CN103704422B - Method for preparing and extracting theabrownin by using tea leaves as raw material - Google Patents
Method for preparing and extracting theabrownin by using tea leaves as raw material Download PDFInfo
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- CN103704422B CN103704422B CN201310713639.XA CN201310713639A CN103704422B CN 103704422 B CN103704422 B CN 103704422B CN 201310713639 A CN201310713639 A CN 201310713639A CN 103704422 B CN103704422 B CN 103704422B
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- theabrownin
- raw material
- dry powder
- tealeaves
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- 238000000034 method Methods 0.000 title claims abstract description 21
- 239000002994 raw material Substances 0.000 title claims abstract description 14
- 241001122767 Theaceae Species 0.000 title claims abstract 5
- 239000000843 powder Substances 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000003960 organic solvent Substances 0.000 claims abstract description 9
- 239000012535 impurity Substances 0.000 claims abstract description 7
- 230000001590 oxidative effect Effects 0.000 claims abstract description 7
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 7
- 239000007787 solid Substances 0.000 claims abstract description 7
- RYYVLZVUVIJVGH-UHFFFAOYSA-N caffeine Chemical compound CN1C(=O)N(C)C(=O)C2=C1N=CN2C RYYVLZVUVIJVGH-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000000605 extraction Methods 0.000 claims abstract description 5
- LPHGQDQBBGAPDZ-UHFFFAOYSA-N Isocaffeine Natural products CN1C(=O)N(C)C(=O)C2=C1N(C)C=N2 LPHGQDQBBGAPDZ-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229960001948 caffeine Drugs 0.000 claims abstract description 3
- VJEONQKOZGKCAK-UHFFFAOYSA-N caffeine Natural products CN1C(=O)N(C)C(=O)C2=C1C=CN2C VJEONQKOZGKCAK-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000000835 fiber Substances 0.000 claims abstract description 3
- 239000012141 concentrate Substances 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 6
- 238000002347 injection Methods 0.000 claims description 4
- 239000007924 injection Substances 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 238000007654 immersion Methods 0.000 claims description 2
- 238000002386 leaching Methods 0.000 claims description 2
- 238000005374 membrane filtration Methods 0.000 claims description 2
- 238000005507 spraying Methods 0.000 claims description 2
- 238000001035 drying Methods 0.000 abstract description 3
- 238000011084 recovery Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000001816 cooling Methods 0.000 abstract 1
- 238000001914 filtration Methods 0.000 abstract 1
- 239000012528 membrane Substances 0.000 abstract 1
- 239000008213 purified water Substances 0.000 abstract 1
- 238000002791 soaking Methods 0.000 abstract 1
- 238000001694 spray drying Methods 0.000 abstract 1
- 244000269722 Thea sinensis Species 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 5
- 235000013616 tea Nutrition 0.000 description 5
- 239000008280 blood Substances 0.000 description 3
- 210000004369 blood Anatomy 0.000 description 3
- 238000004821 distillation Methods 0.000 description 2
- 235000009569 green tea Nutrition 0.000 description 2
- 235000019224 Camellia sinensis var Qingmao Nutrition 0.000 description 1
- 208000024172 Cardiovascular disease Diseases 0.000 description 1
- 235000006468 Thea sinensis Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000020279 black tea Nutrition 0.000 description 1
- 208000026106 cerebrovascular disease Diseases 0.000 description 1
- 206010012601 diabetes mellitus Diseases 0.000 description 1
- 230000002526 effect on cardiovascular system Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 235000020339 pu-erh tea Nutrition 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
Abstract
The invention discloses a method for preparing and extracting theabrownin by using tea leaves as a raw material. The method comprises the steps of (1) crushing the tea leaves, putting the crushed tea leaves into an extraction container, and injecting purified water for soaking to obtain extract liquor for later use; (2) cooling the extract liquor, and filtering the extract liquor by using a straight film to remove fiber impurities; (3) performing membrane concentration; (4) extracting a dichloromethane solution at normal temperature to remove caffeine, and taking a lower-level water layer; (5) injecting the lower-level water layer into the container to perform an oxidative polymerization reaction; (6) performing vacuum concentration on the solution to obtain a concentrated solution with the concentration of 20-50%; (7) performing spray drying on the concentrated solution to obtain dry powder; and (8) putting the obtained dry powder into a CO2 supercritical environment to remove trace impurities and trace organic solvents, and then drying to ensure that the water content of the dry powder is less than 4%, thereby obtaining a solid theabrownin product. The method disclosed by the invention has the advantages that the content of theabrownin is increased, the manufacturing cost is reduced, the recovery rate is increased, and the problems that a variety of organic solvents are used in the prior art, the number of residual organic solvents is large and the like are solved.
Description
Technical field
The invention belongs to field of deep tea processing technology, being specially a kind of tealeaves is that the method extracting theabrownin prepared by raw material.
Background technology
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.The technology for producing of current theabrownin 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.
Summary of the invention
Technical problem solved by the invention is to provide a kind of efficient, the method that quick, low cost, high-recovery prepare theabrownin, to solve the problem proposed in above-mentioned background technology.
For achieving the above object, the invention provides following technical scheme:
Tealeaves is that the method extracting theabrownin prepared by raw material, comprises the following steps:
(1) put into leaching vessel after tea leaf powder being broken to sheet, the pure water injecting 80 DEG C-90 DEG C soaks 40-60min, and be extracted liquid, the same terms repeats lixiviate once again, merges twice extract for subsequent use;
(2) twice extract after merging is cooled to after 40 DEG C below and performs membrane filtration, remove fiber impurity;
(3) film is concentrated into the concentrate that concentration is 2-5%;
(4) add isopyknic dichloromethane solution at normal temperatures, extraction removes caffeine, gets lower aqueous layer;
(5) oxidative polymerization is carried out by the lower aqueous layer obtained injection container;
(6), after having reacted, be the concentrate of 20-50% by solution for vacuum concentration to concentration;
(7) concentrate is carried out spraying dry, obtained dry powder;
(8) gained dry powder is put into CO2 overcritical, remove trace impurity and minim organic solvent further, then dry further, make the moisture of dry powder below 4%, the theabrownin product of solid shape can be obtained.
In step (1), the tealeaves of input and the weight part ratio of water are 1:10, and tealeaves circulating-heating in immersion process makes liquid keep constant temperature.
In step (5), the time of described oxidative polymerization is 30-60min.
In step (7), the moisture of described dry powder is 15%.
In step (8), in described solid theabrownin, the content of theabrownin is more than 90%.
In sum, beneficial effect of the present invention:
Invention increases theabrownin content, reduce cost of manufacture, improve the rate of recovery, the problem such as overcome prior art with an organic solvent wide in variety, organic solvent residual is large.
Accompanying drawing explanation
Fig. 1 is present invention process flow chart.
Detailed description of the invention
Below in conjunction with the embodiment of the present invention, be clearly and completely described the technical scheme in the embodiment of the present invention, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
Embodiment 1
Tealeaves is that the method extracting theabrownin prepared by raw material, comprises the following steps:
(1) get common green tea (or other local tea variety) 20g, grind slabbing and be placed in beaker the pure water 200ml that injects 90-100% and companion's heating keeps extracting liq after constant temperature 60min, repeat to extract once with condition;
(2) above-mentioned 400ml extract heating is concentrated to 150ml;
(3) previous step 150ml concentrate is added the extraction of 150ml chloroformic solution and leave lower aqueous layer 150ml;
(4) oxidative polymerization 60min is carried out by the airtight molten ware of previous step water layer 150ml injection;
(5) polymerisation to be oxidized complete after distillation be drying to obtain more than 80% solid fraction theabrownin fine work 5.35g.
Embodiment 2
Tealeaves is that the method extracting theabrownin prepared by raw material, comprises the following steps:
(1) get common green tea (or other local tea variety) 20g, grind slabbing and be placed in beaker the pure water 100ml that injects 70-80% and companion's heating keeps extracting liq after constant temperature 40min, repeat to extract once with condition;
(2) above-mentioned 200ml extract heating is concentrated to 150ml;
(3) previous step 150ml concentrate is added the extraction of 150ml chloroformic solution and leave lower aqueous layer 150ml;
(4) oxidative polymerization 30min is carried out by the airtight molten ware of previous step water layer 150ml injection;
(5) polymerisation to be oxidized complete after distillation be drying to obtain theabrownin content more than 80% solid fraction theabrownin fine work 4.45g.
To those skilled in the art, obviously the invention is not restricted to the details of above-mentioned one exemplary embodiment, and when not deviating from spirit of the present invention or essential characteristic, the present invention can be realized in other specific forms.Therefore, no matter from which point, all should embodiment be regarded as exemplary, and be nonrestrictive, scope of the present invention is limited by claims instead of above-mentioned explanation, and all changes be therefore intended in the implication of the equivalency by dropping on claim and scope are included in the present invention.
In addition, be to be understood that, although this description is described according to embodiment, but not each embodiment only comprises an independently technical scheme, this narrating mode of description is only for clarity sake, those skilled in the art should by description integrally, and the technical scheme in each embodiment also through appropriately combined, can form other embodiments that it will be appreciated by those skilled in the art that.
Claims (5)
1. be that raw material is prepared and extracted the method for theabrownin with tealeaves, it is characterized in that, comprise the following steps:
(1) put into leaching vessel after tea leaf powder being broken to sheet, the pure water injecting 80 DEG C-90 DEG C soaks 40-60min, and be extracted liquid, the same terms repeats lixiviate once again, merges twice extract for subsequent use;
(2) twice extract after merging is cooled to after 40 DEG C below and performs membrane filtration, remove fiber impurity;
(3) film is concentrated into the concentrate that concentration is 2-5%;
(4) add isopyknic dichloromethane solution at normal temperatures, extraction removes caffeine, gets lower aqueous layer;
(5) oxidative polymerization is carried out by the lower aqueous layer obtained injection container;
(6), after having reacted, be the concentrate of 20-50% by solution for vacuum concentration to concentration;
(7) concentrate is carried out spraying dry, obtained dry powder;
(8) gained dry powder is put into CO2 overcritical, remove trace impurity and minim organic solvent further, then dry further, make the moisture of dry powder below 4%, the theabrownin product of solid shape can be obtained.
2. a kind of tealeaves according to claim 1 is that the method extracting theabrownin prepared by raw material, and it is characterized in that, in step (1), the tealeaves of input and the weight part ratio of water are 1:10, and tealeaves circulating-heating in immersion process makes liquid keep constant temperature.
3. a kind of tealeaves according to claim 1 is that the method extracting theabrownin prepared by raw material, and it is characterized in that, in step (5), the time of described oxidative polymerization is 30-60min.
4. a kind of tealeaves according to claim 1 is that the method extracting theabrownin prepared by raw material, and it is characterized in that, in step (7), the moisture of described dry powder is 15%.
5. a kind of tealeaves according to claim 1 is that the method extracting theabrownin prepared by raw material, and it is characterized in that, in step (8), in described solid theabrownin, the content of theabrownin is more than 90%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310713639.XA CN103704422B (en) | 2013-12-23 | 2013-12-23 | Method for preparing and extracting theabrownin by using tea leaves as raw material |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310713639.XA CN103704422B (en) | 2013-12-23 | 2013-12-23 | Method for preparing and extracting theabrownin by using tea leaves as raw material |
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| Publication Number | Publication Date |
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| CN103704422A CN103704422A (en) | 2014-04-09 |
| CN103704422B true CN103704422B (en) | 2015-06-17 |
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| CN201310713639.XA Active CN103704422B (en) | 2013-12-23 | 2013-12-23 | Method for preparing and extracting theabrownin by using tea leaves as raw material |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104365912A (en) * | 2014-11-27 | 2015-02-25 | 桂林瑞丰环保微生物应用研究所 | Method for preparing and extracting theabrownin |
| CN104614335A (en) * | 2015-02-12 | 2015-05-13 | 张进 | Method for rapidly identifying theabrownin |
| CN113841760A (en) * | 2021-09-30 | 2021-12-28 | 北京小罐茶业有限公司 | A beverage prepared from tea and coffee, and its preparation method |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1480457A (en) * | 2003-06-25 | 2004-03-10 | 张守政 | Method for extracting tea polyhenols and tea pigment |
| CN1482126A (en) * | 2003-07-21 | 2004-03-17 | 红河唐人生物发展有限公司 | Tea polyphenols extracting process |
| CN101474313A (en) * | 2009-02-02 | 2009-07-08 | 普洱市人民政府茶产业发展办公室科技服务中心 | Application of theabrownin in pharmacy |
| CN102334574A (en) * | 2011-08-23 | 2012-02-01 | 广西师范学院 | Method for extracting theabrownin crude product from Liupu tea |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008118933A (en) * | 2006-11-13 | 2008-05-29 | Taiyo Kagaku Co Ltd | Polyphenol composition |
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- 2013-12-23 CN CN201310713639.XA patent/CN103704422B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1480457A (en) * | 2003-06-25 | 2004-03-10 | 张守政 | Method for extracting tea polyhenols and tea pigment |
| CN1482126A (en) * | 2003-07-21 | 2004-03-17 | 红河唐人生物发展有限公司 | Tea polyphenols extracting process |
| CN101474313A (en) * | 2009-02-02 | 2009-07-08 | 普洱市人民政府茶产业发展办公室科技服务中心 | Application of theabrownin in pharmacy |
| CN102334574A (en) * | 2011-08-23 | 2012-02-01 | 广西师范学院 | Method for extracting theabrownin crude product from Liupu tea |
Non-Patent Citations (1)
| Title |
|---|
| 秦谊,等.普洱茶茶褐素提取工艺及理化性质的初步研究.《林产化学与工业》.2009,第29卷(第5期),第95-98页. * |
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Effective date of registration: 20170216 Address after: 661000 Yunnan Honghe Mengzi economic and Technological Development Zone Patentee after: Yunnan Tang biological Polytron Technologies Inc. Address before: 661400 Yunnan Province Honghe Hani and Yi Autonomous Prefecture, Gejiu City, Jiangchuan No. 18 lane of No. 802 Patentee before: Zhang Songbo Patentee before: Gao Yi Patentee before: Yang Ge Patentee before: Bai Xiong |
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Effective date of registration: 20231103 Address after: Room 1608 and 1609, 16th Floor, Building 23, Phase 4B, Dianchi Kangqiao Community, southeast of the intersection of South Second Ring Road and Qianwei West Road, Xishan District, Kunming City, Yunnan Province, 650100 Patentee after: Yunnan Tangren Zhongchuang Science and Technology Research Institute Address before: 661000 Mengzi Economic and Technological Development Zone, Honghe Prefecture, Yunnan Province Patentee before: Yunnan Tang biological Polytron Technologies Inc. |
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