CN104351444A - Method for selecting and collecting aroma components in green tea leaves and aroma components prepared according to method - Google Patents
Method for selecting and collecting aroma components in green tea leaves and aroma components prepared according to method Download PDFInfo
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- CN104351444A CN104351444A CN201410565048.7A CN201410565048A CN104351444A CN 104351444 A CN104351444 A CN 104351444A CN 201410565048 A CN201410565048 A CN 201410565048A CN 104351444 A CN104351444 A CN 104351444A
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Abstract
The invention relates to a method for selecting and collecting aroma components in green tea leaves. The method comprises the following steps: 1) putting the green tea leaves into a heating container, adding water, heating to collect tea aroma, guiding the tea aroma into a liquid nitrogen-containing collecting bottle, and stopping heating after a tea soup is slightly boiled; pouring the tea soup into the collecting bottle, and combing the tea soup in a round-bottom flask and the aroma components in the collecting bottle so as to obtain green tea water before being applied to a solid phase extraction column; 2) taking the green tea water, diluting the green tea water by using deionized water according to a certain dilution ratio, applying the green tea water onto the LiChrolutEN solid phase extraction column, and eluting the solid phase extraction column by using ultrapure water; vacuumizing the solid phase extraction column, and eluting volatile components in the solid phase extraction column by using dichloromethane; concentrating and drying dichloromethane eluent to obtain final green tea essential oil. By the method, the extracted aroma components are free of solvent residue and special smell, fresh and strong in aroma and higher in extraction rate.
Description
Technical field
The invention belongs to active skull cap components extractive technique field, particularly relate to flavor matter prepared by the method for aroma component in a kind of selection green tea and the method.
Background technology
Tea tree Camellia dicotyledon, about 30 belong to, and 500 kinds, are distributed in subtropical and tropical zones.There are 14 genus in China, 397 kinds, various places on the south main product the Changjiang river, and wherein Camellia Camellia and what Pterostyrax Schima etc. are all rich in economic worth.As the tealeaves of one of the large beverage in the world three, being not only excellent health drink, is also a kind of good Chinese medicine; Wherein, the tealeaves of azymous tea (degree of fermentation is zero) is called green tea, containing 300 number of chemical compositions in explored green tea, as tea polyphenols, amino acid, caffeine, vitamin, pectin element, organic acid, lipopolysaccharides, protein, aromatic compound, mineral matter, carbohydrate, enzyme, pigment etc., can play heatstroke prevention disappear cotton-padded mattress, refresh oneself, nourishing the stomach, anti-cancer, fat-reducing, the function such as fitness.
In addition to water, in green tea water, principle active component is that a large amount of involatile substance is as tea polyphenols, carbohydrate, pigment, amino acid, caffeine, vitamin etc.Generally speaking, the total content of aroma substance is no more than 2% of tea body, contains nearly more than 600 kinds of aroma substances in the aroma component of green tea research data display, and the distribution of these Aromatic Matter Contents is not from ng/L level to g/L level etc.In the aroma substance composition of these trace, 99% is alcohol common in green tea water, acid and Ester, and remaining 1% component determining tea aroma feature is made up of at the aroma substance of μ g/L or even ng/L nearly hundred kinds of content.These have the trace of the significant contribution even selective collection of trace aroma substance to be parts the most difficult in current Tea Samples pretreatment technology to green tea water characteristic perfume.
At present, common tea aroma collecting material method comprises liquid-liquid extraction, SPE, head-space sampling, SPME, Stir Bar Sorptive Extraction etc.In the comparative studies of these methods, can find out that it respectively has pluses and minuses.Liquid-liquid extraction is most popular abstraction technique in fragrance research, and it has, and treating capacity is large, the advantage various, cycles of concentration is higher selected by solvent, is used for the qualitative analysis of tea aroma compound; Due to liquid-liquid extraction workload greatly, the shortcoming such as the many and dosing accuracy of organic solvent use amount is poor, be badly in need of technology that is more convenient, safe, the fragrance of extraction collection efficiently at present.Head-space sampling, SPME and Stir Bar Sorptive Extraction have simple to operate, fast, solvent-free, the feature that is easy to automation mechanized operation, be suitable for the quantitative analysis of a large amount of sample, but due to the selective preference difference of sorbing material, easily cause the loss of some type aroma substance, these methods are difficult to realize comprehensive extraction of tea aroma material, enrichment.SPE is current the most widely used Sample Pretreatment Technique, is widely used in the analysis of the field samples such as food, medicine, tobacco, environment.SPE has flexible operation, sorbing material wide variety, and solvent use amount is few, and cycles of concentration high is particularly suitable for separation, the enrichment of tealeaves class trace and the important volatile compound of trace.Due to the complexity of green tea water aroma component kind, character, the levels span of volatile compound is large, does not also have a kind of pre-treating method meeting all demands at present, and disposable completing concentrates the enrichment of all aroma substances.
Summary of the invention
In order to solve above-mentioned technical problem, the first object of the present invention is to provide method and the method for aroma component in a kind of selection green tea.The second object of the present invention is to provide flavor matter prepared by above-mentioned method.Method of the present invention, be more suitable for extracting the few and aroma substance composition that the levels span of volatile compound is large of composition in tealeaves, no solvent residue in the flavor matter of extraction, without specific peculiar smell, fragrance is fresh, strong, and recovery rate is higher.
In order to realize first above-mentioned object, present invention employs following technical scheme:
A method for aroma component in selection green tea, the method comprises the following steps:
1) be placed in by green tea and add container, add water, it is fragrant that tea is collected in heating, imports in the receiving flask containing liquid nitrogen by tea perfume, millet paste through 1 ~ 10min is micro-boil after stop heating; Getting a certain amount of millet paste pours in receiving flask, merges the millet paste in round-bottomed flask and the green tea aroma component in receiving flask, obtains the green tea water before solid-phase extraction column;
2) get green tea water, with deionized water according to loading LiChrolut EN solid-phase extraction column after the dilution of certain extension rate, in control procedure, loading flow velocity is not higher than 5.0 mL/min, with ultra-pure water wash-out solid-phase extraction column after completion of the sample; Solid-phase extraction column is taken out under vacuum the volatile component in rear dichloromethane eluent extraction column; Dichloromethane eluant concentrates after drying, is final green tea tea essential oil.
As preferably, bright front green tea selected by described green tea.
As preferably, in described step 1), green tea carries out pre-treatment: take a certain amount of dry green tea, is placed in 45 DEG C of vacuum drying chambers and is dried to close to over dry, then vacuum drying chamber temperature is adjusted to 105 DEG C and dries to constant weight, and pulverizes, after sieving, for subsequent use.
As preferably, after described green tea sieves, granularity is 40 ~ 80 orders.
As preferably, in described step 1), the solid-liquid ratio of green tea and water is selected at 1:10 ~ 1:30.
As preferably, in described step 1), micro-time of boiling is 2 ~ 6min.
As preferably, described step 2) in first adopt with 20 mL carrene respectively before LiChrolut EN solid-phase extraction column loading, 20 mL methyl alcohol and 30mL ultra-pure water carry out activation process.
As preferably, described step 2) in loading extension rate be 1 ~ 5 times.
As preferably, described step 2) in loading flow velocity be 1.0 ~ 3.0 mL/min.
In order to realize second above-mentioned object, present invention employs following technical scheme:
Flavor matter in the green tea that method described in above-mentioned any one technical scheme prepares.
Because tealeaves does not belong to aromatics plant, the aroma substance composition contained by it is few and the levels span of volatile compound is large, extracts tea fragrant raw material fragrance very challenging.The present invention adopts the selective absorption of LiChrolut EN resin, good suction-operated is had for volatile compound, and to content in sample abundanter the adsorption effect such as tea polyphenols, carbohydrate, pigment, amino acid, caffeine, vitamin poor, technical process can reduce the loss of target aroma component as far as possible, finally obtains the fragrant extract of natural tea.Finished product green tea tea essential oil no solvent residue, without specific peculiar smell, fragrance is fresh, strong, and recovery rate is higher.The recovery rate that the present invention measures the bright front green tea tea essential oil of gained can reach 8.26%, in DPPH free radical system, the IC of bright front green tea tea essential oil
50be 51.23 μ g/mL.
Detailed description of the invention
Below provide embodiment, the invention will be further described.
embodiment 1
A method for aroma component in selection green tea, the method comprises the following steps:
(1) filling of SPE: load Merck KGaA Millipore Corp. LiChrolut EN(1000 mg tea perfume to good adsorption function voluntarily) solid-phase extraction column;
(2) activation process of LiChrolut EN solid-phase extraction column: first adopt 20 mL carrene respectively before loading, 20 mL methyl alcohol and 30mL ultra-pure water carry out activation process
(3) bright front green tea (producing region, Zhejiang) pre-treatment: take the bright front green tea of a certain amount of drying, being placed in 45 DEG C of vacuum drying chambers is dried to close to over dry, then vacuum drying chamber temperature is adjusted to 105 DEG C to dry to constant weight, and after sieving by the requirement of certain bright front green tea granularity selection respectively, for subsequent use;
(4) preparation of tea: accurately take the bright front green tea of 60 object, be placed on and be enclosed within 1000 mL round-bottomed flasks of electric jacket, feed liquid ratio according to 1:20 adds boiling water, import fragrant for the tea of discharging in round-bottomed flask in the receiving flask containing liquid nitrogen with glass tube, millet paste removes round-bottomed flask device after 4min micro-time of boiling; Getting a certain amount of millet paste pours in receiving flask, merges the millet paste in round-bottomed flask and the green tea aroma component in receiving flask, obtains the bright front green tea water before solid-phase extraction column;
(5) loading: get a certain amount of bright front green tea water, with deionized water according to loading LiChrolut EN solid-phase extraction column after the extension rate dilution of 2 times, in control procedure, loading flow velocity is 2.0 mL/min, with the material such as bright front green tea water, pigment, sugar residual in 50mL ultra-pure water wash-out solid-phase extraction column after completion of the sample.The volatile component in 20mL dichloromethane eluent extraction column is used after solid-phase extraction column being drained under vacuum is 0.1MPa 10 min; Dichloromethane eluant nitrogen after anhydrous sodium sulfate drying blows and is concentrated into 0.5mL, is final bright front green tea tea essential oil.
The recovery rate measuring gained bright front green tea tea essential oil is 8.26%, in DPPH free radical system, the IC of bright front green tea tea essential oil
50be 51.23 μ g/mL.
embodiment 2
A method for aroma component in selection green tea, the method comprises the following steps:
(1) filling of SPE: load Merck KGaA Millipore Corp. LiChrolut EN(1000 mg tea perfume to good adsorption function voluntarily) solid-phase extraction column;
(2) activation process of LiChrolut EN solid-phase extraction column: first adopt with 20 mL carrene respectively before loading, 20 mL methyl alcohol and 30mL ultra-pure water carry out activation process
(3) bright front green tea (producing region, Zhejiang) pre-treatment: take the bright front green tea of a certain amount of drying, being placed in 45 DEG C of vacuum drying chambers is dried to close to over dry, then vacuum drying chamber temperature is adjusted to 105 DEG C to dry to constant weight, and after sieving by the requirement of certain bright front green tea granularity selection respectively, for subsequent use;
(4) preparation of tea: accurately take the bright front green tea of 40 object, be placed on and be enclosed within 1000 mL round-bottomed flasks of electric jacket, feed liquid ratio according to 1:10 adds boiling water, import fragrant for the tea of discharging in round-bottomed flask in the receiving flask containing liquid nitrogen with glass tube, millet paste removes round-bottomed flask device after 6min micro-time of boiling; Getting a certain amount of millet paste pours in receiving flask, merges the millet paste in round-bottomed flask and the green tea aroma component in receiving flask, obtains the bright front green tea water before solid-phase extraction column;
(5) loading: get a certain amount of bright front green tea water, with deionized water according to loading LiChrolut EN solid-phase extraction column after the extension rate dilution of 5 times, in control procedure, loading flow velocity is 3.0 mL/min, with the material such as bright front green tea water, pigment, sugar residual in 50mL ultra-pure water wash-out solid-phase extraction column after completion of the sample.The volatile component in 20mL dichloromethane eluent extraction column is used after solid-phase extraction column being drained under vacuum is 0.1MPa 10 min; Dichloromethane eluant nitrogen after anhydrous sodium sulfate drying blows and is concentrated into 0.5mL, is final bright front green tea tea essential oil.
The recovery rate measuring gained bright front green tea tea essential oil is 7.76%, in DPPH free radical system, the IC of bright front green tea tea essential oil
50be 52.05 μ g/mL.
embodiment 3
A method for aroma component in selection green tea, the method comprises the following steps:
(1) filling of SPE: load Merck KGaA Millipore Corp. LiChrolut EN(1000 mg tea perfume to good adsorption function voluntarily) solid-phase extraction column;
(2) activation process of LiChrolut EN solid-phase extraction column: first adopt with 20 mL carrene respectively before loading, 20 mL methyl alcohol and 30mL ultra-pure water carry out activation process
(3) bright front green tea (producing region, Zhejiang) pre-treatment: take the bright front green tea of a certain amount of drying, being placed in 45 DEG C of vacuum drying chambers is dried to close to over dry, then vacuum drying chamber temperature is adjusted to 105 DEG C to dry to constant weight, and after sieving by the requirement of certain bright front green tea granularity selection respectively, for subsequent use;
(4) preparation of tea: accurately take the bright front green tea of 80 object, be placed on and be enclosed within 1000 mL round-bottomed flasks of electric jacket, feed liquid ratio according to 1:30 adds boiling water, import fragrant for the tea of discharging in round-bottomed flask in the receiving flask containing liquid nitrogen with glass tube, millet paste removes round-bottomed flask device after 2min micro-time of boiling; Getting a certain amount of millet paste pours in receiving flask, merges the millet paste in round-bottomed flask and the green tea aroma component in receiving flask, obtains the bright front green tea water before solid-phase extraction column;
(5) loading: get a certain amount of bright front green tea water, with deionized water according to loading LiChrolut EN solid-phase extraction column after the extension rate dilution of 3 times, in control procedure, loading flow velocity is 1.0 mL/min, with the material such as bright front green tea water, pigment, sugar residual in 50mL ultra-pure water wash-out solid-phase extraction column after completion of the sample.The volatile component in 20mL dichloromethane eluent extraction column is used after solid-phase extraction column being drained under vacuum is 0.1MPa 10 min; Dichloromethane eluant nitrogen after anhydrous sodium sulfate drying blows and is concentrated into 0.5mL, is final bright front green tea tea essential oil.
The recovery rate measuring gained bright front green tea tea essential oil is 7.88%, in DPPH free radical system, the IC of bright front green tea tea essential oil
50be 52.38 μ g/mL.
embodiment 4
A method for aroma component in selection green tea, the method comprises the following steps:
(1) filling of SPE: load Merck KGaA Millipore Corp. LiChrolut EN(1000 mg tea perfume to good adsorption function voluntarily) solid-phase extraction column;
(2) activation process of LiChrolut EN solid-phase extraction column: first adopt with 20 mL carrene respectively before loading, 20 mL methyl alcohol and 30mL ultra-pure water carry out activation process
(3) bright front green tea (producing region, Zhejiang) pre-treatment: take the bright front green tea of a certain amount of drying, being placed in 45 DEG C of vacuum drying chambers is dried to close to over dry, then vacuum drying chamber temperature is adjusted to 105 DEG C to dry to constant weight, and after sieving by the requirement of certain bright front green tea granularity selection respectively, for subsequent use;
(4) preparation of tea: accurately take the bright front green tea of 60 object, be placed on and be enclosed within 1000 mL round-bottomed flasks of electric jacket, feed liquid ratio according to 1:20 adds boiling water, import fragrant for the tea of discharging in round-bottomed flask in the receiving flask containing liquid nitrogen with glass tube, millet paste removes round-bottomed flask device after 2min micro-time of boiling; Getting a certain amount of millet paste pours in receiving flask, merges the millet paste in round-bottomed flask and the green tea aroma component in receiving flask, obtains the bright front green tea water before solid-phase extraction column;
(5) loading: get a certain amount of bright front green tea water, with deionized water according to loading LiChrolut EN solid-phase extraction column after the extension rate dilution of 2 times, in control procedure, loading flow velocity is 3.0 mL/min, with the material such as bright front green tea water, pigment, sugar residual in 50mL ultra-pure water wash-out solid-phase extraction column after completion of the sample.The volatile component in 20mL dichloromethane eluent extraction column is used after solid-phase extraction column being drained under vacuum is 0.1MPa 10 min; Dichloromethane eluant nitrogen after anhydrous sodium sulfate drying blows and is concentrated into 0.5mL, is final bright front green tea tea essential oil.
The recovery rate measuring gained bright front green tea tea essential oil is 8.17%, in DPPH free radical system, the IC of bright front green tea tea essential oil
50be 55.02 μ g/mL.
Claims (10)
1. the method for aroma component in selection green tea, is characterized in that the method comprises the following steps:
1) be placed in by green tea and add container, add water, it is fragrant that tea is collected in heating, imports in the receiving flask containing liquid nitrogen by tea perfume, millet paste through 1 ~ 10min is micro-boil after stop heating; Getting a certain amount of millet paste pours in receiving flask, merges the millet paste in round-bottomed flask and the green tea aroma component in receiving flask, obtains the green tea water before solid-phase extraction column;
2) get green tea water, with deionized water according to loading LiChrolut EN solid-phase extraction column after the dilution of certain extension rate, in control procedure, loading flow velocity is not higher than 5.0 mL/min, with ultra-pure water wash-out solid-phase extraction column after completion of the sample; Solid-phase extraction column is taken out under vacuum the volatile component in rear dichloromethane eluent extraction column; Dichloromethane eluant concentrates after drying, is final green tea tea essential oil.
2. the method for aroma component in a kind of selection green tea according to claim 1, is characterized in that: bright front green tea selected by green tea.
3. the method for aroma component in a kind of selection green tea according to claim 1 and 2, it is characterized in that: in step 1), green tea carries out pre-treatment: take a certain amount of dry green tea, being placed in 45 DEG C of vacuum drying chambers is dried to close to over dry, then vacuum drying chamber temperature is adjusted to 105 DEG C to dry to constant weight, pulverize, after sieving, for subsequent use.
4. the method for aroma component in a kind of selection green tea according to claim 3, is characterized in that: after green tea sieves, granularity is 40 ~ 80 orders.
5. the method for aroma component in a kind of selection green tea according to claim 1 and 2, is characterized in that: in step 1), the solid-liquid ratio of green tea and water is selected at 1:10 ~ 1:30.
6. the method for aroma component in a kind of selection green tea according to claim 1 and 2, is characterized in that: in step 1), micro-time of boiling is 2 ~ 6min.
7. the method for aroma component in a kind of selection green tea according to claim 1, it is characterized in that: step 2) in first adopt with 20 mL carrene respectively before LiChrolut EN solid-phase extraction column loading, 20 mL methyl alcohol and 30mL ultra-pure water carry out activation process.
8. in a kind of selection green tea according to claim 1 or 7, the method for aroma component, is characterized in that: step 2) in loading extension rate be 1 ~ 5 times.
9. in a kind of selection green tea according to claim 1 or 7, the method for aroma component, is characterized in that: step 2) in loading flow velocity be 1.0 ~ 3.0 mL/min.
10. the flavor matter in the green tea that the method described in claim 1 ~ 9 any one claim prepares.
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| 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 |
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| CN104849387A (en) * | 2015-05-22 | 2015-08-19 | 福建中烟工业有限责任公司 | Tea brewing fragrance substance detection method, tea cover cup fragrance collecting method and tea cover cup fragrance collecting device |
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