CN104365912A - Method for preparing and extracting theabrownin - Google Patents

Method for preparing and extracting theabrownin Download PDF

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Publication number
CN104365912A
CN104365912A CN201410699230.1A CN201410699230A CN104365912A CN 104365912 A CN104365912 A CN 104365912A CN 201410699230 A CN201410699230 A CN 201410699230A CN 104365912 A CN104365912 A CN 104365912A
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China
Prior art keywords
theabrownin
obtains
tealeaves
water layer
earth
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CN201410699230.1A
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Chinese (zh)
Inventor
林炳营
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GUILIN RUIFENG ENVIRONMENTAL PROTECTION MICROBIOLOGY APPLICATION INSTITUTE
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GUILIN RUIFENG ENVIRONMENTAL PROTECTION MICROBIOLOGY APPLICATION INSTITUTE
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Priority to CN201410699230.1A priority Critical patent/CN104365912A/en
Publication of CN104365912A publication Critical patent/CN104365912A/en
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Abstract

The invention belongs to the technical field of biological pharmacy, and particularly relates to a method for preparing and extracting theabrownin. The method comprises the following steps: baking, grinding, extracting, concentrating, extracting and the like. The method is simple in process, low in cost, safe and reliable, and is suitable for production of middle and small-sized enterprises.

Description

A kind of preparation of theabrownin and extracting method
Technical field
The invention belongs to biological pharmacy technical field, be specifically related to a kind of preparation and extracting method of theabrownin.
Background technology.
Polyphenols in tealeaves is the important active substances in tealeaves, it is the general name of multiple phenolic compound in tealeaves, it is the main constituent of fresh leaves of tea plant, be wherein its bulk composition with catechin, account for 60% ~ 80% of polyphenols total amount, have close relationship with the soup look of tea, flavour and fragrance.
Water-soluble products mainly theaflavin, thearubigin and the theabrownin of polyphenols.Theabrownin is the general name of the very complicated product of a class formation that catechin oxidation polymerization is formed, in the process of Pu'er tea 80% theaflavin and thearubigin oxidation, polymerization, form theabrownin, and its content is multiplied, thus the convergence of millet paste and bitter taste are obviously reduced, add higher sugar and solubility water extraction content, the flavour which forms Pu'er tea is mellow, the material base that soup look reddish brown.
Theabrownin can effectively reduce blood fat, blood sugar and blood viscosity, in cardiovascular and cerebrovascular disease and diabetes mellitus prevention, have remarkable effect, can be used as the supplementary material of food and health products etc., has wide application prospect.Current theabrownin technology for producing is little, mainly contain and take fermentation method for raw material with tea fresh leaves etc. or from the black tea such as Pu'er tea, adopt multiple organic solvent extraction and purifying, due to the complicated component of raw material, in the impurity of these methods in its preparation technology downstream and organic solvent removing, target product purification etc., technological process is loaded down with trivial details, energy consumption cost is high, environmental pollution is serious.
But in the prior art, the extraction of theabrownin is subject to very many-sided restriction.First be the content in raw material, wherein in green tea and white tea, content is very micro-, and in black tea, theabrownin content is also only 5% ~ 10%, and what theabrownin content was the highest is black tea, so it is very limited to extract raw material; Next is extracting method, and existing most of theabrownin adopts organic reagent extraction to obtain, and there is safety issue, cannot be used for medicine and field of food, the scope of application is subject to larger restriction.
Summary of the invention
The object of this invention is to provide a kind of preparation and extracting method of theabrownin.The method technique is simple, and cost is low, safe and reliable, is applicable to medium-sized and small enterprises production and application.
The preparation of theabrownin and an extracting method, comprise the following steps:
1) tealeaves slightly fermented is cured 2h ~ 4h under 140 DEG C ~ 155 DEG C conditions, taking-up is cured sample and is cooled to room temperature, obtains the tealeaves after baking and banking up with earth;
2) by step 1) obtain bake and bank up with earth after tealeaves pulverize, cross 45 ~ 65 mesh sieves, immerses 85 DEG C ~ 95 DEG C pure water immersion 1h ~ 3h, be extracted liquid, the same terms repeats lixiviate twice again, merges three extracts for subsequent use;
3) extract after merging is cooled to carry out film after less than 35 DEG C overanxious, removes fiber impurity;
4) by step 3) the extract concentration that obtains is the concentrate of 1 ~ 4%;
5) add the dichloromethane solution of 1 ~ 1.5 times of volume at normal temperatures, extraction removes caffeine, gets lower aqueous layer and adds ammoniacal liquor reaction 24 ~ 48 hours, obtain theabrownin crude product;
6) extracted by theabrownin crude product ethyl propionate, obtain water layer, water layer uses ethanol extraction again, obtains water layer, obtains theabrownin after drying.
Preferably, comprise the following steps:
1) tealeaves slightly fermented is cured 4h under 150 DEG C of conditions, taking-up is cured sample and is cooled to room temperature, obtains the tealeaves after baking and banking up with earth;
2) by step 1) obtain bake and bank up with earth after tealeaves pulverize, cross 65 mesh sieves, immerses 85 DEG C pure water immersion 3h, be extracted liquid, the same terms repeats lixiviate twice again, merges three extracts for subsequent use;
3) extract after merging is cooled to carry out film after less than 35 DEG C overanxious, removes fiber impurity;
4) by step 3) the extract concentration that obtains is the concentrate of 3%;
5) add the dichloromethane solution of 1.5 times of volumes at normal temperatures, extraction removes caffeine, gets lower aqueous layer and adds ammoniacal liquor and react 24 hours, obtain theabrownin crude product;
6) extracted by theabrownin crude product ethyl propionate, obtain water layer, water layer uses ethanol extraction again, obtains water layer, obtains theabrownin after drying.
Preferably, comprise the following steps:
1) tealeaves slightly fermented is cured 4h under 140 DEG C of conditions, taking-up is cured sample and is cooled to room temperature, obtains the tealeaves after baking and banking up with earth;
2) by step 1) obtain bake and bank up with earth after tealeaves pulverize, cross 45 mesh sieves, immerses 95 DEG C pure water immersion 1h, be extracted liquid, the same terms repeats lixiviate twice again, merges three extracts for subsequent use;
3) extract after merging is cooled to carry out film after less than 35 DEG C overanxious, removes fiber impurity;
4) by step 3) the extract concentration that obtains is the concentrate of 4%;
5) add the dichloromethane solution of 1 times of volume at normal temperatures, extraction removes caffeine, gets lower aqueous layer and adds ammoniacal liquor and react 48 hours, obtain theabrownin crude product;
6) extracted by theabrownin crude product ethyl propionate, obtain water layer, water layer uses ethanol extraction again, obtains water layer, obtains theabrownin after drying.
Preferably, comprise the following steps:
1) tealeaves slightly fermented is cured 3h under 148 DEG C of conditions, taking-up is cured sample and is cooled to room temperature, obtains the tealeaves after baking and banking up with earth;
2) by step 1) obtain bake and bank up with earth after tealeaves pulverize, cross 55 mesh sieves, immerses 90 DEG C pure water immersion 2h, be extracted liquid, the same terms repeats lixiviate twice again, merges three extracts for subsequent use;
3) extract after merging is cooled to carry out film after less than 35 DEG C overanxious, removes fiber impurity;
4) by step 3) the extract concentration that obtains is the concentrate of 2.5%;
5) add the dichloromethane solution of 1.3 times of volumes at normal temperatures, extraction removes caffeine, gets lower aqueous layer and adds ammoniacal liquor and react 36 hours, obtain theabrownin crude product;
6) extracted by theabrownin crude product ethyl propionate, obtain water layer, water layer uses ethanol extraction again, obtains water layer, obtains theabrownin after drying.
Detailed description of the invention
Be described principle of the present invention and feature below, example, only for explaining the present invention, is not intended to limit scope of the present invention.
Embodiment 1
The preparation of theabrownin and an extracting method, comprise the following steps:
1) tealeaves slightly fermented is cured 4h under 150 DEG C of conditions, taking-up is cured sample and is cooled to room temperature, obtains the tealeaves after baking and banking up with earth;
2) by step 1) obtain bake and bank up with earth after tealeaves pulverize, cross 65 mesh sieves, immerses 85 DEG C pure water immersion 3h, be extracted liquid, the same terms repeats lixiviate twice again, merges three extracts for subsequent use;
3) extract after merging is cooled to carry out film after less than 35 DEG C overanxious, removes fiber impurity;
4) by step 3) the extract concentration that obtains is the concentrate of 3%;
5) add the dichloromethane solution of 1.5 times of volumes at normal temperatures, extraction removes caffeine, gets lower aqueous layer and adds ammoniacal liquor and react 24 hours, obtain theabrownin crude product;
6) extracted by theabrownin crude product ethyl propionate, obtain water layer, water layer uses ethanol extraction again, obtains water layer, obtains theabrownin after drying.
Embodiment 2
The preparation of theabrownin and an extracting method, comprise the following steps:
1) tealeaves slightly fermented is cured 4h under 140 DEG C of conditions, taking-up is cured sample and is cooled to room temperature, obtains the tealeaves after baking and banking up with earth;
2) by step 1) obtain bake and bank up with earth after tealeaves pulverize, cross 45 mesh sieves, immerses 95 DEG C pure water immersion 1h, be extracted liquid, the same terms repeats lixiviate twice again, merges three extracts for subsequent use;
3) extract after merging is cooled to carry out film after less than 35 DEG C overanxious, removes fiber impurity;
4) by step 3) the extract concentration that obtains is the concentrate of 4%;
5) add the dichloromethane solution of 1 times of volume at normal temperatures, extraction removes caffeine, gets lower aqueous layer and adds ammoniacal liquor and react 48 hours, obtain theabrownin crude product;
6) extracted by theabrownin crude product ethyl propionate, obtain water layer, water layer uses ethanol extraction again, obtains water layer, obtains theabrownin after drying.
Embodiment 3
The preparation of theabrownin and an extracting method, comprise the following steps:
1) tealeaves slightly fermented is cured 3h under 148 DEG C of conditions, taking-up is cured sample and is cooled to room temperature, obtains the tealeaves after baking and banking up with earth;
2) by step 1) obtain bake and bank up with earth after tealeaves pulverize, cross 55 mesh sieves, immerses 90 DEG C pure water immersion 2h, be extracted liquid, the same terms repeats lixiviate twice again, merges three extracts for subsequent use;
3) extract after merging is cooled to carry out film after less than 35 DEG C overanxious, removes fiber impurity;
4) by step 3) the extract concentration that obtains is the concentrate of 2.5%;
5) add the dichloromethane solution of 1.3 times of volumes at normal temperatures, extraction removes caffeine, gets lower aqueous layer and adds ammoniacal liquor and react 36 hours, obtain theabrownin crude product;
6) extracted by theabrownin crude product ethyl propionate, obtain water layer, water layer uses ethanol extraction again, obtains water layer, obtains theabrownin after drying.
The foregoing is only better embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.

Claims (4)

1. the preparation of theabrownin and an extracting method, comprises the following steps:
1) tealeaves slightly fermented is cured 2h ~ 4h under 140 DEG C ~ 155 DEG C conditions, taking-up is cured sample and is cooled to room temperature, obtains the tealeaves after baking and banking up with earth;
2) by step 1) obtain bake and bank up with earth after tealeaves pulverize, cross 45 ~ 65 mesh sieves, immerses 85 DEG C ~ 95 DEG C pure water immersion 1h ~ 3h, be extracted liquid, the same terms repeats lixiviate twice again, merges three extracts for subsequent use;
3) extract after merging is cooled to carry out film after less than 35 DEG C overanxious, removes fiber impurity;
4) by step 3) the extract concentration that obtains is the concentrate of 1 ~ 4%;
5) add the dichloromethane solution of 1 ~ 1.5 times of volume at normal temperatures, extraction removes caffeine, gets lower aqueous layer and adds ammoniacal liquor reaction 24 ~ 48 hours, obtain theabrownin crude product;
6) extracted by theabrownin crude product ethyl propionate, obtain water layer, water layer uses ethanol extraction again, obtains water layer, obtains theabrownin after drying.
2. the preparation of theabrownin according to claim 1 and extracting method, comprises the following steps:
1) tealeaves slightly fermented is cured 4h under 150 DEG C of conditions, taking-up is cured sample and is cooled to room temperature, obtains the tealeaves after baking and banking up with earth;
2) by step 1) obtain bake and bank up with earth after tealeaves pulverize, cross 65 mesh sieves, immerses 85 DEG C pure water immersion 3h, be extracted liquid, the same terms repeats lixiviate twice again, merges three extracts for subsequent use;
3) extract after merging is cooled to carry out film after less than 35 DEG C overanxious, removes fiber impurity;
4) by step 3) the extract concentration that obtains is the concentrate of 3%;
5) add the dichloromethane solution of 1.5 times of volumes at normal temperatures, extraction removes caffeine, gets lower aqueous layer and adds ammoniacal liquor and react 24 hours, obtain theabrownin crude product;
6) extracted by theabrownin crude product ethyl propionate, obtain water layer, water layer uses ethanol extraction again, obtains water layer, obtains theabrownin after drying.
3. the preparation of theabrownin according to claim 1 and extracting method, comprises the following steps:
1) tealeaves slightly fermented is cured 4h under 140 DEG C of conditions, taking-up is cured sample and is cooled to room temperature, obtains the tealeaves after baking and banking up with earth;
2) by step 1) obtain bake and bank up with earth after tealeaves pulverize, cross 45 mesh sieves, immerses 95 DEG C pure water immersion 1h, be extracted liquid, the same terms repeats lixiviate twice again, merges three extracts for subsequent use;
3) extract after merging is cooled to carry out film after less than 35 DEG C overanxious, removes fiber impurity;
4) by step 3) the extract concentration that obtains is the concentrate of 4%;
5) add the dichloromethane solution of 1 times of volume at normal temperatures, extraction removes caffeine, gets lower aqueous layer and adds ammoniacal liquor and react 48 hours, obtain theabrownin crude product;
6) extracted by theabrownin crude product ethyl propionate, obtain water layer, water layer uses ethanol extraction again, obtains water layer, obtains theabrownin after drying.
4. the preparation of theabrownin according to claim 1 and extracting method, comprises the following steps:
1) tealeaves slightly fermented is cured 3h under 148 DEG C of conditions, taking-up is cured sample and is cooled to room temperature, obtains the tealeaves after baking and banking up with earth;
2) by step 1) obtain bake and bank up with earth after tealeaves pulverize, cross 55 mesh sieves, immerses 90 DEG C pure water immersion 2h, be extracted liquid, the same terms repeats lixiviate twice again, merges three extracts for subsequent use;
3) extract after merging is cooled to carry out film after less than 35 DEG C overanxious, removes fiber impurity;
4) by step 3) the extract concentration that obtains is the concentrate of 2.5%;
5) add the dichloromethane solution of 1.3 times of volumes at normal temperatures, extraction removes caffeine, gets lower aqueous layer and adds ammoniacal liquor and react 36 hours, obtain theabrownin crude product;
6) extracted by theabrownin crude product ethyl propionate, obtain water layer, water layer uses ethanol extraction again, obtains water layer, obtains theabrownin after drying.
CN201410699230.1A 2014-11-27 2014-11-27 Method for preparing and extracting theabrownin Pending CN104365912A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109699662A (en) * 2019-02-26 2019-05-03 廊坊市维金农业科技有限公司 A kind of preparation method of the disease-resistant preparation of the plant anthelmintic containing caffeine
CN115260198A (en) * 2022-07-07 2022-11-01 上海卓鼎生物技术有限公司 Method for extracting, separating and purifying tea extract

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101696269A (en) * 2009-10-29 2010-04-21 中国农业科学院茶叶研究所 Method for preparing theabrownins by using tea polyphenols as raw materials
CN103304801A (en) * 2012-03-14 2013-09-18 云南天士力帝泊洱生物茶集团有限公司 Method for preparing theabrownin
CN103504048A (en) * 2012-06-29 2014-01-15 云南天士力帝泊洱生物茶集团有限公司 High, medium and low-poly theabrownin and preparation method thereof
CN103704422A (en) * 2013-12-23 2014-04-09 张松波 Method for preparing and extracting theabrownin by using tea leaves as raw material

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101696269A (en) * 2009-10-29 2010-04-21 中国农业科学院茶叶研究所 Method for preparing theabrownins by using tea polyphenols as raw materials
CN103304801A (en) * 2012-03-14 2013-09-18 云南天士力帝泊洱生物茶集团有限公司 Method for preparing theabrownin
CN103504048A (en) * 2012-06-29 2014-01-15 云南天士力帝泊洱生物茶集团有限公司 High, medium and low-poly theabrownin and preparation method thereof
CN103704422A (en) * 2013-12-23 2014-04-09 张松波 Method for preparing and extracting theabrownin by using tea leaves as raw material

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
何英姿等: "六堡茶茶褐素的提取工艺及其抗氧化活性研究", 《安徽农业科学》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109699662A (en) * 2019-02-26 2019-05-03 廊坊市维金农业科技有限公司 A kind of preparation method of the disease-resistant preparation of the plant anthelmintic containing caffeine
CN115260198A (en) * 2022-07-07 2022-11-01 上海卓鼎生物技术有限公司 Method for extracting, separating and purifying tea extract

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Application publication date: 20150225