CN104849393A - Method for determining glucosidic bonded fragrance component in tobacco - Google Patents
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Abstract
The invention discloses a method for determining glucosidic bonded fragrance components in tobacco. The method comprises the following steps: drying tobacco leaves, crushing, screening, sequentially performing rough extraction and fine extraction so as to obtain a refined tobacco glucosidic extract, adding an internal standard solution into the refined tobacco glucosidic extract, blow-drying the refined tobacco glucosidic extract with N2, and adding a derivatization solvent and an acylation reagent for derivatization, thereby obtaining a tobacco glucosidic derivatization product; analyzing the tobacco glucosidic derivatization product by using a gas chromatograph-mass spectrometer. By adopting the method, glucosidic bonded fragrance components in tobacco not only can be completely extracted, but also can be effectively separated and purified, and meanwhile due to derivatization and analysis with the gas chromatograph-mass spectrometer, qualitative and quantitative analysis on the glucosidic bonded fragrance components in tobacco can be comprehensively and accurately achieved.
Description
One, technical field
The present invention relates to an assay method growing tobacco middle glycoside link state flavor component, belong to Tobacco Analysis field.
Two, background technology
The fundamental purpose that people smoke enjoys tobacco to burn and suck the pleasant fragrances produced in process, meets psychological and physiological demand, so tobacco flavor is the central factor of cigarette quality.Since 20 century 70s, carried out large quantifier elimination both at home and abroad to the aroma component of tobacco, report, for natural plants, aroma component not only exists with the form of free state, also exists with bonding state forms such as glucosides.It is be present in tobacco leaf with the form of glucosides greatly that tobacco gathers some volatile flavor compounds, and they have important impact for tobacco modulation, fragrance release, organoleptic quality.
Glucosides is the compound that sugar or sugared derivant and aglucon are connected to form by glycosidic bond, glucosides class material in tobacco is the secondary metabolite that tobacco leaf is formed in growth course, molecular weight is larger, boiling point is higher, fragrance is less or itself do not have fragrance, but burn and suck in process at cigarette and can discharge fragrance fragrance through high-temperature heating or burning cracking, have very large contribution to the quality of cigarette.
The dive development & application of Studies of The Aromatic Substances of glucosides class is the important directions of current tobacco essence spices, but due to the bottleneck of analysis means, for the endogenous latent Studies of The Aromatic Substances of tobacco, particularly glycosidic bond and state flavor component are not also in depth understood and utilized fully at present.What glucoside compound specifically exist in conjunction with state form with, and the composition in each tobacco leaf and the difference of content and how to shift in flue gas are studied less.And, because glucosides class material is tobacco leaf secondary metabolite, of a great variety and be difficult to obtain standard specimen, commonsense method cannot carry out the research of qualitative, quantitative accurately.At present conventional analytical approach is acidolysis or enzymolysis processing, and then by Gc-ms, its shortcoming is that acid hydrolysis is relatively more violent, does not have a selectivity, truly can not reflect glucosides constituents in tobacco; And enzymolysis is consuming time longer, the selection for enzyme requires higher, and cannot judge the composition of glucosides glycogen part exactly.
Three, summary of the invention
The present invention aims to provide an assay method growing tobacco middle glycoside link state flavor component, to solve the deficiency of existing analytical approach, can carry out qualitative and quantitative analysis to glycoside link state flavor component in tobacco comprehensively, exactly.
In tobacco of the present invention, the assay method of glycoside link state flavor component comprises the following steps:
(1) extract: cross 40 mesh sieves after drying tobacco being pulverized and obtain offal, take 1g offal and put into container, add 20-50mL Extraction solvent, extract glycosidic bond and state flavor component, after getting supernatant liquid filtering, evaporated under reduced pressure solvent obtains tobacco glucosides crude extract.
(2) separation and purification: tobacco glucosides crude extract step (1) obtained is dissolved in 10mL deionized water, be added on solid-phase extraction column, solid-phase extraction column is slow transitted through with 0.5mL/min, use 20mL ultrapure water, 15mL n-pentane/methylene chloride (volume ratio 2:1) wash-out more successively, elution speed is no more than 1.0mL/min, finally uses 20mL methanol-eluted fractions, and elution speed is 2.0mL/min, collect meoh eluate, be concentrated into and dryly obtain tobacco glucosides extract.
(3) derivatization: add inner mark solution 1mL (methanol solution of 2-nitrobenzene-β-D-Glucose glycosides, concentration 1.0mg/mL) in the tobacco glucosides extract that step (2) obtains, N
2dry up, add 400 μ L derivatization solvents and 400 μ L acylating reagents, in 50-80 DEG C of water-bath derivatization 60min after sealing, be cooled to room temperature, obtain tobacco glucosides derivatization product.
(4) analyze:
Gc-ms is carried out to tobacco glucosides derivatization product.
Chromatographic condition: chromatographic column is DB-5MS post (30m*0.25mm*0.25 μm), temperature programme, initial temperature 120 DEG C, keeps 1min, rises to 220 DEG C, then rise to 280 DEG C with 5 DEG C/min with 3 DEG C/min, keeps 10min.Sample size 1.0 μ L, split ratio 10:1, injector temperature 240 DEG C.
Mass Spectrometry Conditions: ion source temperature 230 DEG C, level Four bar temperature 150 DEG C, Ionization mode EI, electron energy 70eV, scan pattern is full scan, mass range 40-600amu.Aglycon adopts standard substance and NIST to compose storehouse according to qualitative, quantitatively adopts and calculates (assuming that response coefficient is equal) with the derivatization product area ratio of the interior 2-of marking nitrobenzene-β-D-Glucose glycosides.
Tobacco of the present invention comprises flue-cured tobacco, burley tobaccos or Turkish tobaccos.
Described leaching process comprises ultrasonic extraction, concussion is extracted or surname extraction.
Described Extraction solvent comprises water, methyl alcohol, ethanol, ethyl acetate or acetone.
Described SPE solid phase extraction column stuffing comprises Amberlite XAD-2 (Sigma Co., USA), D101 (Anhui Samsung resin) or HP-20 (Mitsubishi chemistry), is commercial goods.
Described derivatization solvent comprises methylene chloride, acetone or pyridine.
Described acylating reagent comprises acetic anhydride, N-methyl-two (trifluoroacetamide), trifluoroacetic anhydride, PFPA or heptafluorobutyric anhydride.
The present invention can not only extract completely to glycoside link state flavor component in tobacco, and can carry out effective abstraction and purification to it.Meanwhile, utilize derivatization and gas chromatography mass spectrometry methods analyst, qualitative and quantitative analysis can be carried out to glycosidic bond in tobacco and state flavor component comprehensively, exactly.More traditional acidolysis or enzymolysis analysis method, the method is consuming time shorter, easy and simple to handle, and accurately can reflect the structure of aglycon and glycogen simultaneously.
Four, accompanying drawing explanation
Fig. 1 is the TIC figure (A: embodiment 1 that in embodiment 1-3, GC/MS analyzes glucosides derivatization product; B: embodiment 2; C: embodiment 3).
Five, embodiment
Embodiment 1:
1, take flue-cured tobacco offal sample 1g and put into container, add 20mL methyl alcohol, ultrasonic extraction 60min under ultrasonic power 350W and ultrasonic frequency 70kHz, after getting supernatant liquid filtering, evaporated under reduced pressure solvent obtains tobacco glucosides crude extract.
2, tobacco glucosides crude extract step 1 obtained is dissolved in 10mL deionized water, be added on solid-phase extraction column that Amberlite XAD-2 is filler, solid-phase extraction column is slow transitted through with 0.5mL/min, use 20mL ultrapure water, 15mL n-pentane/methylene chloride (2/1, v/v) wash-out more successively, elution speed is no more than 1.0mL/min, finally use 20mL methanol-eluted fractions, elution speed is 2.0mL/min, collects meoh eluate, is concentrated into and does tobacco glucosides extract.
3, in tobacco glucosides extract, inner mark solution 1mL (methanol solution of 2-nitrobenzene-β-D-Glucose glycosides, concentration 1.0mg/mL) is added, N
2dry up, add 400 μ L methylene chloride and 400 μ L acetic anhydride, after sealing, 50 DEG C of water-bath derivatization 60min, are cooled to room temperature, obtain tobacco glucosides derivatization product.
4, Gc-ms is carried out to the tobacco glucosides derivatization product that step 3 obtains:
Chromatographic condition: chromatographic column is DB-5MS post (30m*0.25mm*0.25 μm), temperature programme, initial temperature 120 DEG C, keeps 1min, rises to 220 DEG C, then rise to 280 DEG C with 5 DEG C/min with 3 DEG C/min, keeps 10min.Sample size 1.0 μ L, split ratio 10:1, injector temperature 240 DEG C.
Mass Spectrometry Conditions: ion source temperature 230 DEG C, level Four bar temperature 150 DEG C, Ionization mode EI, electron energy 70eV, scan pattern is full scan, mass range 40-600amu, and chromatogram as shown in Figure 1.Aglycon adopts standard substance and NIST to compose storehouse according to qualitative, quantitatively adopts and calculates (assuming that response coefficient is equal) with the derivatization product area ratio of the interior 2-of marking nitrobenzene-β-D-Glucose glycosides.Relative retention time and the mass spectrometric fragment ion of each compound are as shown in table 1.
The relative retention time of table 1 tobacco glucosides derivatization product and ms fragment
Embodiment 2:
Take Turkish tobaccos offal sample 1g and put into container, add 40mL ethanol, extract 60min in 200r/min concussion, after getting supernatant liquid filtering, evaporated under reduced pressure solvent obtains tobacco glucosides crude extract.
Just glucosides crude extract is dissolved in 10mL deionized water, be added on solid-phase extraction column that D101 is filler, pillar is slow transitted through with 0.5mL/min, use 20mL ultrapure water, 15mL n-pentane/methylene chloride (2/1, v/v) wash-out successively, elution speed is no more than 1.0mL/min, finally use 20mL methanol-eluted fractions, elution speed is 2.0mL/min, collects meoh eluate, is concentrated into and does tobacco glucosides extract.
Inner mark solution 1mL (2-nitrobenzene-β-D-Glucose glycosides, 1.0mg/mL methanol solution) is added, N in glucosides extract
2dry up, add 400 μ L acetone and 400 μ L N-methyl-two (trifluoroacetamide), after sealing, 60 DEG C of water-bath derivatization 60min, are cooled to room temperature, obtain tobacco glucosides derivatization product.
Gc-ms is carried out to tobacco glucosides derivatization product:
Chromatographic condition: chromatographic column is DB-5MS post (30m*0.25mm*0.25 μm), temperature programme, initial temperature 120 DEG C, keeps 1min, rises to 220 DEG C, then rise to 280 DEG C with 5 DEG C/min with 3 DEG C/min, keeps 10min.Sample size 1.0 μ L, split ratio 10:1, injector temperature 240 DEG C.
Mass Spectrometry Conditions: ion source temperature 230 DEG C, level Four bar temperature 150 DEG C, Ionization mode EI, electron energy 70eV, scan pattern is full scan, mass range 40-600amu.Aglycon adopts standard substance and NIST to compose storehouse according to qualitative, quantitatively adopts and calculates (assuming that response coefficient is equal) with the derivatization product area ratio of the interior 2-of marking nitrobenzene-β-D-Glucose glycosides.
Embodiment 3:
Take burley tobaccos offal sample 1g and put into container, add 50mL ethyl acetate, surname extraction 50min, after getting supernatant liquid filtering, evaporated under reduced pressure solvent obtains tobacco glucosides crude extract.
Just glucosides crude extract is dissolved in 10mL deionized water, be added on solid-phase extraction column that HP-20 is filler, pillar is slow transitted through with 0.5mL/min, use 20mL ultrapure water, 15mL n-pentane/methylene chloride (2/1, v/v) wash-out successively, elution speed is no more than 1.0mL/min, finally use 20mL methanol-eluted fractions, elution speed is 2.0mL/min, collects meoh eluate, is concentrated into and does tobacco glucosides extract.
Inner mark solution 1mL (2-nitrobenzene-β-D-Glucose glycosides, 1.0mg/mL methanol solution) is added, N in glucosides extract
2dry up, add 400 μ L acetone and 400 μ L trifluoroacetic anhydride, after sealing, 80 DEG C of water-bath derivatization 60min, are cooled to room temperature, obtain tobacco glucosides derivatization product.
Gc-ms is carried out to tobacco glucosides derivatization product:
Chromatographic condition: chromatographic column is DB-5MS post (30m*0.25mm*0.25 μm), temperature programme, initial temperature 120 DEG C, keeps 1min, rises to 220 DEG C, then rise to 280 DEG C with 5 DEG C/min with 3 DEG C/min, keeps 10min.Sample size 1.0 μ L, split ratio 10:1, injector temperature 240 DEG C.
Mass Spectrometry Conditions: ion source temperature 230 DEG C, level Four bar temperature 150 DEG C, Ionization mode EI, electron energy 70eV, scan pattern is full scan, mass range 40-600amu.Aglycon adopts standard substance and NIST to compose storehouse according to qualitative, quantitatively adopts and calculates (assuming that response coefficient is equal) with the derivatization product area ratio of the interior 2-of marking nitrobenzene-β-D-Glucose glycosides.
This detects data only for above-mentioned detection sample.
The above; be only the present invention's preferably embodiment; but protection scope of the present invention is not limited thereto; anyly be familiar with those skilled in the art in the technical scope that the present invention discloses; be equal to according to technical scheme of the present invention and inventive concept thereof and replace or change, all should be encompassed within protection scope of the present invention.
Claims (7)
1. an assay method growing tobacco middle glycoside link state flavor component, is characterized in that comprising the following steps:
(1) extract: cross 40 mesh sieves after drying tobacco being pulverized and obtain offal, take 1g offal and put into container, add 20-50mL Extraction solvent, extract glycosidic bond and state flavor component, after getting supernatant liquid filtering, evaporated under reduced pressure solvent obtains tobacco glucosides crude extract;
(2) separation and purification: tobacco glucosides crude extract step (1) obtained is dissolved in 10mL deionized water, is added on solid-phase extraction column, passes through solid-phase extraction column with the flow velocity of 0.5mL/min; Use 20mL ultrapure water, 15mL n-pentane/methylene chloride (volume ratio 2:1) wash-out more successively, elution speed≤1.0mL/min; Finally use 20mL methanol-eluted fractions, elution speed is 2.0mL/min, collects meoh eluate, is concentrated into and dryly obtains tobacco glucosides extract;
(3) derivatization: add inner mark solution 1mL, N in the tobacco glucosides extract that step (2) obtains
2dry up, add 400 μ L derivatization solvents and 400 μ L acylating reagents, in 50-80 DEG C of water-bath derivative reaction 60min after sealing, be cooled to room temperature, obtain tobacco glucosides derivatization product.
(4) analyze: Gc-ms is carried out to tobacco glucosides derivatization product.
2. assay method according to claim 1, is characterized in that:
Described tobacco comprises flue-cured tobacco, burley tobaccos or Turkish tobaccos.
3. assay method according to claim 1, is characterized in that:
Described in step (1), Extraction solvent comprises water, methyl alcohol, ethanol, ethyl acetate or acetone.
4. assay method according to claim 1, is characterized in that:
In step (1), extraction glycosidic bond and state flavor component adopt ultrasonic extraction, concussion extraction or surname extraction.
5. assay method according to claim 1, is characterized in that:
The filler of described solid-phase extraction column is Amberlite XAD-2, D101 or HP-20.
6. assay method according to claim 1, is characterized in that:
Inner mark solution described in step (3) is the methanol solution of 2-nitrobenzene-β-D-Glucose glycosides, concentration 1.0mg/mL; Described derivatization solvent is methylene chloride, acetone or pyridine; Described acylating reagent is acetic anhydride, N-methyl-two (trifluoroacetamide), trifluoroacetic anhydride, PFPA or heptafluorobutyric anhydride.
7. assay method according to claim 1, is characterized in that:
In step (4), the optimum configurations of Gc-ms is as follows:
Chromatographic condition: chromatographic column is DB-5MS post, temperature programme, initial temperature 120 DEG C, keeps 1min, rises to 220 DEG C, then rise to 280 DEG C with 5 DEG C/min with 3 DEG C/min, keeps 10min; Sample size 1.0 μ L, split ratio 10:1, injector temperature 240 DEG C;
Mass Spectrometry Conditions: ion source temperature 230 DEG C, level Four bar temperature 150 DEG C, Ionization mode EI, electron energy 70eV, scan pattern is full scan, mass range 40-600amu.
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| CN111175420A (en) * | 2020-03-18 | 2020-05-19 | 福建中烟工业有限责任公司 | Separation and analysis method for aroma components in tobacco leaves |
| CN111208239A (en) * | 2020-02-25 | 2020-05-29 | 浙江工业大学 | Impurity removal and purification method of bonded-state aroma substance |
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| CN114806712A (en) * | 2022-04-18 | 2022-07-29 | 湖北中烟工业有限责任公司 | Fruity latent aroma extract for cigarettes as well as preparation method and application thereof |
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| CN108095187A (en) * | 2017-11-24 | 2018-06-01 | 云南中烟工业有限责任公司 | A kind of enrichment method of tobacco glucosides |
| CN107927283A (en) * | 2017-12-12 | 2018-04-20 | 陕西理工大学 | A kind of method using SPE pillars extraction millet paste aroma substance |
| CN109521124A (en) * | 2019-01-23 | 2019-03-26 | 邯郸学院 | The gas chromatography-mass spectrum detection method of demethyl coclaurine in a variety of matrix samples |
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| 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 |
| CN111208239A (en) * | 2020-02-25 | 2020-05-29 | 浙江工业大学 | Impurity removal and purification method of bonded-state aroma substance |
| WO2021169929A1 (en) * | 2020-02-25 | 2021-09-02 | 浙江工业大学 | Impurity removal and purification method for bonded state aromatic substance |
| CN111398438A (en) * | 2020-03-06 | 2020-07-10 | 浙江工业大学 | Method for promoting release of bonded aroma substances in fruit juice |
| CN111175420A (en) * | 2020-03-18 | 2020-05-19 | 福建中烟工业有限责任公司 | Separation and analysis method for aroma components in tobacco leaves |
| CN112394129A (en) * | 2020-11-25 | 2021-02-23 | 江苏中烟工业有限责任公司 | Chemical component analysis pretreatment method of extract essence perfume |
| CN114806712A (en) * | 2022-04-18 | 2022-07-29 | 湖北中烟工业有限责任公司 | Fruity latent aroma extract for cigarettes as well as preparation method and application thereof |
| CN114806712B (en) * | 2022-04-18 | 2023-05-09 | 湖北中烟工业有限责任公司 | Fruit-aroma-containing and diving-aroma extract for cigarettes as well as preparation method and application thereof |
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