into the long-neck sample bottle through an air inlet pipe by a circulating stripping pump for continuous sweeping, wherein the air sweeping flow rate is 1000ml/min, and the sweeping time is 24 h. And (3) condensing the gas for sweeping the tobacco shreds by a spiral condensing tube at 5 ℃, inputting the gas into the adsorption liner tube through an air outlet pipe for enrichment for 24 hours, and finally taking out the adsorption liner tube enriched with the aroma components, and analyzing by adopting a thermal desorption-gas chromatography-mass spectrometry combined technology. In addition, the adsorption liner tube enriched with aroma components can also be taken out, and is eluted with anhydrous ethanol for 3 times, and the dosage is 2mL each time, so that the required aroma component sample is obtained.
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 (10)
1. A method for analyzing aroma components in tobacco comprises the following steps: continuously heating a tobacco sample to be detected, simultaneously adopting a closed loop gas stripping method to enrich aroma components in the tobacco, then thermally desorbing, and adopting a gas chromatography-mass spectrometer for qualitative and quantitative analysis.
2. The analysis method according to claim 1, wherein the tobacco sample to be tested is subjected to a balancing treatment before heating, the balancing treatment is to fill the tobacco sample to be tested into a sample bottle for heating and balancing, and the heating and balancing temperature is 40-90 ℃; and/or the tobacco sample to be detected comprises tobacco leaves, tobacco shreds or a Cambridge filter disc for trapping cigarette mainstream smoke; and/or heating the tobacco sample to be detected to 40-90 ℃.
3. An assay method according to claim 1 or 2, wherein the tobacco sample to be tested is equilibrated and/or heated in a flask.
4. The analytical method according to claim 1, wherein the closed loop air stripping method is that gas generated by heating a tobacco sample to be tested is circulated in a closed loop to enrich the aroma components in the adsorbent; along the circulation direction of the gas, the gas is sequentially subjected to heating, condensation, heating, adsorbent adsorption and heating.
5. The analytical method of claim 4, wherein the flow rate of the gas in the closed-circuit channel is 500 to 1000 mL/min; and/or the circulation flow time is 5-24 h; and/or the adsorbent is one or more selected from Tenax, activated carbon and molecular sieve; and/or the usage amount of the adsorbent is 20-200 mg; and/or, the condensation provides a temperature of 0-5 ℃; and/or, in the closed path, heating provides a temperature of 40-90 ℃.
6. The analytical method of claim 1, wherein the thermal desorption conditions are: the first-stage desorption temperature is 250 ℃ and 280 ℃, and the desorption time is 5-10 min; the secondary desorption temperature is 260-290 ℃, and the desorption time is 3-8 min; the split ratio is 9:1-99: 1.
7. The analytical method of claim 1, wherein the gas chromatography conditions comprise one or more of:
a DB-WAX capillary column is adopted;
the carrier gas adopts high-purity helium;
the flow rate of the carrier gas is 1-5 ml/min;
in the gas chromatography heating procedure, the initial temperature is 30-50 ℃ and is kept for 2-5 minutes, the heating speed is 2-5 ℃/min, and the temperature is increased to 220-240 ℃ and is kept for 10-20 minutes.
8. The method of claim 1, wherein the mass spectrometry conditions comprise one or more of:
the temperature of the transmission line is 230-250 ℃;
the ion source temperature is 220-240 ℃;
the quadrupole temperature was 140 ℃ and 160 ℃.
9. The analytical method of claim 1, wherein the closed loop stripping is performed in a closed loop stripping apparatus comprising a flask, a heating assembly, a condensing assembly, and a closed loop channel; the air inlet end of the closed-loop channel is communicated with the air outlet of the flask, the air outlet end of the closed-loop channel is communicated with the flask, and the closed-loop channel is sequentially provided with a heating module, an adsorbent and an air pump along the air flowing direction; the heating component is used for supplying heat to the flask so as to heat the tobacco sample to be measured and the gas in the flask; the condensation assembly acts on the neck of the flask for cooling the gas passing through the neck.
10. The analytical method of claim 9, wherein the air pump is an electrically diaphragm air pump; and/or the condensation component comprises a condenser and a spiral condensation pipe, and the spiral condensation pipe is sleeved on the bottleneck of the flask; and/or the air outlet end of the flask is arranged at the top of the flask; and/or the air outlet end of the closed-loop channel is arranged at the bottom of the flask.
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