CN1876656A - Triptolide purification method - Google Patents
Triptolide purification method Download PDFInfo
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- CN1876656A CN1876656A CN 200510026668 CN200510026668A CN1876656A CN 1876656 A CN1876656 A CN 1876656A CN 200510026668 CN200510026668 CN 200510026668 CN 200510026668 A CN200510026668 A CN 200510026668A CN 1876656 A CN1876656 A CN 1876656A
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- triptolide
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Abstract
The invention relates the purity method of triptolide alcohol, comprising the following steps: using tripterygium wilfordii as raw material, adding adsorbent and dispersion dissolvent, adsorbing, filtering, thickening, drying, and getting tripterygium wilfordii extract concrete. The method has the advantages of simple operation, short time and high triptolide alcohol transition rate.
Description
Technical field
The present invention relates to the Chinese drug preparation technique field, be specifically related to a kind of triptolide purification method.
Background technology
Triptolide (triptolide), promptly triptolide is one of main component in the trypterygine, it is an immunosuppressant main active ingredient in the trypterygine preparation, also is toxic component simultaneously, in present Chinese medicine preparation its content is had strict control.
Because the effective dose and the toxic dose of triptolide are very approaching, negated substantially with single component developing new drug possibility.Yet as effective lead drug (lead drug), over nearly more than 20 years, the medicine scholar is constantly screening the triptolide derivative always both at home and abroad, and has obtained many encouraging progress.
For potential triptolide derivative new drug development, the preparation of the triptolide of precursor structure is relatively a reality and a urgent problem with supply.With regard to present progress, but the complete synthesis level that does not reach practical application as yet of triptolide that is to say that the plain raw material of present first generally is that extraction separation obtains from plant.
Triptolide content in trypterygine or Tripterygium hypoglaucum is all very low, generally between 10～30ppm, and extract through solvent, in the conventional medicinal extract behind the purifying, its first cellulose content is not high yet, generally about in the of 1%.If directly go up column chromatography for separation first element with the medicinal extract of these quality, the efficient of its preparation work is lower certainly, and cost is also quite expensive, is unfavorable for possible from now on industrialization production.Therefore, how adopting economically and reasonably method to extract triptolide from trypterygine or Tripterygium hypoglaucum is a difficult problem that always perplexs people.
Summary of the invention
Technical problem to be solved by this invention is to adopt simple, economic purification process, improves the content of triptolide in the Radix Tripterygii Wilfordii extract greatly, makes preparation high purity triptolide become possibility.
Triptolide purification method disclosed by the invention is to be raw material with common Radix Tripterygii Wilfordii extract, and by adding sorbent material and disperseing solvent, fully absorption is filtered, and concentrates, and drying obtains the Radix Tripterygii Wilfordii extract medicinal extract of purifying.
The preferred purification process of the present invention is:
Get 1 part of commercially available common Radix Tripterygii Wilfordii extract, add 3～10 parts of sorbent materials, under 30～50 ℃, whipped state, dissolve extract with solvent, filter then, filter cake washs for several times with fresh solvent, and used solvent total amount is 15～30 times of extract amount, merging filtrate and washing lotion, concentrate, drying obtains the Radix Tripterygii Wilfordii extract extract powder of purifying.
Commercially available common Radix Tripterygii Wilfordii extract of the present invention is meant and adopts ordinary method to extract the Radix Tripterygii Wilfordii extract that obtains that the content of its triptolide is about 1%.
Described sorbent material is selected from adsorption mediums commonly used such as silica gel, neutral alumina, Mierocrystalline cellulose and diatomite.
Described solvent is selected from lower aliphatic alkane, lower aliphatic ketone, ester, lower halogenated alkane or their mixture.
The purifying medicinal extract yield that obtains with the inventive method is about 50%, and through the HPLC assay, its triptolide content is about 2%, and the rate of transform of triptolide composition reaches more than 95%.
Because triptolide content in Chinese medicine trypterygine or Tripterygium hypoglaucum is all very low, therefore in the extraction separation process to it, the actual transfer rate of making great efforts the every step process triptolide composition of raising just seems and is even more important.Through column chromatography for separation, triptolide exists certain, irresistible adsorptivity loss, along with employed sorbing material different in kind, the triptolide composition rate of transform is generally 60～85%, therefore in actual industrial production, should reduce the number of times of capable column chromatography for separation as far as possible,, improve actual productivity and prepare yield so that reduce the loss of the plain composition of first the biglyyest.
The present invention is directed to above-mentioned triptolide separation characteristic, handle the method for Radix Tripterygii Wilfordii extract, obtained satisfied effect to disperse absorption method.About the characteristics of this dispersion absorption method and column chromatography relatively see Table 1.
Table 1. disperses absorption method to separate the plain characteristics of first with column chromatography relatively
| Project approach | The triptolide composition rate of transform | Solvent consumption (medicinal extract amount multiple) | Prepare man-hour | Medicinal extract volume reduction | Medicinal extract raw material treatment capacity |
| Dispersion method of the present invention | ＞95％ | 10～30 | 1 day | 1 times | Do not limit |
| Chromatography | 60～85％ | 60～90 | 2 weeks | 5～10 times | Limited |
From above-mentioned contrast as can be seen, the present invention is a raw material with commercially available Radix Tripterygii Wilfordii extract, and the dispersion adsorption method that adopts conventional sorbing material to carry out non-column chromatography is handled, and the purifying medicinal extract volume of gained reduces half, and its triptolide content doubles.Characteristics such as that these method sharpest edges are is simple to operate, preparation man-hour is short, triptolide rate of transform height and solvent consumption are little, more real is the medicinal extract of handling by the inventive method, when subsequent rows column chromatography for separation first is plain, disturb impurity greatly to reduce, lay a good foundation for finally obtaining the high purity triptolide easily.
Description of drawings
Fig. 1 embodiment 1 product HPLC figure
Fig. 2 triptolide reference substance HPLC figure
Embodiment
Embodiment 1
Get Radix Tripterygii Wilfordii extract (triptolide content 1%) 2kg, 12kg silica gel adds chloroform 15kg, fully stirs under 30 ℃ of heat-retaining conditions, and extract is fully dissolved, and filters then, and filter cake washs for several times with chloroform, and the total consumption of chloroform is 30kg.Combined chloroform liquid, it is dried to contract, and obtains purifying Radix Tripterygii Wilfordii extract 0.9kg, and its triptolide content is that 2.2% (HPLC method) sees that Fig. 1, Fig. 2 are the triptolide reference substance.
Embodiment 2
Get Radix Tripterygii Wilfordii extract 1kg (triptolide content 1%), neutral alumina 5kg, add ethyl acetate 10kg, under 40 ℃ of heat-retaining conditions, fully stir, the dissolving extract, filter then, filter cake washs for several times with remaining 5kg ethyl acetate, combined ethyl acetate filtrate and washings, vacuum concentration, drying, get purified extract 0.5kg, its triptolide content is 2.0%.
Embodiment 3
Get Radix Tripterygii Wilfordii extract 1kg (triptolide content 1%), diatomite 10kg, with 15kg acetone-hexanaphthene (1: 1), fully stir the dissolving extract down at 35 ℃, filter then, filter cake washs for several times with the above-mentioned solvent of 10kg, merging filtrate and washings, vacuum concentration, drying, get purified extract 0.6kg, its triptolide content is 1.7%.
Claims (3)
1, a kind of triptolide purification method is characterized in that this method is:
Get 1 part of common Radix Tripterygii Wilfordii extract, add 3～10 parts of sorbent materials, under 30～50 ℃, whipped state, dissolve extract with solvent, filter then, filter cake washs for several times with fresh solvent, and used solvent total amount is 15～30 times of extract amount, merging filtrate and washing lotion, concentrate, drying obtains the Radix Tripterygii Wilfordii extract extract powder of purifying.
2, triptolide purification method according to claim 1 is characterized in that wherein said sorbent material is selected from silica gel, neutral alumina, Mierocrystalline cellulose and diatomite.
3, triptolide purification method according to claim 1 is characterized in that wherein said solvent is selected from lower aliphatic alkane, lower aliphatic ketone, ester, lower halogenated alkane or their mixture.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100266684A CN100387604C (en) | 2005-06-10 | 2005-06-10 | Triptolide purification method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100266684A CN100387604C (en) | 2005-06-10 | 2005-06-10 | Triptolide purification method |
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| CN1876656A true CN1876656A (en) | 2006-12-13 |
| CN100387604C CN100387604C (en) | 2008-05-14 |
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| CNB2005100266684A Active CN100387604C (en) | 2005-06-10 | 2005-06-10 | Triptolide purification method |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101235041A (en) * | 2007-10-26 | 2008-08-06 | 北京美迪克斯生物技术有限公司 | Four kinds of tripterygium wilfordii derivative and preparing method of pharmaceutics thereof |
| CN101088519B (en) * | 2007-07-17 | 2010-08-18 | 上海美通生物科技有限公司 | Tripterygium glycosides extract and its extraction process |
| CN101991633B (en) * | 2009-10-10 | 2012-11-07 | 上海复旦复华药业有限公司 | Method for extracting tripterygium glycosides, and product and inclusion compound and medicinal composition thereof |
| CN103610727A (en) * | 2013-11-26 | 2014-03-05 | 浙江得恩德制药有限公司 | Method for reducing organic solvent residue in tripterygium glycoside |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1052860A (en) * | 1989-12-22 | 1991-07-10 | 中国医学科学院皮肤病研究所 | The preparation method of tripchlorolide and antifertility purposes |
-
2005
- 2005-06-10 CN CNB2005100266684A patent/CN100387604C/en active Active
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101088519B (en) * | 2007-07-17 | 2010-08-18 | 上海美通生物科技有限公司 | Tripterygium glycosides extract and its extraction process |
| CN101235041A (en) * | 2007-10-26 | 2008-08-06 | 北京美迪克斯生物技术有限公司 | Four kinds of tripterygium wilfordii derivative and preparing method of pharmaceutics thereof |
| CN101235041B (en) * | 2007-10-26 | 2013-05-29 | 北京美迪克斯生物技术有限公司 | Four kinds of tripterygium wilfordii derivative and preparing method of pharmaceutics thereof |
| CN101991633B (en) * | 2009-10-10 | 2012-11-07 | 上海复旦复华药业有限公司 | Method for extracting tripterygium glycosides, and product and inclusion compound and medicinal composition thereof |
| CN103610727A (en) * | 2013-11-26 | 2014-03-05 | 浙江得恩德制药有限公司 | Method for reducing organic solvent residue in tripterygium glycoside |
| CN103610727B (en) * | 2013-11-26 | 2015-12-30 | 浙江得恩德制药有限公司 | A kind of method reducing organic solvent residual in tripterygium glycosides |
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| Publication number | Publication date |
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| CN100387604C (en) | 2008-05-14 |
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Assignee: Shanghai Hua Yu Chinese Herbs Co., Ltd. Assignor: Shanghai Chinese Medicine Inst. Contract record no.: 2011310000002 Denomination of invention: Triptolide purification method Granted publication date: 20080514 License type: Exclusive License Open date: 20061213 Record date: 20110111 |