CN101661022A - Method for separating and analyzing volatile and semi-volatile flavor components in tobacco by using liquid chromatography-gas chromatography/mass spectrometry technology - Google Patents

Method for separating and analyzing volatile and semi-volatile flavor components in tobacco by using liquid chromatography-gas chromatography/mass spectrometry technology Download PDF

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Publication number
CN101661022A
CN101661022A CN200910172254A CN200910172254A CN101661022A CN 101661022 A CN101661022 A CN 101661022A CN 200910172254 A CN200910172254 A CN 200910172254A CN 200910172254 A CN200910172254 A CN 200910172254A CN 101661022 A CN101661022 A CN 101661022A
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China
Prior art keywords
tobacco
volatile
liquid chromatography
component
flavor component
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CN200910172254A
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Inventor
刘绍锋
白军超
谢复炜
刘惠民
夏巧玲
张晓兵
赵晓东
郭吉兆
赵阁
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Zhengzhou Tobacco Research Institute of CNTC
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Zhengzhou Tobacco Research Institute of CNTC
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Abstract

A method for separating and analyzing volatile and semi-volatile flavor components in tobacco by using liquid chromatography-gas chromatography/mass spectrometry technology comprises the following steps: 1. taking a given weight of tobacco products and extracting the volatile and semi-volatile flavor components from the tobacco by simultaneously adopting distillation and extraction; 2. concentrating the extracted samples with a concentrator; 3. carrying out group component separation on the concentrated extracted samples by normal-phase liquid chromatography and collecting distillates by different time sections; and 4. concentrating the collected distillates by the concentrator and respectively entering a gas chromatography-mass spectrometer (GC-MS) for detailed analysis. Compared with theprior art, the method of the invention can effectively extract the volatile and semi-volatile flavor components from the tobacco, carry out group component separation on the extract liquor by normal-phase liquid chromatography, then carry out accurate GC-MS qualitative and quantitative analysis on each group component according to different boiling points, not only has good selectivity and high separation efficiency but also ensures more accurate qualitative and quantitative analysis of each component.

Description

Utilize the method for volatility, half volatile flavor component in liquid chromatography-gas chromatography combined with mass spectrometry technical point compartment analysis tobacco
Technical field
The present invention relates to the tobacco component method for separating and analyzing, particularly a kind of method of utilizing volatility, half volatile flavor component in liquid chromatography-gas chromatography combined with mass spectrometry technical point compartment analysis tobacco, this method utilization is distillation extraction simultaneously, concentrating instrument concentrates, then concentrating sample being carried out positive liquid chromatography family separates, and the collection cut, at last the cut of collecting is done the makings analysis, realized, high selectivity compartment analysis efficient to the tobacco flavor composition.
Background technology
Chemical constitution in tobacco and the flue gas is very complicated, according to the pertinent literature report, has had been found that more than 5,000 kind of compound (Dube, M.F.and Green, C.R.36 in tobacco and the cigarette smoke ThTCRC, 1982).In these compounds, smoking property of cigarette there is the flavor component of material impact mainly from volatility in the tobacco and half volatile material.Owing to contain the compound of different structures such as alcohols, aldehydes, ketone, ester class in these volatility, the half volatile flavor component, thereby they are considered to the tobacco components of the more difficult compartment analysis of a class.At present, the analytical approach of tobacco volatility, half volatile flavor component mainly contain one dimension chromatographic separation technology (as vapor-phase chromatography, gas chromatography-mass spectrography) ( -Laakso, T.; Laakso, I.; Hiltunen, R.Anal.Chim.Acta, 2002,465,39-62.) and comprehensive two dimensional gas chromatography-mass spectrometry (deer is loud and clear, Zhong Qiaoxia, Zhao Mingyue, the road is prosperous, Liu Huimin, the He Yang is bright, Liang Lili, Xu Guowang, tobacco science and technology, 2007, the 1 phases, 32-37.)。The one dimension chromatogram is difficult to realize the baseline separation of tobacco complicated ingredient owing to the restriction of chromatographic peak capacity, brings difficulty therefore for the accurate qualitative, quantitative of related component; Comprehensive two dimensional gas chromatography-mass spectrometry has improved the separating power of chromatogram greatly, but because the second dimension gas chromatographic column is shorter, separation is restricted; In addition, also there is the shortcoming that instrument costs an arm and a leg etc. in comprehensive two dimensional gas chromatography-mass spectrometry.
Liquid chromatography-gas chromatography combined with mass spectrometry, because of it has possessed liquid chromatography its specific structure selectivity and gas chromatography simultaneously the different boiling component being carried out the ability of high efficiency separation, is to answer the needs that complex sample separates and a kind of novel two-dimentional chromatographic separation technology that grows up.This technology has been carried out relevant applied research work at environmental analysis and petrochemical industry at present.But, particularly carry out relevant research work yet there are no aspect the tobacco flavor constituent analysis in the tobacco component analysis.
Summary of the invention
Purpose of the present invention provides a kind of volatility important in liquid chromatography-gas chromatography combined with mass spectrometry technical point compartment analysis tobacco, method of half volatile flavor component utilized just at existing weak point in the prior art.This method can be carried out the flavor component in the tobacco earlier the component separation of liquid chromatography family effectively, carries out gas chromatography again and separates, and mass spectrometry is quantitative, thereby realizes the accurate qualitative, quantitative of the flavor component in the tobacco.
The objective of the invention is to be achieved through the following technical solutions: the method for volatility, half volatile flavor component in liquid chromatography-gas chromatography combined with mass spectrometry technical point compartment analysis tobacco of utilizing of the present invention may further comprise the steps successively:
(1) extraction of flavor component in the tobacco;
(2) after extraction is finished, add anhydrous sodium sulfate drying in the extract and spend the night, transfer under the concentrating instrument concentrated then;
(3) concentrating sample is done positive liquid chromatography family component and separate, and time segment is carried out fraction collection;
(4) cut of collecting of respectively organizing is done concentration once more, add the interior mark of specified rate then;
(5) the sample air inlet phase successively chromatograph-mas spectrometer to gained separates, and each group flavor component is carried out qualitative and quantitative analysis;
GC conditions is:
Chromatographic column: DB-5MS (60m * 0.25mm * 0.25 μ m); Temperature programme: 60 ℃ (keeping 1min), 2 ℃/min rises to 280 ℃, keeps 25min.
Described tobacco extracts separates through liquid chromatography family component earlier, and then does the gas chromatography-mass spectrum compartment analysis.
Extraction process adopts the while distilling and extracting device to carry out, and this installs an end and fills a certain amount of tobacco sample, and places heat source furnace to heat; The other end fills dichloromethane extraction liquid, places water-bath to heat;
Described tobacco can be the broken end of tobacco leaf, also can be cigarette shreds.
Described positive liquid chromatography is separated can adopt amino analytical column, also can adopt cyano group, silica gel or alcohol radical isopolarity analytical column.
Described concentration process can blow concentratedly for nitrogen, also can concentrate for rotary evaporation.
Mark can be phenethyl acetate in described, also can be methyl nicotinate.
Outstanding advantage of the present invention is: can extract volatility, half volatile flavor component effectively from tobacco, and with the positive liquid chromatography extract is done family's component and separate, each family's component is done the accurate qualitative and quantitative analysis of GC-MS by the boiling point difference then, existing method separation selectivity is poor, efficient is low thereby solved, and inaccurate etc. the shortcoming of qualitative, quantitative.
Description of drawings
Fig. 1 is the operational flowchart of the inventive method.
Fig. 2 separates spectrogram for the positive liquid chromatography.
Fig. 3-a is gas chromatography-mass spectrometry analysis spectrogram (a first family component).
Fig. 3-b is gas chromatography-mass spectrometry analysis spectrogram (a second family component).
Fig. 3-c is gas chromatography-mass spectrometry analysis spectrogram (three races's component).
Fig. 3-d is gas chromatography-mass spectrometry analysis spectrogram (the 4th family's component).
Fig. 3-e is gas chromatography-mass spectrometry analysis spectrogram (the 5th family's component).
Specific embodiments
The present invention is further described in conjunction with the embodiments, but does not limit the present invention:
The broken end of embodiment tobacco leaf
1. while distilling and extracting device one termination fills the 1000mL flat bottom flask of 25 gram offal, 350mL water and 90g sodium chloride, uses the electric furnace of may command voltage to heat.Another termination of distilling and extracting device fills the 100mL flask of 45mL methylene chloride simultaneously, and this end heats on water-bath, and bath temperature is 60 ℃.After extraction is finished, add the 9g anhydrous sodium sulfate, dried overnight.After extract is concentrated into 1mL.
2. concentrating sample separates through the positive liquid chromatography: select amino analytical column (250mm * 2.0mmi.d.) for use, normal hexane-methylene chloride-acetonitrile (volume ratio is 90: 6.6: 3.4) is as moving phase, and sample size is 5 μ L, and flow rate of mobile phase is 0.2mL/min, under this chromatographic condition, sample after separating is collected successively, obtained 5 groups of components, be respectively a, b, c, d, e.
3. positive liquid phase separation spectrogram is seen accompanying drawing 2.
4. 5 groups of components collecting are concentrated into 1mL respectively under Nitrogen evaporator, adding 10 μ L concentration then is 1.0208 * 10 -2The phenethyl acetate of g/mL is done interior mark, and split sampling does not change gas chromatograph-mass spectrometer over to and does labor at last.The makings analysis condition is as follows:
The GC/MS condition:
TraceGC/DSQ II gas chromatograph-mass spectrometer
Chromatographic column: DB-5MS (60m * 0.25mm i.d. * 0.25 μ m d.f.)
Carrier gas, flow velocity: He, 1.0mL/min
Injector temperature: 240 ℃
Heating schedule: 60 ℃ (keeping 1min), 2 ℃/min was raised to 280 ℃ (keeping 25min)
Sample size: 1 μ L
Ionization voltage: 70ev
Qualitative and quantitative analysis:
Selecting the characteristic ion of compound is quota ion, calculates its relative content with its quota ion area and interior scalar quantity ion area ratio.
5. the makings analysis of spectra is seen Fig. 3 a-3e.
Among Fig. 3-a: 1. solanone, 2. damascenone, 3. geranyl acetone, 4. pohytol, 5. farnesyl acetone, 6. margaric acid.
Among Fig. 3-b: 7. alpha, beta-lonone, 8. six hydrogen actinidia lactones, 9. Megastigmatrienone A, 10. Megastigmatrienone B, 11. Megastigmatrienone C, 12. Megastigmatrienone D.
Among Fig. 3-c: 13. phenylethyl alcohols, 14. acetyl pyrroles, 15. p-Hydroxybenzylalcohols, 16. phenethyl alcohol.
Among Fig. 3-d: 17.3-hydroxyl-damascenone.
Among Fig. 3-e: 18.2,3-dipyridine, 19. hexadecylic acids.

Claims (7)

1, a kind of method of utilizing volatility, half volatile flavor component in liquid chromatography-gas chromatography combined with mass spectrometry technical point compartment analysis tobacco, it is characterized in that: this method may further comprise the steps successively:
(1) extraction of flavor component in the tobacco;
(2) after extraction is finished, add anhydrous sodium sulfate drying in the extract and spend the night, transfer under the concentrating instrument concentrated then;
(3) concentrating sample is done positive liquid chromatography family component and separate, and time segment is carried out fraction collection;
(4) cut of collecting of respectively organizing is done concentration once more, add the interior mark of specified rate then;
(5) the sample air inlet phase successively chromatograph-mas spectrometer to gained separates, and each group flavor component is carried out qualitative and quantitative analysis;
GC conditions is:
Chromatographic column: DB-5MS (60m * 0.25mm * 0.25 μ m); Temperature programme: 60 ℃ (keeping 1min), 2 ℃/min rises to 280 ℃, keeps 25min.
2, the method for volatility, half volatile flavor component in the compartment analysis tobacco according to claim 1 is characterized in that: described tobacco extracts separates through liquid chromatography family component earlier, and then does the gas chromatography-mass spectrum compartment analysis.
3, the method for volatility, half volatile flavor component in the compartment analysis tobacco according to claim 1 is characterized in that: described tobacco can be the broken end of tobacco leaf, also can be cigarette shreds.
4, the method for volatility, half volatile flavor component in the compartment analysis tobacco according to claim 1, it is characterized in that: extraction process adopts the while distilling and extracting device to carry out, this installs an end and fills a certain amount of tobacco sample, and places heat source furnace to heat; The other end fills dichloromethane extraction liquid, places water-bath to heat;
5, the method for volatility, half volatile flavor component in the compartment analysis tobacco according to claim 1 is characterized in that: described positive liquid chromatography is separated can adopt amino analytical column, also can adopt cyano group, silica gel or alcohol radical polarity analytical column.
6, the method for volatility, half volatile flavor component in the compartment analysis tobacco according to claim 1 is characterized in that: described concentration process can blow concentratedly for nitrogen, also can concentrate for rotary evaporation.
7, the method for volatility, half volatile flavor component in the compartment analysis tobacco according to claim 1 is characterized in that: mark can be phenethyl acetate in described, also can be methyl nicotinate.
CN200910172254A 2009-09-24 2009-09-24 Method for separating and analyzing volatile and semi-volatile flavor components in tobacco by using liquid chromatography-gas chromatography/mass spectrometry technology Pending CN101661022A (en)

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CN102253159A (en) * 2011-04-15 2011-11-23 中国烟草总公司郑州烟草研究院 Method for analyzing tobacco flavor components by adopting multi-dimensional hyphenated chromatographic technique
CN102297797A (en) * 2010-06-23 2011-12-28 中国科学院大连化学物理研究所 Gas phase-liquid phase online coupling method for purifying dioxin type sample
CN102565233A (en) * 2012-01-18 2012-07-11 中国烟草总公司郑州烟草研究院 Method for determining volatile and semi-volatile secondary metabolite in fresh tobacco leaves
CN102680627A (en) * 2012-05-15 2012-09-19 上海烟草集团有限责任公司 Method for analyzing and identifying key aromatic substances in tobacco leaf
CN103091417A (en) * 2013-01-15 2013-05-08 云南烟草科学研究院 Method for measuring volatile and semi-volatile neutral scent components in tobacco and sample collection device
CN103162994A (en) * 2013-03-29 2013-06-19 贵州省烟草科学研究院 Ultra-low temperature extraction device and analysis method of smoke aroma components by using ultra-low temperature extraction device
CN103226136A (en) * 2012-10-15 2013-07-31 红塔烟草(集团)有限责任公司 Detection and determination method for flavor type of cigarette
CN104138028A (en) * 2014-07-15 2014-11-12 上海烟草集团有限责任公司 Extraction method for flavor components in tobacco and application of extraction method
CN105203653A (en) * 2015-09-11 2015-12-30 浙江中烟工业有限责任公司 Cigarette paper quality stability testing method
CN105891349A (en) * 2016-03-28 2016-08-24 浙江中烟工业有限责任公司 Method for determining volatile components in tobaccos through infrared-aided headspace solid-phase microextraction-gas chromatography-mass spectrometry
CN106053619A (en) * 2016-05-11 2016-10-26 中国烟草总公司郑州烟草研究院 A high-throughput analysis method for measuring volatile and semi-volatile components in particulate matters of cigarette main stream smoke
CN106404966A (en) * 2016-11-09 2017-02-15 湖北中烟工业有限责任公司 Pretreatment method for analysis of aroma components of reconstituted tobaccos
CN108414640A (en) * 2018-03-27 2018-08-17 云南中烟工业有限责任公司 A kind of high-performance liquid chromatogram determination method of Ethyl vanillin β-D-Glucose glycosides

Cited By (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102297797A (en) * 2010-06-23 2011-12-28 中国科学院大连化学物理研究所 Gas phase-liquid phase online coupling method for purifying dioxin type sample
CN102297797B (en) * 2010-06-23 2013-04-17 中国科学院大连化学物理研究所 Gas phase-liquid phase online coupling method for purifying dioxin type sample
CN102253159A (en) * 2011-04-15 2011-11-23 中国烟草总公司郑州烟草研究院 Method for analyzing tobacco flavor components by adopting multi-dimensional hyphenated chromatographic technique
CN102565233A (en) * 2012-01-18 2012-07-11 中国烟草总公司郑州烟草研究院 Method for determining volatile and semi-volatile secondary metabolite in fresh tobacco leaves
CN102680627A (en) * 2012-05-15 2012-09-19 上海烟草集团有限责任公司 Method for analyzing and identifying key aromatic substances in tobacco leaf
CN103226136A (en) * 2012-10-15 2013-07-31 红塔烟草(集团)有限责任公司 Detection and determination method for flavor type of cigarette
CN103091417A (en) * 2013-01-15 2013-05-08 云南烟草科学研究院 Method for measuring volatile and semi-volatile neutral scent components in tobacco and sample collection device
CN103091417B (en) * 2013-01-15 2014-08-27 云南烟草科学研究院 Method for measuring volatile and semi-volatile neutral scent components in tobacco and sample collection device
CN103162994A (en) * 2013-03-29 2013-06-19 贵州省烟草科学研究院 Ultra-low temperature extraction device and analysis method of smoke aroma components by using ultra-low temperature extraction device
CN104138028B (en) * 2014-07-15 2016-02-24 上海烟草集团有限责任公司 A kind of extracting method of tobacco flavor composition and application thereof
CN104138028A (en) * 2014-07-15 2014-11-12 上海烟草集团有限责任公司 Extraction method for flavor components in tobacco and application of extraction method
CN105203653A (en) * 2015-09-11 2015-12-30 浙江中烟工业有限责任公司 Cigarette paper quality stability testing method
CN105891349A (en) * 2016-03-28 2016-08-24 浙江中烟工业有限责任公司 Method for determining volatile components in tobaccos through infrared-aided headspace solid-phase microextraction-gas chromatography-mass spectrometry
CN106053619A (en) * 2016-05-11 2016-10-26 中国烟草总公司郑州烟草研究院 A high-throughput analysis method for measuring volatile and semi-volatile components in particulate matters of cigarette main stream smoke
CN106053619B (en) * 2016-05-11 2018-10-09 中国烟草总公司郑州烟草研究院 Volatilization in a kind of high throughput assay cigarette mainstream smoke condensate, half volatile ingredient analysis method
CN106404966A (en) * 2016-11-09 2017-02-15 湖北中烟工业有限责任公司 Pretreatment method for analysis of aroma components of reconstituted tobaccos
CN106404966B (en) * 2016-11-09 2019-04-26 湖北中烟工业有限责任公司 A kind of pre-treating method of reconstituted tobacco aroma component analysis
CN108414640A (en) * 2018-03-27 2018-08-17 云南中烟工业有限责任公司 A kind of high-performance liquid chromatogram determination method of Ethyl vanillin β-D-Glucose glycosides

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