CN103267819A - Method to analyze tobacco glycoside through derivatization - Google Patents
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- CN103267819A CN103267819A CN2013101241439A CN201310124143A CN103267819A CN 103267819 A CN103267819 A CN 103267819A CN 2013101241439 A CN2013101241439 A CN 2013101241439A CN 201310124143 A CN201310124143 A CN 201310124143A CN 103267819 A CN103267819 A CN 103267819A
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Abstract
The invention discloses a method to analyze tobacco glycoside through derivatization, which adopts N-methylene bis (trifluoro acetamide) as the derivatization reagent to derivate the extracted purified tobacco glycoside directly, and then utilizes a GC-MS for qualitative and quantitative analysis. The invention is provided with features like simple design, good reappearance, high accuracy, fast analysis speed etc, and is suitable for simultaneous detection to multiple glycosides components in tobaccos of different types.
Description
Technical field
The invention belongs to the tobacco chemistry analysis field, be specifically related to the method that a kind of derivatization method is analyzed the tobacco glucosides.
Background technology
Glucosides is dehydration such as the hydroxyl, amino, thiol base in the hemiacetal hydroxyl of monose or compound sugar and another molecule and the compound that produces, is the compound that sugar or sugared derivant and aglucon are connected to form by glycosidic bond.Tobacco glucosides class material is the secondary metabolite that tobacco forms in growth and development process, and it can discharge the fragrance component of free state by self enzymolysis.Glucosides can also discharge the compound with fragrance fragrance through high temperature heating or burning cracking, thereby improves the fragrance matter of cigarette smoke, increases perfume quantity.In addition, glucosides itself also can provide the jealous of fragrant, sweet and typical this perfume (or spice) of tobacco.So glucoside compound has material impact to quality and the style and features of tobacco.
Chromatographic process analysis is often adopted in the analysis of glucosides in the tobacco leaf, and at present, acidolysis or enzymolysis-gas chromatography-mass spectrography (GC-MS) and liquid chromatograph mass spectrography method (LC-MS) are main analytical approach.Acidolysis mainly is under heating and acid condition, with the glycosidic bond fracture, discharges free state fragrance component and corresponding saccharide residue.Although it is simple, easy to operate and easily to characteristics such as isolated compound are qualitative that acidolysis has; but glucosides is when acidolysis; its aglycone (aroma substance part) usually can produce rearrangement, and the material that causes detecting is not in esse composition in the tobacco, thereby produces wrong judgement.In addition, this method also can't be learnt the composition of saccharide residue.Enzymolysis is the single-minded and high efficiency of utilizing glycosidase, uses corresponding glycosidase the glycosidic bond hydrolysis, thereby discharges corresponding aglycone and saccharide residue.The enzymolysis glucosides can not produce rearrangement in conjunction with the attitude fragrance component, can identify corresponding aglycone accurately, evaluation to glucosides is very helpful, but the degree of glycosidase hydrolysis glucosides is subjected to the influence of aglycone structure, cause glucosides enzymolysis degree difference under identical enzymatic hydrolysis condition of different structure, thereby produce certain error.In addition, enzymolysis is consuming time longer, is unfavorable for the detection of gross sample.The glucosides fragrance component that liquid chromatograph mass spectrography is measured in the tobacco also has a spot of report.The liquid chromatography biggest advantage is that the glucosides extract need not acidolysis, enzymolysis or derivatization, and direct injection analysis gets final product.Although liquid chromatography-mass spectrography pre-treatment condition is simple, there is very big defective in the structural confirmation aspect, and in addition, liquid chromatography also can't well be separated the very similar glucosides of structure, and degree of separation is lower than gas chromatography.
The present invention is directed to the existing deficiency that exists in the tobacco glucosides composition technology of analyzing improves, specialized designs a kind of derivatization reagent directly the tobacco glucosides composition behind the extraction and cleaning is carried out derivatization, utilize gas chromatograph-mass spectrometer to carry out qualitative and quantitative analysis then, can be used for analysis and the quality evaluation of multiple glucosides composition in the tobacco.This method simplicity of design practicality can be analyzed multiple glucosides composition in the dissimilar tobaccos simultaneously.This method is compared than existing method, the tobacco aglycone can not be subjected to the influence of external condition (as acidolysis) and produce rearrangement reaction, different glucosides compositions its derivatization efficient unanimity under identical derivatization condition has guaranteed the consistance that different glucosides are analyzed simultaneously simultaneously.This method has characteristics such as simplicity of design, favorable reproducibility, accuracy height, analysis speed be fast simultaneously, detects when being fit in the dissimilar tobaccos multiple glucosides composition.
Summary of the invention
The technical problem to be solved in the present invention is: have rearrangement reaction at acidolysis disposal route of the prior art, and the degree of enzyme hydrolysis glucosides is subjected to the influence of aglycone structure, the glucosides enzymolysis degree difference under identical enzymatic hydrolysis condition that causes different structure, can produce certain deficiencies such as experimental error, the present invention has designed a kind of derivatization reagent and directly the tobacco glucosides composition behind the extraction and cleaning has been carried out derivatization, utilize gas chromatograph-mass spectrometer to carry out qualitative and quantitative analysis then, can be used for the analysis of multiple glucosides composition in the tobacco, thereby cigarette quality is carried out objective evaluation, the present invention has simplicity of design, favorable reproducibility, the accuracy height, characteristics such as analysis speed is fast detect when being fit in the dissimilar tobaccos multiple glucosides composition.
The present invention may further comprise the steps the assay method of glucosides composition in the tobacco:
(1) extract: take by weighing tobacco powder to tool plug triangular flask, the adding methanol extract liquid is ultrasonic, gets supernatant liquor after leaving standstill and filters, and filtrate is concentrated near doing with Rotary Evaporators, and is to be clean;
(2) purify: the extract in above-mentioned (1) is dissolved it with deionized water, lysate is transferred in the XAD-2 macroporous resin column, use earlier water wash, use ether drip washing again, the eluent of wash-out is carried out in collection with ethyl acetate, eluent with anhydrous sodium sulfate drying after, with Rotary Evaporators it is concentrated, treat derivatization;
(3) derivatization: the concentrate after above-mentioned (2) purified is transferred in the chromatogram bottle and dries up with Nitrogen evaporator, add (MBTFA) derivatization reagent of pyridine solution and N-methyl two (trifluoroacetamide) simultaneously, fully shake up the back and react in water-bath, reaction finishes the back cooling, treats the sample introduction analysis;
(4) carry out qualitative and quantitative analysis with gas chromatograph-mass spectrometer, select mass spectral two kinds of ionization mode-electron impact ion sources (EI) and negative chemical ionization source (NCI) simultaneously target compound to be carried out qualitative evaluation, mark relative quantification method is carried out quantitative test to glycoside compounds in selecting.
The gas chromatography mass spectrometry of selecting among the present invention (GC-MS) analysis condition:
Gas chromatography-electron ionization-mass spectrum (GC-EI-MS) method: chromatographic column: HP-5MS (60 m * 0.25 mmi.d. * 0.25 μ md.f.); Sample size: 2 μ L; Do not shunt; Carrier gas: helium; Flow velocity: 0.8 mL/min; Injector temperature: 280 ℃; Temperature programme: 150 ℃ of initial temperatures.Keep 2min, the speed with 4 ℃ of per minutes is elevated to 210 ℃ then, keeps 2 min, and the speed with 5 ℃ of per minutes is elevated to 280 ℃ again, keeps 30 min; Ion source temperature: 230 ℃, level Four bar temperature: 150 ℃; Ionization energy: 70 eV, the transmission line temperature: 280 ℃, full scan mass number scope 40-600 aum, solvent delay: 8.00 min; Drainage pattern: full scan (Scan) is gathered.
Gas chromatography-negative chemical ionization-mass spectrum (GC-NCI-MS) method: chromatographic column: HP-5MS (60 m * 0.25 mmi.d. * 0.25 μ md.f.); Sample size: 2 μ L; Do not shunt; Carrier gas: helium; Flow velocity: 0.8 mL/min; Injector temperature: 280 ℃; Temperature programme: 150 ℃ of initial temperatures; Keep 2 min, the speed with 4 ℃ of per minutes is elevated to 210 ℃ then, keeps 2 min, and the speed with 5 ℃ of per minutes is elevated to 280 ℃ again, keeps 30 min; Ion source temperature: 150 ℃, level Four bar temperature: 150 ℃; Ionization energy: 128 eV, filament current are 49.5 μ A transmission line temperature: 280 ℃, methane gas (99.995%) flow is 40 mL/min, full scan mass number scope 100-1050 amu, solvent delay: 8.00 min; Drainage pattern: full scan (Scan) is gathered.
Among the present invention, selected gas chromatograph-mass spectrometer is provided by Agilent, and the Rotary Evaporators of selection is provided by HEIDOLPH, and the Nitrogen evaporator of selection is provided by U.S. Organomation.
The derivatization reagent of selecting among the present invention be N-methyl two (trifluoroacetamides) (MBTFA).
The decontaminating column of selecting among the present invention is the XAD-2 macroporous resin column.
The interior mark compound of selecting among the present invention is phenyl-β-D-glucopyranoside.
The beneficial effect that the present invention reaches: by analyzing the mass spectrum information under electron impact ion source (EI) and two kinds of different ions source effects of negative chemical ionization source (NCI), its makings separating effect is seen accompanying drawing 2 and accompanying drawing 3 respectively, respectively the glycosyl behind the derivatization and aglycone are carried out the mass spectrum evaluation, identified the basic structure of 16 kinds of glycoside compounds in the tobacco.Solve acidolysis disposal route of the prior art and had rearrangement reaction; The degree of enzyme hydrolysis glucosides is subjected to the influence of aglycone structure, causes glucosides enzymolysis degree difference under identical enzymatic hydrolysis condition of different structure, can produce certain deficiencies such as experimental error.
The present invention is simultaneously through parallel five times precision test, 16 kinds of glycoside compounds of the tobacco of analyzing stability better, its relative standard deviation (RSD) all is lower than below 10%, wherein except the relative standard deviation (RSD) of P8, P12, P14 glycoside compounds between 5%-10%, the relative standard deviation of all the other glycoside compounds (RSD) all is lower than below 5%, shows that this method has stability and reappearance preferably.
Description of drawings:Fig. 1 is the chemical equation of tobacco glucosides class derivatization.
Fig. 2 is GC-EI-MS chromatogram behind the tobacco glucosides derivatization.
GC-NCI-MS chromatogram behind Fig. 3 tobacco glucosides derivatization.
Embodiment:
The present invention is further described by following instantiation, but does not limit the present invention.
(1) pre-treatment
Take by weighing in 2.0000g tobacco powder sample to the 100 mL tool plug triangular flask, the interior mark phenyl-β-D-glucopyranoside that adds 250 μ g, ultrasonic extraction 30 min of methyl alcohol that add 20 mL simultaneously leave standstill and get supernatant liquor behind 15 min and filter, and filtrate is concentrated near doing with Rotary Evaporators.Deionized water with 25 mL dissolves it then, lysate is transferred in the XAD-2 macroporous resin column, discard with 50 mL water wash earlier, discard with 50 mL ether drip washing again, advance wash-out with 100 mL ethyl acetate at last, eluent with anhydrous sodium sulfate drying after, with Rotary Evaporators it is steamed to 1 mL, with Nitrogen evaporator it is dried up again, the N-methyl two (trifluoroacetamide) that adds the pyridine of 500 μ L and 30 μ L simultaneously is derivatization reagent (MBTFA), fully shake up the back at 60 ℃ of water-bath 50 min, reaction finishes the back cooling, and last gas chromatography mass spectrometry carries out qualitative and quantitative analysis to sample.
(2) the qualitative and quantitative test of instrument:
The present invention carries out qualitative analysis to the tobacco glucosides composition behind the derivatization respectively by the mass spectral two kinds of ionization source mode-electron impact ion sources of single level Four bar (EI) and negative chemical ionization source (NCI), and mark relative quantification method is carried out quantitative test in adopting, simultaneously this method is carried out precision test (n=5), its analysis result sees Table 1.
Gas chromatography-electron ionization-mass spectrum (GC-EI-MS) analysis condition: chromatographic column: HP-5MS (60 m * 0.25 mmi.d. * 0.25 μ md.f.); Sample size: 2 μ L; Do not shunt; Carrier gas: helium; Flow velocity: 0.8 mL/min; Injector temperature: 280 ℃; Temperature programme: 150 ℃ of initial temperatures; Keep 2min, the speed with 4 ℃ of per minutes is elevated to 210 ℃ then, keeps 2 min, and the speed with 5 ℃ of per minutes is elevated to 280 ℃ again, keeps 30 min; Ion source temperature: 230 ℃, level Four bar temperature: 150 ℃; Ionization energy: 70 eV, the transmission line temperature: 280 ℃, full scan mass number scope 40-600 aum, solvent delay: 8.00 min; Drainage pattern: full scan (Scan) is gathered.
Gas chromatography-negative chemical ionization-mass spectrum (GC-NCI-MS) analysis condition: chromatographic column: HP-5MS (60 m * 0.25 mmi.d. * 0.25 μ md.f.); Sample size: 2 μ L; Do not shunt; Carrier gas: helium; Flow velocity: 0.8 mL/min; Injector temperature: 280 ℃; Temperature programme: 150 ℃ of initial temperatures.Keep 2 min, the speed with 4 ℃ of per minutes is elevated to 210 ℃ then, keeps 2 min, and the speed with 5 ℃ of per minutes is elevated to 280 ℃ again, keeps 30 min; Ion source temperature: 150 ℃, level Four bar temperature: 150 ℃; Ionization energy: 128 eV, filament current are 49.5 μ A transmission line temperature: 280 ℃, methane gas (99.995%) flow is 40 mL/min, full scan mass number scope 100-1050 amu, solvent delay: 8.00 min; Drainage pattern: full scan (Scan) is gathered.
Mass spectrum information and the precision data of 16 kinds of glycoside compounds in the tobacco that employing the inventive method obtains, it is five times that relative standard deviation (RSD) is measured number of times, concrete data see Table 1.
Embodiment 2
Adopt the method for the embodiment of the invention 1 to select first flue-cured tobacco, Turkish tobaccos and suncured tabacco to carry out the detection analysis of glucosides component content respectively.The first flue-cured tobacco place of production is the Guiding, Guizhou, and the Turkish tobaccos place of production is the Liangshan Mountain, Yunnan, and the suncured tabacco place of production is the Guizhou Jianhe, is the middle part blade, and specimen in use is undressed preceding tobacco leaf, and after tobacco leaf advanced redrying or processing processing, the content of glucosides might change.Data are three times and measure mean value, and its analysis result sees Table 2:
Claims (4)
1. a derivatization method is analyzed the method for tobacco glucosides, may further comprise the steps:
(1) extract: take by weighing tobacco powder to tool plug triangular flask, the adding methanol extract liquid is ultrasonic, gets supernatant liquor after leaving standstill and filters, and filtrate is concentrated near doing with Rotary Evaporators, and is to be clean;
(2) purify: the extract in above-mentioned (1) is dissolved it with deionized water, lysate is transferred in the XAD-2 macroporous resin column, use earlier water wash, use ether drip washing again, the eluent of wash-out is carried out in collection with ethyl acetate, eluent with anhydrous sodium sulfate drying after, with Rotary Evaporators it is concentrated, treat derivatization;
(3) derivatization: the concentrate after above-mentioned (2) purified is transferred in the chromatogram bottle and dries up with Nitrogen evaporator, add two (trifluoroacetamide) derivatization reagents of pyridine solution and N-methyl simultaneously, fully shake up the back and react in water-bath, reaction finishes the back cooling, treats the sample introduction analysis;
(4) carry out qualitative and quantitative analysis with gas chromatograph-mass spectrometer, select mass spectral two kinds of ionization mode-electron impact ion sources and negative chemical ionization source simultaneously target compound to be carried out qualitative evaluation, mark relative quantification method is carried out quantitative test to glycoside compounds in selecting.
2. a kind of derivatization method according to claim 1 is analyzed the method for tobacco glucosides, it is characterized in that: gas chromatography-electron ionization-mass spectrophotometry condition: chromatographic column: HP-5MS; Sample size: 2 μ L; Do not shunt; Carrier gas: helium; Flow velocity: 0.8 mL/min; Injector temperature: 280 ℃; Temperature programme: 150 ℃ of initial temperatures; Keep 2min, the speed with 4 ℃ of per minutes is elevated to 210 ℃ then, keeps 2 min, and the speed with 5 ℃ of per minutes is elevated to 280 ℃ again, keeps 30 min; Ion source temperature: 230 ℃, level Four bar temperature: 150 ℃; Ionization energy: 70 eV, the transmission line temperature: 280 ℃, full scan mass number scope 40-600 aum, solvent delay: 8.00 min; Drainage pattern: full scan collection.
3. a kind of derivatization method according to claim 1 is analyzed the method for tobacco glucosides, it is characterized in that:
Gas chromatography-negative chemical ionization-mass spectrophotometry condition: chromatographic column: HP-5MS; Sample size: 2 μ L; Do not shunt; Carrier gas: helium; Flow velocity: 0.8 mL/min; Injector temperature: 280 ℃; Temperature programme: 150 ℃ of initial temperatures; Keep 2 min, the speed with 4 ℃ of per minutes is elevated to 210 ℃ then, keeps 2 min, and the speed with 5 ℃ of per minutes is elevated to 280 ℃ again, keeps 30 min; Ion source temperature: 150 ℃, level Four bar temperature: 150 ℃; Ionization energy: 128 eV, filament current are 49.5 μ A, the transmission line temperature: 280 ℃, the methane gas flow is 40 mL/min, full scan mass number scope 100-1050 amu, solvent delay: 8.00 min; Drainage pattern: full scan collection.
4. analyze the method for tobacco glucosides according to each described a kind of derivatization method of claim 1 ~ 3, it is characterized in that: interior mark compound is phenyl-β-D-glucopyranoside.
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| CN104569197A (en) * | 2014-12-30 | 2015-04-29 | 广东中烟工业有限责任公司 | Silylation GC/MS (gas chromatography-mass spectrometry) detection method for simultaneous determination of saccharide, 1, 2-propylene glycol and glycerin in tobacco |
| CN104849393A (en) * | 2015-06-09 | 2015-08-19 | 安徽中烟工业有限责任公司 | Method for determining glucosidic bonded fragrance component in tobacco |
| CN106442794A (en) * | 2016-10-21 | 2017-02-22 | 安徽农业大学 | Method for separating and detecting coniferyl alcohol and sinapyl alcohol through gas chromatography-mass spectrometry (GC-MS) |
| CN107827939A (en) * | 2017-10-26 | 2018-03-23 | 盐城市春竹香料有限公司 | A kind of glucoside and preparation method thereof and its purposes |
| JP2019517005A (en) * | 2016-02-26 | 2019-06-20 | プロザイム，インコーポレイテッド | Use of bispyridines to improve the labeling of nucleophiles |
| CN110824075A (en) * | 2019-10-16 | 2020-02-21 | 西北农林科技大学 | Extraction and purification method of grape aroma glucoside and warehouse building identification quantification method thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104569197A (en) * | 2014-12-30 | 2015-04-29 | 广东中烟工业有限责任公司 | Silylation GC/MS (gas chromatography-mass spectrometry) detection method for simultaneous determination of saccharide, 1, 2-propylene glycol and glycerin in tobacco |
| 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 |
| CN104849393A (en) * | 2015-06-09 | 2015-08-19 | 安徽中烟工业有限责任公司 | Method for determining glucosidic bonded fragrance component in tobacco |
| JP2019517005A (en) * | 2016-02-26 | 2019-06-20 | プロザイム，インコーポレイテッド | Use of bispyridines to improve the labeling of nucleophiles |
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| CN106442794A (en) * | 2016-10-21 | 2017-02-22 | 安徽农业大学 | Method for separating and detecting coniferyl alcohol and sinapyl alcohol through gas chromatography-mass spectrometry (GC-MS) |
| CN106442794B (en) * | 2016-10-21 | 2018-12-18 | 安徽农业大学 | A kind of method of gas chromatography mass spectrometry separation detection coniferyl alcohol and sinapinic alcohol |
| CN107827939A (en) * | 2017-10-26 | 2018-03-23 | 盐城市春竹香料有限公司 | A kind of glucoside and preparation method thereof and its purposes |
| CN110824075A (en) * | 2019-10-16 | 2020-02-21 | 西北农林科技大学 | Extraction and purification method of grape aroma glucoside and warehouse building identification quantification method thereof |
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Application publication date: 20130828 |