CN101178391B - Derivative application process which is suitable for directly determining Cembrane diterpene alcoholate in tobacco and tobacco product - Google Patents
Derivative application process which is suitable for directly determining Cembrane diterpene alcoholate in tobacco and tobacco product Download PDFInfo
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- CN101178391B CN101178391B CN2007101930934A CN200710193093A CN101178391B CN 101178391 B CN101178391 B CN 101178391B CN 2007101930934 A CN2007101930934 A CN 2007101930934A CN 200710193093 A CN200710193093 A CN 200710193093A CN 101178391 B CN101178391 B CN 101178391B
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Abstract
The invention relates to a derivatization reagent which is applicable to the direct measurement of cembrane diterpene alcohol in the tobacco and tobacco products, which is characterized in that: a solvent which is difficult to volatilize (DMF or DMSO) and another silylation reagent (BSTFA or TMCS) are mixed according to a certain proportion and are reacted for special time at a certain temperature to complete the derivatization of the surface components of the tobacco, so as to prepare the sample of the surface substances which can be directly applied in the gas chromatography-mass spectrometry analysis. The derivatization reagent can be combined with the gas chromatography-mass spectrometry, so as to realize the rapid and accurate measurement of the surface substances in the tobacco and tobacco products. The invention has the advantage that the invention can carry out the effective derivatization and the content measurement of cembrane diterpene alcohol, sucrose esters and so on of tobacco and other complicated systems.
Description
Technical field
The present invention relates to the used derivatization reagent of tobacco, particularly a kind of derivatization reagent that is applicable to surface masses such as direct mensuration tobacco and the pure and mild sucrose ester of tobacco product Chinese and Western cypress alkane diterpene, thus this derivatization reagent can with the gas chromatography mass spectrometry analytical approach in conjunction with the surface mass of realizing in rapid and accurate determination tobacco and the tobacco product.
Background technology
Chemical constitution in the tobacco is varied and very complicated, and the pure and mild sucrose ester of western cypress alkane diterpene etc. is a kind of general important chemical constitution distributed more widely in tobacco surface, and they are considered to important fragrance matter precursor.But because comparatively difficult to the extraction and the separation and purification of such material, thereby they are acknowledged as the difficult tobacco components of accurately measuring.The analytical approach of such material roughly has vapor-phase chromatography, gas chromatography mass spectrometry method, LC-MS method in the tobacco at present, 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.Therefore, a kind of reagent that the derivatization of such material is measured that can directly apply to of searching is most important.
Summary of the invention
Purpose of the present invention provides a kind of derivatization reagent and application process thereof that is applicable to direct mensuration tobacco and tobacco product Chinese and Western cypress alkane diterpene alcohol just at existing problem in the prior art, this reagent can be realized effective derivatization with the surface masses such as the pure and mild sucrose ester of western cypress alkane diterpene in the tobacco effectively, thereby realizes the accurate quantification analysis of such material in the tobacco.
The objective of the invention is to be achieved through the following technical solutions: the derivatization reagent of direct mensuration tobacco and tobacco product Chinese and Western cypress alkane diterpene alcohol that is applicable to of the present invention comprises that a kind of difficult solvent flashing and another kind of silylating reagent constitute jointly, wherein difficult solvent flashing and silylating reagent are with 2: 1-1: 2 volume ratio successively joins in the tobacco sample to be measured, described difficult solvent flashing is dimethyl formamide DMF or dimethyl methyl sulfone DMSO, described silylating reagent is N, two (TMS) trifluoroacetamides (BSTFA) of O-or trimethyl chlorosilane (TMCS).
Above-mentioned western cypress alkane diterpene alcohol comprises the diterpene alcohol of α and two kinds of configurations of β.
The derivatization application process of derivatization reagent of the present invention comprises following processing step:
A. earlier difficult solvent flashing dimethyl formamide DMF or dimethyl methyl sulfone DMSO are added in the tobacco sample to be measured that solvent extraction gets, fully mix;
B. again BSTFA or trimethyl chlorosilane TMCS are joined in the testing sample that is mixed with difficult solvent flashing;
C, with said mixture 60-80 ℃ of down reaction 0.5-1.5 hour, the surface mass that can utilize chemical analysis method to carry out in the tobacco sample to be measured is measured.
In the present invention, the addition of difficult solvent flashing tobacco sample to be measured relatively is 20%-80%.
Chemical analysis method of the present invention is the gas chromatography-mass spectrography analysis determining method.
Reagent of the present invention has can be to carrying out effective derivatization such as the pure and mild sucrose ester of western cypress alkane diterpene of the such complex system of tobacco etc. and accurately measuring the advantage of its content.
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 0.4g of 40 mesh sieves in glass flask, add 20ml extraction solvent methylene chloride, at normal temperatures, the ultrasonic extraction frequency is ultrasonic 10min under 50KHz and the ultrasonic power 350w, be cooled to room temperature after, 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 10ml with the methenyl choloride washing.Take out 1 milliliter, under inert gas shielding, be concentrated into do after.Add earlier difficult solvent flashing (as DMF0.25ml), adding silylating reagent (as BSTFA0.25ml) then in proportion, to make cumulative volume be 0.5ml, 70 ℃ of reactions 1 hour down.
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 2000ml extraction solvent methylene chloride, tobacco leaf is dipped three times each six seconds kinds in beaker.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 methenyl choloride.Take out 1 milliliter, under inert gas shielding, be concentrated into dried.Add earlier difficult solvent flashing (as DMSO 0.5ml), adding silylating reagent (as BSTFA0.25ml 0) then in proportion, to make cumulative volume be 0.75ml, 70 ℃ of reactions 1 hour down.
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 500ml extraction solvent methylene chloride, tobacco leaf is dipped five times each six or 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 settled to 10ml with the methenyl choloride washing.Take out 1 milliliter, under inert gas shielding, be concentrated into dried.Add earlier difficult solvent flashing (as DMF0.25ml), adding silylating reagent (as TMCS 0.25ml) then in proportion, to make cumulative volume be 0.5ml, 70 ℃ of reactions 1 hour down.
C, the gained sample is carried out GC-MS analyze.
Claims (1)
1. one kind is applicable to the direct derivatization application process of measuring tobacco and tobacco product Chinese and Western cypress alkane diterpene alcohol, and it is characterized in that: it comprises following processing step:
A. earlier difficult solvent flashing dimethyl methyl sulfone DMSO is added in the tobacco sample to be measured that solvent extraction gets, fully mix, the addition of difficult solvent flashing dimethyl methyl sulfone DMSO tobacco sample to be measured relatively is 20%-80%; The described tobacco sample to be measured that gets through solvent extraction, be through dichloromethane solvent extraction, under 10-13kpa, be concentrated into dried, residue with filter paper filtering, filtrate that anhydrous sodium sulfate is housed and wash constant volume, under inert gas shielding, be concentrated into and do and get with methenyl choloride;
B. again trimethyl chlorosilane TMCS is joined in the testing sample that is mixed with difficult solvent flashing dimethyl methyl sulfone DMSO the volume ratio 2 of DMSO and TMCS: 1-1: 2;
C, with said mixture 70 ℃ of down reactions 1 hour, the surface mass that can utilize the gas chromatography-mass spectrography analysis determining method to carry out in the tobacco sample to be measured is measured.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2007101930934A CN101178391B (en) | 2007-12-12 | 2007-12-12 | Derivative application process which is suitable for directly determining Cembrane diterpene alcoholate in tobacco and tobacco product |
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| CN2007101930934A CN101178391B (en) | 2007-12-12 | 2007-12-12 | Derivative application process which is suitable for directly determining Cembrane diterpene alcoholate in tobacco and tobacco product |
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| CN101178391A CN101178391A (en) | 2008-05-14 |
| CN101178391B true CN101178391B (en) | 2011-07-27 |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103134872B (en) * | 2013-02-18 | 2014-06-11 | 柳州高通食品化工有限公司 | Method for analyzing distribution of various esters in sucrose fatty acid ester with gel permeation chromatography |
| 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 |
| CN104569197B (en) * | 2014-12-30 | 2016-10-26 | 广东中烟工业有限责任公司 | The silanization GC/MS detection method of sugar, 1,2-propylene glycol and the glycerol in mensuration Nicotiana tabacum L. simultaneously |
| CN106483231A (en) * | 2016-10-09 | 2017-03-08 | 江西出入境检验检疫局检验检疫综合技术中心 | The assay method of total monoesters and free propylene glycol content in a kind of methyl glycol fatty acid ester |
| CN110632220B (en) * | 2019-10-31 | 2022-07-08 | 上海烟草集团有限责任公司 | Method for analyzing sucrose ester in tobacco by multi-dimensional liquid chromatography-mass spectrometry |
| CN111094970A (en) * | 2019-12-13 | 2020-05-01 | 广州嘉德乐生化科技有限公司 | Method for analyzing sucrose ester sample |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1616962A (en) * | 2004-09-07 | 2005-05-18 | 常德卷烟厂 | Method for detecting tobacco specific nitrosamine by liquid phase chromatography and series mass spectrometry |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1616962A (en) * | 2004-09-07 | 2005-05-18 | 常德卷烟厂 | Method for detecting tobacco specific nitrosamine by liquid phase chromatography and series mass spectrometry |
Non-Patent Citations (5)
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| DAVID G. WATSON .etal.SESQUITERPENOID PHYTOALEXINS FROM SUSPENDED CALLUS CULTURES OF NICOTIANA TABACUM.《Journal of Chromatography A》.1985,第24卷(第10期),第2195－2200页. |
| DAVID G. WATSON .etal.SESQUITERPENOID PHYTOALEXINS FROM SUSPENDED CALLUS CULTURES OF NICOTIANA TABACUM.《Journal of Chromatography A》.1985,第24卷(第10期),第2195-2200页. * |
| Department Willmitzer.etal.Comprehensive chemical derivatization for gas chromatography–mass spectrometry-based multi-targeted profiling of the major phytohormones.《Phytochemistry》.2003,第993卷第89-102页. * |
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