CN101178390A - Method for determining Cembrane diterpene alcoholate in tobacco and tobacco product by gas chromatography-mass spectrometry - Google Patents
Method for determining Cembrane diterpene alcoholate in tobacco and tobacco product by gas chromatography-mass spectrometry Download PDFInfo
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- CN101178390A CN101178390A CNA200710193092XA CN200710193092A CN101178390A CN 101178390 A CN101178390 A CN 101178390A CN A200710193092X A CNA200710193092X A CN A200710193092XA CN 200710193092 A CN200710193092 A CN 200710193092A CN 101178390 A CN101178390 A CN 101178390A
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Abstract
The invention relates to a method of making use of gas chromatography-mass spectrometry for the measurement of cembrane diterpene alcohol in the tobacco and the tobacco products, which is characterized in that: the invention includes the following steps: a. firstly, a certain amount of tobacco products are taken, a certain amount of extraction solvent halohydrocarbon is added; after that, ultrasonic waves are used for vibration extraction of the diterpene alcohol; b. the extraction solvent is evaporated till the dryness under certain condition and another halohydrocarbon is added, appropriate amount is taken after the dissolution and volume control; c. the taken solvent is evaporated under certain condition, a certain volume of another solvent which is difficult to volatilize and the same proportion of certain silicon derivatization reagent are added, so as to carry out the derivatization under the certain temperature condition. The cembrane diterpene alcohol in which can be measured directly by gas chromatography-mass spectrometry after the full derivatization. Compared with the prior art, the method of the invention can not only carry out the extraction analysis of cembrane diterpene alcohol of the tobacco and other complicated systems, but also has high extraction efficiency, simple and rapid operation.
Description
Technical field
The present invention relates to the tobacco assay method, particularly a kind of method of utilizing gas chromatography-mass spectrography to measure tobacco and tobacco product Chinese and Western cypress alkane diterpene alcohol, this technology is utilized ultrasonic extraction, solvent processing, thus derivatization reagent derivatization and gas chromatography mass spectrometry analysis realize rapid and accurate determination.
Background technology
Chemical constitution in the tobacco is varied and very complicated, and western cypress alkane diterpene alcohol is a kind of general important chemical constitution distributed more widely in the tobacco, and they are considered to important fragrance matter precursor.But because comparatively difficult to the extraction and the separation and purification of western cypress alkane diterpene alcohol, thereby they are considered to one of difficult tobacco components of accurately measuring.The analytical approach of tobacco west cypress alkane diterpene alcohol greatly promptly has vapor-phase chromatography, gas chromatography mass spectrometry method at present, the LC-MS method is arranged again, even thin-layered chromatography all has application.If, then can not realize the separation of these two kinds of materials because gas phase and makings method for combined use do not carry out derivatization treatment when analyzing, when carrying out derivatization treatment, to the grasp yardstick of derivatization condition can cause again accurate quantification be difficult to realize.For liquid phase and liquid matter condition,, these two kinds of materials are realized that baseline separation and accurate quantification analysis are very difficult because of the restriction of extraction solvent and sample introduction solvent.
Summary of the invention
Purpose of the present invention provides the method for utilizing gas chromatography-mass spectrography to measure tobacco and tobacco product Chinese and Western cypress alkane diterpene alcohol just at existing weak point in the prior art.This method can at first realize the western cypress alkane diterpene alcohol in the tobacco to extract fully effectively, carries out a kind of effective derivatization method again, thereby realizes the accurate quantification analysis of the western cypress alkane diterpene alcohol in the tobacco.
The objective of the invention is to be achieved through the following technical solutions: the method for utilizing gas chromatography-mass spectrography to measure tobacco and tobacco product Chinese and Western cypress alkane diterpene alcohol of the present invention may further comprise the steps successively:
(1), the extraction of tobacco product Chinese and Western cypress alkane diterpene alcohol compound: take by weighing tobacco or tobacco product in container, with the diterpene alcohol compound in a kind of halogenated hydrocarbons reagent 1 extracted tobacco or the tobacco product;
(2), extract is concentrated into dried;
(3), use 2 pairs of samples of another kind of chlorohydrocarbon reagent and wash, and constant volume;
(4), the solution 0.5-5ml in the removing step (3) behind the constant volume in a container, be concentrated into dried;
(5), in this container, add a kind of difficult solvent flashing, this difficulty solvent flashing is any one in toluene, ethylene dichloride, dimethyl formamide (DMF) or the dimethyl sulfoxide (DMSO) (DMSO), addition is 0.2-1 a times of dry in the step (4), add silylating reagent simultaneously with difficult solvent flashing equivalent, this this silylating reagent is N, two (TMS) trifluoroacetamides (BSTFA) of O-or trimethyl chlorosilane (TMCS), under 30-90 ℃ a certain temperature silanization 0.5-5 hour;
(6), the gained sample is carried out the gas chromatography-mass spectrography analysis,
Gas phase condition is: chromatographic column: DB-5MS, and 30m * 0.25mm * 2.5 μ m, temperature programme: 120 ℃ (5min), 20 ℃/min rise to 210 ℃, and 0.5 ℃/min rises to 220 ℃ then, and 10 ℃/min rises to 280 ℃.Keep 30min.
In the present invention, described tobacco or tobacco product can be the broken end of tobacco, the blue or green tobacco leaf of flue-cured tobacco or the blue or green tobacco leaf of Turkish tobaccos.Described extraction process can be ultrasonic extraction, also can be to soak extraction, or dips extraction.
Described halogenated hydrocarbons reagent 1 can be and comprises that one of one, two or three carbon atom replaces or polysubstituted hydrocarbon chlorohydrocarbon, includes the interior mark of the pure and mild sucrose octaacetate of n-heptadecane in this reagent.Described chlorohydrocarbon reagent 2 can be methenyl choloride, also can be toluene or 1,2-ethylene dichloride.
In the present invention, can adopt concentrating under reduced pressure when extract concentrates, vacuum tightness is between 5kPa-500kPa, and temperature is controlled between 20-60 ℃.It is to carry out under inert gas shielding or be concentrated into dried at low temperatures that being concentrated in step (4) done process.
Outstanding advantage of the present invention is: can effectively the western cypress alkane diterpene alcohol in the tobacco at first be realized extracting fully, carry out a kind of effective derivatization method again, thereby realize the accurate quantification analysis of the western cypress alkane diterpene alcohol in the tobacco.Method of the present invention not only has the western cypress alkane diterpene alcohol that can extract analysis such as the such complex system of tobacco, and extraction efficiency height, easy and simple to handle, quick.
Description of drawings
Accompanying drawing is the operational flowchart of the inventive method.
Embodiment
The present invention is further described below with reference to embodiment, but does not limit the present invention:
Embodiment 1
A, took by weighing the tobacco sample 0.2-0.5g of 40 mesh sieves in glass flask, the methylene chloride (including the interior mark of the sucrose octaacetate of the pure and mild 6mg/ml of 16mg/ml n-heptadecane) that adds 20-50ml, at normal temperatures, the ultrasonic extraction frequency is ultrasonic 10min under 50KHz and the ultrasonic power 350w, after being cooled to room temperature, with the filter paper elimination offal that the 5g anhydrous sodium sulfate is housed.
B, under 10-13kpa, be concentrated into gained filtrate dried.Residue is settled to 5-10ml with methenyl choloride.Take out 1 milliliter, under inert gas shielding, be concentrated into dried.Add 1: 1 DMF of 500ul: BSTFA, reacted 0.5-1.5 hour down at 60-80 ℃.
C, the gained sample is carried out GC-MS analyze.
Embodiment 2
A, get the blue or green tobacco leaves of two flue-cured tobaccos, in the glass beaker of 5000ml, add 1 of 2000ml, the 2-ethylene dichloride, (including the sucrose octaacetate of the pure and mild 6mg/ml of 16mg/ml n-heptadecane) dips tobacco leaf three times in beaker, each six seconds kinds.Dip in the back solution filter paper filtering that 50 gram anhydrous sodium sulfates are housed.
B, under 10-13kpa, be concentrated into gained filtrate dried.Residue is settled to 50ml with methylene chloride.Take out 1 milliliter, under inert gas shielding, be concentrated into dried.Add 1: 1 DMSO of 500ul: TMCS, reacted 0.5-1.5 hour down at 60-80 ℃.
C, the gained sample is carried out GC-MS analyze.
Embodiment 3
A, get the blue or green tobacco leaves of five Turkish tobaccos, in the glass beaker of 2000ml, add the methenyl choloride (including the sucrose octaacetate of the pure and mild 6mg/ml of 16mg/ml n-heptadecane) of 500ml, tobacco leaf is dipped five times each three seconds kinds in beaker.Dip in the back solution filter paper filtering that 15 gram anhydrous sodium sulfates are housed.
B, under 10-13kpa, be concentrated into gained filtrate dried.Residue is with 1, and the 2-ethylene dichloride is settled to 10ml.Take out 1 milliliter, under inert gas shielding, be concentrated into dried.Add 1: 1 DMF of 500ul: TMCS, reacted 0.5-1.5 hour down at 60-80 ℃.
C, the gained sample is carried out GC-MS analyze.
Claims (7)
1. method of utilizing gas chromatography-mass spectrography to measure tobacco and tobacco product Chinese and Western cypress alkane diterpene alcohol, it is characterized in that: this method may further comprise the steps successively:
(1), the extraction of tobacco product Chinese and Western cypress alkane diterpene alcohol compound: take by weighing tobacco or tobacco product in container, with the diterpene alcohol compound in a kind of halogenated hydrocarbons reagent 1 extracted tobacco or the tobacco product;
(2), extract is concentrated into dried;
(3), use 2 pairs of samples of another kind of chlorohydrocarbon reagent and wash, and constant volume;
(4), the solution 0.5-5ml in the removing step (3) behind the constant volume in a container, be concentrated into dried;
(5), in this container, add a kind of difficult solvent flashing, this difficulty solvent flashing is any one in toluene, ethylene dichloride, dimethyl formamide (DMF) or the dimethyl formamide (DMF), addition is 0.2-1 a times of dry in the step (4), add silylating reagent simultaneously with difficult solvent flashing equivalent, this silylating reagent is N, two (TMS) trifluoroacetamides (BSTFA) of O-or trimethyl chlorosilane (TMCS), under 30-90 ℃ a certain temperature silanization 0.5-5 hour;
(6), the gained sample is carried out the gas chromatography-mass spectrography analysis,
Gas phase condition is: chromatographic column: DB-5MS, and 30m * 0.25mm * 2.5 μ m, temperature programme: 120 ℃ (5min), 20 ℃/min rise to 210 ℃, and 0.5 ℃/min rises to 220 ℃ then, and 10 ℃/min rises to 280 ℃.Keep 30min.
2. the method for mensuration tobacco according to claim 1 and tobacco product Chinese and Western cypress alkane diterpene alcohol is characterized in that: described tobacco or tobacco product can be the broken end of tobacco, the blue or green tobacco leaf of flue-cured tobacco or the blue or green tobacco leaf of Turkish tobaccos.
3. the method for mensuration tobacco according to claim 1 and tobacco product Chinese and Western cypress alkane diterpene alcohol, it is characterized in that: described extraction process can be ultrasonic extraction, also can be to soak extraction, or dips extraction.
4. the method for the western cypress alkane diterpene alcohol in mensuration tobacco according to claim 1 and the tobacco product is characterized in that: halogenated hydrocarbons reagent 1 can be and comprises that one of one, two or three carbon atom replaces or polysubstituted hydrocarbon chlorohydrocarbon.
5. the method for mensuration tobacco according to claim 1 and tobacco product Chinese and Western cypress alkane diterpene alcohol, it is characterized in that: can adopt concentrating under reduced pressure when extract concentrates, vacuum tightness is between 5kPa-500kPa, and temperature is controlled between 20-60 ℃.
6. the method for mensuration according to claim 1 tobacco and tobacco product Chinese and Western cypress alkane diterpene alcohol is characterized in that: chlorohydrocarbon reagent 2 can be methenyl choloride, also can be methylene chloride or 1,2-ethylene dichloride.
7. the method for mensuration according to claim 1 tobacco and tobacco product Chinese and Western cypress alkane diterpene alcohol is characterized in that: in the step (4) to be concentrated into the process of doing be to carry out under inert gas shielding, or under the cryoconcentration process, carry out.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102590412A (en) * | 2012-01-18 | 2012-07-18 | 中国烟草总公司郑州烟草研究院 | Method for detecting secondary metabolites in fresh tobacco leaves by using derivatization GC-MS |
| CN104101662A (en) * | 2014-08-01 | 2014-10-15 | 中国烟草总公司郑州烟草研究院 | Metabonomics method for testing terpenoids in fresh tobacco leaves |
| CN104655772A (en) * | 2014-12-30 | 2015-05-27 | 广东中烟工业有限责任公司 | Method for detecting alpha-2, 7, 11-cembrane triene-4, 6-diol (alpha-CBD) in tobacco |
| CN105001052A (en) * | 2015-07-03 | 2015-10-28 | 中国农业科学院烟草研究所 | Method used for extracting cembrenediols from tobacco inflorescence |
| CN105891367A (en) * | 2016-04-27 | 2016-08-24 | 中国烟草总公司郑州烟草研究院 | Gas chromatography-quadrupole time-of-flight mass spectrometry/flame ionization detection method for tobacco essence perfume |
| CN106290605A (en) * | 2016-07-22 | 2017-01-04 | 云南中烟工业有限责任公司 | One assay method growing tobacco middle sesquiterpenoids |
| CN109633014A (en) * | 2018-12-29 | 2019-04-16 | 中国烟草总公司郑州烟草研究院 | The method and its application of 21 kinds of terpenoid contents in a kind of measurement tobacco leaf |
| CN111812038A (en) * | 2020-06-05 | 2020-10-23 | 宜宾北方川安化工有限公司 | Method for determining content of sucrose octaacetate in double-base gunpowder |
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| CN1288439C (en) * | 2004-09-07 | 2006-12-06 | 常德卷烟厂 | Method for detecting tobacco specific nitrosamine by liquid phase chromatography and series mass spectrometry |
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2007
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102590412A (en) * | 2012-01-18 | 2012-07-18 | 中国烟草总公司郑州烟草研究院 | Method for detecting secondary metabolites in fresh tobacco leaves by using derivatization GC-MS |
| CN102590412B (en) * | 2012-01-18 | 2014-06-25 | 中国烟草总公司郑州烟草研究院 | Method for detecting secondary metabolites in fresh tobacco leaves by using derivatization GC-MS |
| CN104101662A (en) * | 2014-08-01 | 2014-10-15 | 中国烟草总公司郑州烟草研究院 | Metabonomics method for testing terpenoids in fresh tobacco leaves |
| CN104101662B (en) * | 2014-08-01 | 2015-07-08 | 中国烟草总公司郑州烟草研究院 | Metabonomics method for testing terpenoids in fresh tobacco leaves |
| CN104655772A (en) * | 2014-12-30 | 2015-05-27 | 广东中烟工业有限责任公司 | Method for detecting alpha-2, 7, 11-cembrane triene-4, 6-diol (alpha-CBD) in tobacco |
| CN105001052A (en) * | 2015-07-03 | 2015-10-28 | 中国农业科学院烟草研究所 | Method used for extracting cembrenediols from tobacco inflorescence |
| CN105891367A (en) * | 2016-04-27 | 2016-08-24 | 中国烟草总公司郑州烟草研究院 | Gas chromatography-quadrupole time-of-flight mass spectrometry/flame ionization detection method for tobacco essence perfume |
| CN105891367B (en) * | 2016-04-27 | 2018-06-15 | 中国烟草总公司郑州烟草研究院 | A kind of gas-chromatography of essence spice for cigarette-quadrupole rod flight time mass spectrum/flame ion detection method |
| CN106290605A (en) * | 2016-07-22 | 2017-01-04 | 云南中烟工业有限责任公司 | One assay method growing tobacco middle sesquiterpenoids |
| CN106290605B (en) * | 2016-07-22 | 2018-06-12 | 云南中烟工业有限责任公司 | One assay method for growing tobacco middle sesquiterpenoids |
| CN109633014A (en) * | 2018-12-29 | 2019-04-16 | 中国烟草总公司郑州烟草研究院 | The method and its application of 21 kinds of terpenoid contents in a kind of measurement tobacco leaf |
| CN109633014B (en) * | 2018-12-29 | 2022-05-24 | 中国烟草总公司郑州烟草研究院 | Method for measuring contents of 21 terpenoids in tobacco leaves and application thereof |
| CN111812038A (en) * | 2020-06-05 | 2020-10-23 | 宜宾北方川安化工有限公司 | Method for determining content of sucrose octaacetate in double-base gunpowder |
| CN111812038B (en) * | 2020-06-05 | 2023-09-01 | 宜宾北方川安化工有限公司 | Method for measuring content of sucrose octaacetate in double-base gunpowder |
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