CN108845067A - A kind of purge and trap method of flavor component in tobacco and tobacco product - Google Patents
A kind of purge and trap method of flavor component in tobacco and tobacco product Download PDFInfo
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- CN108845067A CN108845067A CN201810399851.6A CN201810399851A CN108845067A CN 108845067 A CN108845067 A CN 108845067A CN 201810399851 A CN201810399851 A CN 201810399851A CN 108845067 A CN108845067 A CN 108845067A
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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
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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
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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
- G01N2030/062—Preparation extracting sample from raw material
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Abstract
The present invention discloses a kind of purge and trap method of flavor component in tobacco and tobacco product, and sample extracts through ultrasonic water bath first, obtains extract liquor, purge and trap is then carried out under salting-out condition, the specific steps are：The clipped processing of tobacco sample, high temperature ultrasonic extracts in water, and salt is added in extract liquor, carries out purge and trap, then flavor component is desorbed through Thermal desorption, is detected using Gc/ms Analyser, to realize the qualitative and quantitative analysis of flavor component.Compared with prior art, the present invention does not use organic reagent in the extraction process of flavor component, avoids the loss of part flavor component and the pollution to environment.This method realizes the quick and precisely analysis of multiple fragrance ingredient, have many advantages, such as to detect ingredient is more, high sensitivity, quantify it is accurate, easy to operate quick.
Description
Technical field
The present invention designs the separating and extracting process of flavor component in tobacco, and in particular to fragrant in a kind of tobacco and tobacco product
The purge and trap method of taste ingredient.
Background technique
It is cigarette product flavor that flavor component, which is flavor component an important factor for influencing product quality, in tobacco, in tobacco
Important component.The flavor component component of tobacco aroma feature has hundreds of, these flavor component contents are usually micro
Grade even trace level, therefore the research for quick and precisely analyzing flavor component technology is most important.
Currently, common Studies on Analysis of Flavor Constituents method is solvent extraction, steam distillation, liquid-phase micro-extraction while distilling
The methods of extraction.Solvent extraction needs to use organic reagent, and usually requires in advance tobacco drying or pulverization process, in heat
It air-dries in dry or crushing process, flavor component is also constantly losing；Steam distillation low efficiency and cumbersome；Liquid-phase micro-extraction
It needs to use organic reagent, and needs to be concentrated；The extraction efficiency of Simultaneous distillation-extraction is higher, but there are time-consuming, laborious, You Jirong
The disadvantages of agent usage amount is big.
Chinese patent literature CN201410336052.6 discloses the extracting method and its application of a kind of tobacco flavor ingredient,
A kind of method of ultrasonic disruption assisted extraction tobacco flavor ingredient is provided, but this method still uses organic reagent molten as extracting
Agent.Chinese patent literature CN201510117465.X discloses a kind of volatilization of tobacco, half extracting method for volatilizing flavor component, should
Document uses Puffing and trapping, but this method is only applicable to volatilization and half volatile ingredient, while time-consuming and catches for purge
It needs that organic solvent elution by several times is added after collection.Chinese patent literature 201580010569.9 discloses the extraction side of fragranced ingredient
The manufacturing method of method and the constituent element of preference, by heating cigarette ingredient Jing Guo alkali process, by the gas of release with catching
Collect solvent trapping, but the undulate quantity of pH of this method amount of collected based on trapping solution and the residual quantity of nicotine component determine.
Summary of the invention
Present invention aim to address problem of the existing technology, flavor component is fast in realization tobacco and tobacco product
Fast accurate analysis, the present invention provides a kind of purge and trap methods of flavor component in tobacco and tobacco product, specially ultrasonic
Water-bath extraction-purge and trap-gas chromatography/mass spectrometry method, method use the Liquid sample introduction mode of purge and trap instrument.
To achieve the above object, the technical solution adopted by the present invention is that：
A kind of purge and trap method of flavor component in tobacco and tobacco product, sample is using water as extractant, first through super
Sound water-bath extraction, then carries out purge and trap under salting-out condition；The temperature of the ultrasonic water bath extraction is 72~95 DEG C, the time
For 10~120min.
Ultrasonic water bath extraction and purge and trap are combined by the method for the present invention, can under conditions of not using organic reagent
Achieve the purpose that effectively to extract flavor component in tobacco and tobacco product, the middle organic reagent that relies on is to tobacco compared with the prior art
The method that ingredient extracts, this method had not only avoided the loss of flavor component caused by organic reagent, but also reduced organic examination
Pollution of the agent to environment.
Preferably, the salting-out condition is that the sodium chloride that weight percent is 5~35% is added in extract liquor, and purging is caught
The purging temperature of collection is 40~95 DEG C.Salting out can change the solubility of sample, and component is promoted to be separated from the water out.It is molten
Xie Du higher component, purging efficiency is lower, and for highly-water-soluble component, purging effect could be improved by being only improved purging temperature
Rate.
Preferably, in a kind of tobacco and tobacco product flavor component purge and trap method, include the following steps：
(1) tobacco and tobacco product are handled to the pipe tobacco for being 1mm × 10mm for area；
(2) pipe tobacco is weighed, is mixed with water by constant weight volume ratio, obtains aqueous solution；
(3) ultrasonic water bath extraction is carried out to aqueous solution, obtains extract liquor；
(4) it draws extract liquor to be placed in purging bottle, sodium chloride is added；
(5) sample in purging bottle is purged air through, is bubbled and evaporates flavor component with purge gass by water phase；
(6) it is captured when flavor component passes through collecting trap, then is desorbed and flavor component blowback is entered into gas chromatographic sample introduction mouth,
After chromatography post separation, detected into mass spectrum.
It is found by many experiments, tobacco and tobacco product is handled to the pipe tobacco for being 1mm × 10mm for area, compared cigarette
Grass and tobacco product processing are conventional smashed tobacco powder, can substantially reduce the loss of the flavor component as caused by mechanical force.
It is highly preferred that the pipe tobacco and water volume ratio 1 by weight:16~1:18 mixing.
It is highly preferred that the temperature of the ultrasonic water bath extraction is 80 DEG C, time 60min.
It is highly preferred that the ultrasonic power of the ultrasonic water bath extraction is 1400W.
It is highly preferred that the salting-out condition is that the sodium chloride that weight percent is 25% is added in extract liquor.
It is highly preferred that the purging temperature of the purge and trap is 80 DEG C.
It is highly preferred that desorption temperature is 200 DEG C in step (6)；Desorption time is 2.0min.Higher desorption temperature can
It preferably will volatilize object and be sent into gas chromatographic column, obtain narrow chromatographic peak, generally use 200 DEG C.
The method of the present invention carries out quantitative analysis to flavor component using internal standard method, using methyl phenylacetate as internal standard, with water
Flavor component series standard solution is configured for solvent.
Compared with prior art, the beneficial effects of the invention are as follows：
1, the present invention does not use organic reagent in the extraction process of flavor component, avoids the damage of part flavor component
The pollution become estranged to environment.
2, the present invention is handled without any dehydration and drying before extraction, can effectively reduce the loss of flavor component.
3, the present invention is extracted using ultrasonic water bath, and compared to the extracting process of ultrasonic wave added, this method is without the use of organic examination
Agent but use water as extractant, it is easy to operate and pollution-free.
4, the present invention realizes the quick and precisely extraction of multiple fragrance ingredient, clever with having when gas chromatography/mass spectrometry
Sensitivity is high, detection limit is low, quantitative quick feature accurate, easy to operate.
Detailed description of the invention
Fig. 1 is the total ion chromatogram of flavor component in the embodiment of the present invention 1；
Fig. 2 is the total ion chromatogram of flavor component in the embodiment of the present invention 2.
Specific embodiment
Below in conjunction with the attached drawing in the present invention, technical solution of the present invention is clearly and completely described, it is clear that
Described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on the implementation in the present invention
Example, those of ordinary skill in the art's all other embodiment obtained under the conditions of not making creative work belong to
The scope of protection of the invention.
As a preferred embodiment, in a kind of tobacco and tobacco product flavor component purge and trap method,
Step is：
(1) tobacco and tobacco product are handled to the pipe tobacco for being 1mm × 10mm for area；
(2) pipe tobacco is weighed, is mixed with water by constant weight volume ratio, obtains aqueous solution；
(3) ultrasonic water bath extraction, ultrasonic power 1400W are carried out to aqueous solution, ultrasonic temperature is 75~95 DEG C, when ultrasonic
Between be 10~120min, obtain extract liquor；
(4) it draws extract liquor to be placed in purging bottle, the sodium chloride that weight percent is 5~35% is added；
(5) sample in purging bottle is purged air through, is bubbled and evaporates flavor component with purge gass by water phase, is purged
Temperature is 40~95 DEG C, and purge gass flow is 20ml/min, and purge time is 10~30min；
(6) it is captured when flavor component passes through collecting trap, then is desorbed and flavor component blowback is entered into gas chromatographic sample introduction mouth,
After chromatography post separation, detected into mass spectrum.
Preferably, ultrasonic time described in step (3) is 60min.
Preferably, the sodium chloride that weight percent is 25% is added in step (4).
Preferably, purge time described in step (5) is 25min.
Preferably, desorption temperature is 200 DEG C in step (6)；Desorption time is 2.0min.
The present invention carries out the flavor component extracted from tobacco and tobacco product by gas chromatography/mass spectrometry qualitative
And quantitative detection.
Embodiment 1
The purge and trap method of flavor component, includes the following steps in a kind of tobacco and tobacco product：
(1) tobacco and tobacco product are handled to the pipe tobacco for 1mm × 10mm；
(2) pipe tobacco, by weight volume ratio 1 are weighed:18 mix with water, obtain aqueous solution；
(3) ultrasonic water bath extraction, ultrasonic power 1400W are carried out to aqueous solution, ultrasonic temperature is 80 DEG C, and the time is
60min obtains extract liquor；
(4) it draws 20ml extract liquor to be placed in purging bottle, the sodium chloride that weight percent is 25% is added；
(5) sample in purging bottle is purged air through, is bubbled and evaporates flavor component with purge gass by water phase, is purged
Temperature is 80 DEG C, and purge gass flow is 20ml/min, purge time 25min；
(6) it is captured when flavor component passes through collecting trap, then is desorbed and flavor component blowback is entered into gas chromatographic sample introduction mouth,
After chromatography post separation, detected into mass spectrum.
Desorption temperature is 200 DEG C in step (6)；Desorption time is 2.0min.
Collecting trap is toasted after desorption, baking temperature is 210 DEG C；Baking time is 20min.
Volatile component is detected using Gc/ms Analyser, the testing conditions of gas chromatography/mass spectrometry：
Chromatographic column：Agient DB-17MS capillary column (0.25 μm of the μ m of 30m × 250)；Sample volume：1uL；Injector temperature：250
℃；Split sampling (split ratio 20:1)；Carrier gas：Helium；Flow velocity：20ml/min；Temperature programming：50℃(1min)→3℃/min
→185℃(1min)；Ion source：EI；Ion source temperature：230℃；Transmission line temperature：260℃；Mass Spectrometer Method uses SCAN mould
Formula, 29~350amu of scanning range.
Using methyl phenylacetate as internal standard, configuration flavor component series standard solution, concentration of standard solution are taken water as a solvent
1ng/mL~1ug/mL, using inner mark method ration, coefficient R2It is 0.9986.
Title, quota ion and the content for the flavor component that the present embodiment obtains are shown in Table 1, the total ion current color of flavor component
Spectrogram is shown in Fig. 1.
Embodiment 2
A kind of purge and trap method of flavor component in tobacco and tobacco product, purging temperature described in step (5) are 60
℃.The other the same as in Example 1.
Title, quota ion and the content for the flavor component that the present embodiment obtains are shown in Table 2, the total ion current color of flavor component
Spectrogram is shown in Fig. 2.
Embodiment 3
A kind of purge and trap method of flavor component in tobacco and tobacco product, ultrasonic temperature described in step (3) are 72
℃.The other the same as in Example 1.
The present embodiment detects that can quantify flavor component number is 19, is illustrated in certain temperature range, the ultrasound altogether
When temperature is lower, extraction efficiency is lower.
Embodiment 4
A kind of purge and trap method of flavor component in tobacco and tobacco product, ultrasonic temperature described in step (3) are 95
℃.The other the same as in Example 1.
The present embodiment detects that can quantify flavor component number is 22, when illustrating that ultrasonic temperature is excessively high, may be destroyed altogether
Certain flavor components cause the loss of flavor component.
Embodiment 5
The purge and trap method of flavor component, w/v described in step (2) are in a kind of tobacco and tobacco product
1:16.The other the same as in Example 1.
The present embodiment detects that can quantify flavor component number is 31, illustrates that the bulking value of sample and water compares sample altogether
Ultrasonic water bath effect of extracting has certain influence.
Comparative example 1
A kind of purge and trap method of flavor component in tobacco and tobacco product, ultrasonic temperature described in step (3) are 60
℃.The other the same as in Example 1.
The present embodiment detects that can quantify flavor component number is 9, when illustrating that the ultrasonic temperature is too low altogether, extraction efficiency
It is low.
Comparative example 2
The purge and trap method of flavor component, w/v described in step (2) are in a kind of tobacco and tobacco product
1:20.The other the same as in Example 1.
The present embodiment detects that can quantify flavor component number is 26, illustrates that the bulking value of sample and water compares extraction altogether
The concentration of flavor component has certain influence in liquid, and then influences subsequent testing result.
Comparative example 3
A kind of purge and trap method of flavor component in tobacco and tobacco product, by tobacco and tobacco product in step (1)
Processing is smashed tobacco powder, and specific size is the smashed tobacco powder of 1mm × 1mm.The other the same as in Example 1.
The present embodiment detects that can quantify flavor component number is 27, illustrates that sample handling procedure is likely to result in tobacco altogether
The loss of flavor component, extracting on flavor component has certain influence.
Test result
Title, quota ion and the content of 1 flavor component of table
It include the peak number that goes out including internal standard methyl phenylacetate it can be seen from table 1 and Fig. 1 is 33, from tobacco and tobacco
The flavor component that quantifies isolated in product is 32 kinds, and the minimum concentration of the content detected is 35.90ng/g, illustrates this hair
The flavor component type that bright method is extracted from tobacco and tobacco product is more, and clever with having when gas chromatography/mass spectrometry
Sensitivity is high, detection limits low feature.
Title, quota ion and the content of 2 flavor component of table
When the purging temperature described in step (5) it can be seen from table 2 and Fig. 2 contrast table 1 and Fig. 1 is 60 DEG C, 80 DEG C are compared
When, appearance is reduced, and illustrates that the flavor component extracted is reduced.
3 test result contrast table of table
As can be seen from Table 3, ultrasonic water bath extraction ultrasonic temperature is lower or purge in purging temperature it is lower when,
The inefficient that flavor component extracts, and when the ultrasonic temperature of ultrasonic water bath extraction is excessively high, certain flavor components may be destroyed,
Cause the loss of flavor component.Therefore, only when the purging temperature in the temperature and purge of ultrasonic water bath extraction reaches
It is required that when, it could effectively extract the flavor component in tobacco and tobacco product.In addition, being with sample when sample is smashed tobacco powder
Pipe tobacco comparison, the flavor component detected are reduced, and illustrating that sample handling procedure extracts flavor component to have centainly influences, together
When, the concentration that the bulking value of sample and water compares flavor component in sample ultrasonic water-bath effect of extracting and extract liquor has a fixing
It rings, and then influences subsequent testing result.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (8)
1. a kind of purge and trap method of flavor component in tobacco and tobacco product, which is characterized in that sample using water as extractant,
It is extracted first through ultrasonic water bath, purge and trap is then carried out under salting-out condition；The temperature of ultrasonic water bath extraction is 72~
95 DEG C, the time is 10~120min.
2. the purge and trap method of flavor component, feature exist in a kind of tobacco according to claim 1 and tobacco product
In the salting-out condition is that the sodium chloride that weight percent is 5~35%, the purging of the purge and trap are added in extract liquor
Temperature is 40~95 DEG C.
3. the purge and trap method of flavor component, feature exist in a kind of tobacco according to claim 1 and tobacco product
In including the following steps：
(1) tobacco and tobacco product are handled to the pipe tobacco for being 1mm × 10mm for area；
(2) pipe tobacco is weighed, is mixed with water by constant weight volume ratio, obtains aqueous solution；
(3) ultrasonic water bath extraction is carried out to aqueous solution, obtains extract liquor；
(4) it draws extract liquor to be placed in purging bottle, sodium chloride is added；
(5) sample in purging bottle is purged air through, is bubbled and evaporates flavor component with purge gass by water phase；
(6) it is captured when flavor component passes through collecting trap, then is desorbed and flavor component blowback is entered into gas chromatographic sample introduction mouth, pass through
After chromatography post separation, detected into mass spectrum.
4. according to claim 1~3 in a kind of any described tobacco and tobacco product flavor component purge and trap method,
It is characterized in that, the pipe tobacco and water volume ratio 1 by weight:16~1:18 mixing.
5. according to claim 1~3 in a kind of any described tobacco and tobacco product flavor component purge and trap method,
It is characterized in that, the temperature of the ultrasonic water bath extraction is 80 DEG C, time 60min.
6. according to claim 1~3 in a kind of any described tobacco and tobacco product flavor component purge and trap method,
It is characterized in that, the salting-out condition is that the sodium chloride that weight percent is 25% is added in extract liquor.
7. according to claim 1~3 in a kind of any described tobacco and tobacco product flavor component purge and trap method,
It is characterized in that, the purging temperature of the purge and trap is 80 DEG C.
8. the purge and trap method of flavor component, feature exist in a kind of tobacco according to claim 3 and tobacco product
In desorption temperature is 200 DEG C in step (6)；Desorption time is 2.0min.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114778720A (en) * | 2022-03-31 | 2022-07-22 | 红塔烟草(集团)有限责任公司 | P & T-GC-MS method for detecting characteristic aroma components in tow flavored filter stick |
| CN115201371A (en) * | 2022-07-12 | 2022-10-18 | 榆林学院 | Aromatic plant aroma component detection method |
| CN115326946A (en) * | 2022-06-27 | 2022-11-11 | 红塔烟草(集团)有限责任公司 | Pretreatment method for flavoring glyceryl triacetate for cigarettes |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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