CN101182303A - Method for preparing high-purity beta-carotene from green tea - Google Patents
Method for preparing high-purity beta-carotene from green tea Download PDFInfo
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- CN101182303A CN101182303A CNA2007101644877A CN200710164487A CN101182303A CN 101182303 A CN101182303 A CN 101182303A CN A2007101644877 A CNA2007101644877 A CN A2007101644877A CN 200710164487 A CN200710164487 A CN 200710164487A CN 101182303 A CN101182303 A CN 101182303A
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Abstract
A method of preparing for high-purity beta-carotene from green tea comprises the main content as follows: crushed green tea powder is extracted by the mixed liquid of methanol, ethanol and H2O or at least one solvent thereof; tea-leaf after the extraction is decompressed and dried, and one kind of a plurality of kinds of ethyl acetate, acetone, n-hexane, isohexane, dichloromethane and chloroform are used as extracting solution to extract the crude liquid extract of the beta-carotene; the crude liquid extract after concentration is processed for the gradient elution chromatography by silica gel or alumina column chromatogram, and elution liquid which is used is two kinds of the ethyl acetate, the acetone, the n-hexane, the isohexane, cyclohexane, the dichloromethane and the chloroform. Effluent liquid is collected by parts for vacuum freezing and drying to obtain the high-purity beta-carotene of the green tea. The present invention is applicable to the common green tea and especially the low-grade green tea used as the raw material and has the characteristics of the simple technical process and required equipments, the high extraction of the beta-carotene from the green tea, the high purity of the beta-carotene etc.
Description
Technical field
The invention belongs to the green tea deep process technology, relate to a kind of method of from green tea, extracting the purifying β-Hu Luobusu.
Background technology
There has been history of more than one thousand years as the drink that a kind of special favor and nutrient health-care function have concurrently in tealeaves in China, is the agricultural-food of important cash crop of China and foreign exchange earning.The our times Tea Industry faces the tea yield rate of growth greater than contradictions such as consumption, tealeaves (particularly large green tea) export price drops, the tradition Tea Industry industrial structure is contained to be adjusted, by tealeaves deep processing and comprehensive utilization, realize the tea products diversification, improve the Sustainable development that interrelationship between industries can promote China's tea industry.The extraction of functional component and utilization are the important channels of tea resources comprehensive utilization in the deep processing field of tea, mainly concentrate on materials such as tea-polyphenol, theanine, theoflavin and tea polysaccharide at present, and the extraction purifying of carotenoid material and utilization do not relate to.
(β-carotene) is a kind of fat-soluble carotenoid that extensively is present in the plant to β-Hu Luobusu, belong to the tetraterpenes compound, closely related with HUMAN HEALTH, have functions such as very high pharmaceutical use such as anticancer, anti-oxidant, radioprotective, strengthening immunity, and be the vitamin V of needed by human
AImportant source.Content beta-carotene in the Chen Zongmao report tealeaves can reach 600mg/kg, the superfine content beta-carotene difference of having summed up several main plant of having reported of Wang Xin, and tealeaves is listed as the 3rd, is only second to matrimony vine and clover, is four times of Radix Dauci Sativae approximately.But matrimony vine and clover scarcity of resources, raw materials cost is too high as extracting.The content beta-carotene of tea tree different sites blade, Various Seasonal tealeaves has been measured in the superfine systems analysis of Wang Xin, discover spring, summer and autumn tea tree the content beta-carotene at two leaves and a bud position (being generally the harvesting position of Green Tea Processing raw material) be respectively 44.3,127.1 and 403.5mg/kg, and spring tea tree the content beta-carotene of 3,4,5 blades can reach 600.5338.7 and 337.6 respectively.Famous green tea, medium-to-high grade green tea usually with the two leaves and a bud of tea tree as raw material, pluck spring, to produce the spring tea of high-quality local flavor.And surplus slightly leaf of the tea of a large amount of spring tea and summer autumn tea leaf are underutilized, and small part is processed as low-grade green tea and sells cheap, and summer autumn tea peasant is unwilling to pluck, and causes the large number of biological wasting of resources.China's tealeaves cultivated area the first in the world is green tea production, consumption big country and big trading nation, and large green tea export price in recent years constantly drops, and increases the comprehensive Utilization Ways of tea resources, and is of far-reaching significance for the Sustainable development and the establishment conservation-minded society of agricultural.
Summary of the invention
The present invention seeks to provide a kind of and particularly from low-grade green teas such as surplus slightly leaf of the tea of spring tea and summer autumn tea leaf, extract the purifying β-Hu Luobusu (method of β-carotene) from green tea.
The technical solution used in the present invention is as comprising the steps:
(1) tealeaves pre-treatment:
Select unmetamorphosed green tea (low-grade green tea is better) for use, at room temperature through mechanical disintegration to 100-300 purpose pressed powder, green tea powder is with methyl alcohol, ethanol and H
20 mixed solution or wherein at least a solution extracted 0.5-12.0 hour under 18-35 ℃ of condition, and stirring (mixing speed: 100-400r/min), leave standstill, filter, the filter residue drying under reduced pressure, the mass volume ratio (g/ml) of green tea powder and said extracted liquid is 1: 2-1: 30.
(2) green tea β-Hu Luobusu crude extract preparation:
Filter residue from step (1) extracted 0.5-24.0 hour under 15-50 ℃ of condition with extracting solution, and stirring (mixing speed: 100-400r/min), leave standstill, filter, the filtrate lyophilize is concentrated into the 1/5-2/3 of original volume, obtains green tea β-Hu Luobusu crude extract.Described extracting solution is that in ethyl acetate, acetone, normal hexane, isohexane, methylene dichloride and the trichloromethane one or more are mixed in proportion.The mass volume ratio of tea-leaf power and extracting solution (g/ml) is 1: 2-1: 35.
(3) purifying of green tea β-Hu Luobusu preparation:
Column chromatography is carried out gradient elution from step (2) the gained green tea β-Hu Luobusu crude extract, fraction collection, vacuum lyophilization, high purity green tea β-Hu Luobusu.The column chromatography used medium is silica gel or aluminum oxide.Used elutriant is two kinds in ethyl acetate, acetone, normal hexane, isohexane, hexanaphthene, methylene dichloride and the trichloromethane, and its concentration gradient ratio is changed to 1: 9-5: 5 (volume ratios).Elution flow rate is 0.3-55.0ml/min.
The present invention has significant beneficial effect:
Technical process and required equipment are simple, and raw material employing low-grade green tea, and low production cost is to β-Hu Luobusu extraction yield height in the tealeaves and purity height.Show the β-Hu Luobusu goods chromatographic peak more single (seeing Fig. 1 and 2) that the present invention obtained by standard substance comparison with certain external famous reagent company.From green tea the preparation β-Hu Luobusu obtain goods purity high and with green tea as raw material, its content beta-carotene height, the relevant interference substances content is less and extraction process etc. is relevant.Significance of the present invention be to make tea resources particularly low-grade green tea obtain utilizing more fully, expanded the development and utilization prospect of natural product in the green tea.
Description of drawings
Fig. 1 contrasts the β-Hu Luobusu standard substance HPLC collection of illustrative plates (waters HPLC) of company;
The β-Hu Luobusu HPLC collection of illustrative plates (waters HPLC) that Fig. 2 the present invention is prepared.
Embodiment
Embodiment 1:
(1) gets the low-grade green tea sheet that gather and process summer in Zhejiang Hangzhou tealeaves producing region, at room temperature through mechanical disintegration to 200 order.Green tea powder extracted 5.0 hours and stirred (mixing speed: 150r/min) under 25 ℃ of conditions with 60% aqueous ethanolic solution (g/ml, 1: 10).Leave standstill, filter the filter residue drying under reduced pressure;
(2) filter residue in the step (1) extracted 6 hours under 28 ℃ of conditions with normal hexane (g/ml, 1: 12), and stir (mixing speed: 200r/min), leave standstill, filtration, the filtrate lyophilize is concentrated into 1/3 of original volume, obtains green tea β-Hu Luobusu crude extract;
(3) silica gel column chromatography on step (2) the gained green tea β-Hu Luobusu crude extract, elutriant is ethyl acetate and normal hexane, gradient is in proper order: 1.0: 9.0; 2.0: 8.0; 3.0: 7.0; 3.5: 6.5 (ethyl acetate: normal hexane, V: V), flow velocity is 15ml/min, and the effluent liquid fraction collection detects, and merges, and vacuum lyophilization obtains highly purified green tea β-Hu Luobusu.HPLC analysis revealed, prepared β-Hu Luobusu are single chromatographic peak.
Embodiment 2:
(1) gets the Zhejiang low-grade green tea sheet that the tealeaves producing region gathers and processes autumn that becomes civilized, at room temperature through mechanical disintegration to 300 order.Green tea powder extracted 2.5 hours and stirred (mixing speed: 150r/min) under 18 ℃ of conditions with the mixed solution (1: 1: 0.8) that contains ethanol, first alcohol and water.Leave standstill, filter the filter residue drying under reduced pressure.The mass volume ratio of green tea powder and said extracted liquid (g/ml) is 1: 7.5;
(2) filter residue in the step (1) extracted 3 hours under 22 ℃ of conditions with normal hexane and acetone (1: 1), and stir (mixing speed: 200r/min), leave standstill, filtration, the filtrate lyophilize is concentrated into 1/3 of original volume, obtains green tea β-Hu Luobusu crude extract;
(3) aluminum oxide column chromatography on step (2) the gained green tea β-Hu Luobusu crude extract, elutriant is trichloromethane and isohexane, gradient is in proper order: 1.5: 8.5; 2.3: 7.7; 3: 7; 3.6: 6.4 (trichloromethane: isohexane, V: V), flow velocity is 12ml/min, and the effluent liquid fraction collection detects, and merges, and vacuum lyophilization obtains highly purified green tea β-Hu Luobusu.HPLC analysis revealed, prepared β-Hu Luobusu are single chromatographic peak.
Claims (1)
1. method of extracting β-Hu Luobusu from green tea is characterized in that following processing step:
1) select unmetamorphosed green tea for use, it is pulverized is pressed powder, this green tea powder methyl alcohol, ethanol, H
2The mixture of O or wherein at least a solvent extracted 0.5-12.0 hour under 18-35 ℃ of condition, and stirred, and left standstill, filter, and the filter residue drying under reduced pressure, the mass volume ratio g/ml of green tea powder and said extracted liquid is 1: 2-1: 30;
2) filter residue extracted 0.5-24.0 hour under 15-50 ℃ of condition with extracting solution, and stir, leave standstill, filter, the filtrate lyophilize is concentrated into the 1/5-2/3 of original volume, obtain green tea β-Hu Luobusu crude extract, described extracting solution is one or more mixing in ethyl acetate, acetone, normal hexane, isohexane, methylene dichloride and the trichloromethane, and the mass volume ratio g/ml of tea-leaf power and extracting solution is 1: 2-1: 35;
3) column chromatography is carried out gradient elution on the green tea β-Hu Luobusu crude extract, fraction collection, vacuum lyophilization, get high purity green tea β-Hu Luobusu, the column chromatography used medium is silica gel or aluminum oxide, used elutriant is two kinds in ethyl acetate, acetone, normal hexane, isohexane, hexanaphthene, methylene dichloride and the trichloromethane, and the ratio of its concentration gradient volume ratio is changed to 1: 9-5: 5, and elution flow rate is 0.3-55.0ml/min.
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| CN 200710164487 CN101182303B (en) | 2007-12-05 | 2007-12-05 | Method for preparing high-purity beta-carotene from green tea |
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| CN 200710164487 CN101182303B (en) | 2007-12-05 | 2007-12-05 | Method for preparing high-purity beta-carotene from green tea |
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| CN101182303A true CN101182303A (en) | 2008-05-21 |
| CN101182303B CN101182303B (en) | 2010-06-23 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103012229A (en) * | 2012-12-21 | 2013-04-03 | 宁波红龙生物科技有限公司 | Method for preparing high-purity astaxanthin extract |
| CN106220540A (en) * | 2016-07-28 | 2016-12-14 | 南京正宽医药科技有限公司 | The preparation method of a kind of bata-carotene and bata-carotene compositions |
| CN114097852A (en) * | 2021-11-16 | 2022-03-01 | 中国农业科学院茶叶研究所 | Method for preparing sucrose-free whole wheat tea bread based on seed fermentation in refrigeration |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1683334A (en) * | 2005-03-15 | 2005-10-19 | 中国农业大学 | Method for extracting beta-carrotene |
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2007
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103012229A (en) * | 2012-12-21 | 2013-04-03 | 宁波红龙生物科技有限公司 | Method for preparing high-purity astaxanthin extract |
| CN103012229B (en) * | 2012-12-21 | 2014-08-13 | 宁波红龙生物科技有限公司 | Method for preparing high-purity astaxanthin extract |
| CN106220540A (en) * | 2016-07-28 | 2016-12-14 | 南京正宽医药科技有限公司 | The preparation method of a kind of bata-carotene and bata-carotene compositions |
| CN114097852A (en) * | 2021-11-16 | 2022-03-01 | 中国农业科学院茶叶研究所 | Method for preparing sucrose-free whole wheat tea bread based on seed fermentation in refrigeration |
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| CN101182303B (en) | 2010-06-23 |
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