CN1199965C - Method for separating catechin compound from theopolyphenols - Google Patents
Method for separating catechin compound from theopolyphenols Download PDFInfo
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- CN1199965C CN1199965C CN 00128567 CN00128567A CN1199965C CN 1199965 C CN1199965 C CN 1199965C CN 00128567 CN00128567 CN 00128567 CN 00128567 A CN00128567 A CN 00128567A CN 1199965 C CN1199965 C CN 1199965C
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- tea
- acetone
- polyphenol
- separation method
- ethanol
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- Pyrane Compounds (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The present invention relates to a method for separating catechin compounds from tea polyphenols. Tea polyphenols pass through a dextran Sephadex LH-20 packed column of 1.5 meters, the elution is carried out by acetone-ethanol binary mixed solvent of which the acetone content is in a scope ranging from 10 to 30%, and flow speed is 5 to 30 ml/hr; epigallocatechin gallate (EGCG) and catechin monomers of epigallocatechin gallate (ECG) can be separated, the purity is more than 90%, and the highest purity can reach 95% so as to obtain better effect.
Description
The list that the separation method of catechin compounds relates in the tea-polyphenol among the present invention is meant the single-component compound of isolating catechin ester class from tea-polyphenol from thing, as NVP-XAA 723 (EGCG), and L-Epicatechin gallate (ECG) etc.
The tea leaf extract tea-polyphenol has numerous functions such as medicinal widely and daily, and the someone foretells that tea-polyphenol will be the compound that 21 century human health is produced huge effect.And the tea-polyphenol list has more potential broad prospect of application and great economy value from thing.
People are more to the research of tealeaves separation and Extraction tea-polyphenol, and further in the separating tea multi-phenol research of catechin compounds be in the starting stage.The method that the separation of catechin compounds in the tea-polyphenol is adopted has at present: supercritical extraction (Chinese tea 1997,6,18-19), this method purity is higher, but complex process, it is single to separate component, operation inconvenience, cost height.And high performance liquid preparative chromatography method and high performance countercurrent chromatography method (tealeaves circular 1997,19 (4): 34-36) Zhi Bei tea-polyphenol list is from thing purity height, and recovering effect is better, but has the cost of investment height, shortcomings such as difficult expansion scale.(tealeaves circular 1997,19 (4) 34-36) is the extensive isolating method of a kind of energy to the column chromatography for separation method, is therefore generally paid attention to, and many at present aqueous solution with ethanol or acetone are as eluent, and its shortcoming is difficulty of concentrate drying.
The objective of the invention is at prior art difficult point and deficiency, research also discloses a kind of effective separation method, carries out the separation method of catechin compounds in the fairly large tea-polyphenol, promptly adopts catechin compounds in the column chromatography for separation method separating tea multi-phenol.
The technical solution adopted in the present invention is as follows:
Used tea-polyphenol is the method preparation by patent publication No. CN1194966A high-purity tea polyphenol novel technology for extracting.
Under normal pressure, tea-polyphenol is dissolved in a small amount of solvent identical with eluent, last chromatography column, the wash-out separation obtains the tea-polyphenol list from thing.
It is the Glass tubing of 20 millimeters of φ that column jecket adopts internal diameter, long 1500 millimeters of column jecket, and the column jecket detention space of the list after the separation after thing leaves the post fixed phase stuffing is the least possible.The moving phase flow process adopts the automatic pressure reduction of header tank to carry out.
Make the column packed stationary phase with dextran Sephades LH gel series or polymeric amide.Be best wherein with dextran Sephades LH-20.
The elutriant straight alcohol, the binary liquid mixture that pure acetone or acetone and ethanol are formed.With acetone and alcoholic acid binary liquid mixture is best.Acetone concentration in mixed solution is best with 20% between 10～30%.
Eluent flow rate is controlled at per hour 5～30 milliliters, especially with per hour 10 milliliters be best.Separate the back each component and press the peak fraction collection according to Ultraviolet Detector (UV-280mm) wavelength detection back collection of illustrative plates, through efficient liquid phase chromatographic analysis, NVP-XAA 723 (EGCG) wherein, L-Epicatechin gallate (ECG), purity all more than 90%, reaches as high as 95%.Advantages such as this method compared with prior art has the efficient height, and cost is low, and technology is simple.
Example 1
Take by weighing tea-polyphenol 1.5 gram and be dissolved in 4 milliliters of acetone that contain 20% acetone---in the alcohol mixeding liquid, last dextran Sephades LH-20 post, under normal pressure usefulness contain 20% acetone acetone---the ethanol binary liquid mixture is made elutriant, flow velocity is per hour 30 milliliters.Isolate back is after testing collected each component, purity is 432 milligrams of 93.81% NVP-XAA 723; Purity is 170 milligrams of 90.85% L-Epicatechin gallates.
Example 2
Take by weighing tea-polyphenol 1.5 gram and be dissolved in 4 milliliters of acetone that contain 20% acetone---in the ethanol binary liquid mixture, last dextran Sephades LH-20 post, under normal pressure usefulness contain 20% acetone acetone---the ethanol binary liquid mixture is made elutriant, flow velocity is per hour 10 milliliters.Isolate back is after testing collected each component, purity is 480 milligrams of 95.58% NVP-XAA 723; Purity is 171 milligrams of 91.4% L-Epicatechin gallates.
Example 3
Take by weighing tea-polyphenol 1.5 gram and be dissolved in 4 milliliters of acetone that contain 10% acetone---in the ethanol binary liquid mixture, last dextran Sephades LH-20 post, under normal pressure usefulness contain 10% acetone acetone---the ethanol binary liquid mixture is made elutriant, flow velocity is per hour 26 milliliters.Isolate back is after testing collected each component, purity is 385 milligrams of 90.01% NVP-XAA 723; Purity is 102 milligrams of 93.78% L-Epicatechin gallates.
Claims (5)
1. the separation method of catechin compounds in the tea-polyphenol, it is characterized in that, tea-polyphenol is dissolved in a small amount of solvent, by dextran Sephadex LH gel series or polymeric amide packed column, with acetone content is acetone-ethanol binary mixed solvent or acetone of 10～30%, and ethanol list solvent is made eluent, and its flow velocity is per hour 5～30 milliliters, obtain the tea-polyphenol list from thing NVP-XAA 723, L-Epicatechin gallate through the normal pressure separation.
2. the separation method of catechin compounds in the tea-polyphenol according to claim 1 is characterized in that the filler stationary phase is dextran Sephadex gel LH-20 in the packed column.
3. the separation method of catechin compounds in the tea-polyphenol according to claim 1 is characterized in that, eluent is to be the binary mixed solvent that acetone-ethanol of 10～30% is formed with acetone content.
4. as the separation method of catechin compounds in the tea-polyphenol as described in claim 1 or 3, it is characterized in that in acetone-ethanol binary mixtures of eluents, acetone content is 20%.
5. the separation method of catechin compounds in the tea-polyphenol according to claim 1 is characterized in that the eluent flow velocity is per hour 10 milliliters.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00128567 CN1199965C (en) | 2000-11-15 | 2000-11-15 | Method for separating catechin compound from theopolyphenols |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00128567 CN1199965C (en) | 2000-11-15 | 2000-11-15 | Method for separating catechin compound from theopolyphenols |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1319597A CN1319597A (en) | 2001-10-31 |
| CN1199965C true CN1199965C (en) | 2005-05-04 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 00128567 Expired - Fee Related CN1199965C (en) | 2000-11-15 | 2000-11-15 | Method for separating catechin compound from theopolyphenols |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1199965C (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101176302B (en) * | 2005-11-02 | 2010-10-06 | 中兴通讯股份有限公司 | Branch line signal recovery method and device based on non-integer leakage rate |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101134941B (en) * | 2007-07-27 | 2013-03-06 | 东华大学 | Method for preparing EGCG hydrolytic enzyme and producing EGC and gallic acid by aspergillus oryzae |
| CN101492440B (en) * | 2008-01-24 | 2012-10-03 | 上海新康制药厂 | Separation purification process for main catechin component in tea polyphenol and glycosidase activity |
| CN104725342A (en) * | 2015-03-13 | 2015-06-24 | 湖南农业大学 | Method for preparing green feed additive catechin |
| CN108912410A (en) * | 2018-06-24 | 2018-11-30 | 袁暾 | A kind of beta glucan colloid containing tea extraction |
-
2000
- 2000-11-15 CN CN 00128567 patent/CN1199965C/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101176302B (en) * | 2005-11-02 | 2010-10-06 | 中兴通讯股份有限公司 | Branch line signal recovery method and device based on non-integer leakage rate |
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| Publication number | Publication date |
|---|---|
| CN1319597A (en) | 2001-10-31 |
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Granted publication date: 20050504 Termination date: 20131115 |