CN1506365A - Prepn process of tripterygium extractive - Google Patents
Prepn process of tripterygium extractive Download PDFInfo
- Publication number
- CN1506365A CN1506365A CNA021551332A CN02155133A CN1506365A CN 1506365 A CN1506365 A CN 1506365A CN A021551332 A CNA021551332 A CN A021551332A CN 02155133 A CN02155133 A CN 02155133A CN 1506365 A CN1506365 A CN 1506365A
- Authority
- CN
- China
- Prior art keywords
- extraction
- trypterygine
- organic solvent
- ethanol
- crude extract
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Medicines Containing Plant Substances (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The present invention is the preparation process of tripterygium extractive. The preparation process includes low temperature dynamic countercurrent extraction of tripterygium material with organic solvent, decompressing concentration of the extracted liquid, extraction of the concentrated liquid with organic solvent, normal pressure recovering of organic solvent and vacuum drying to obtain coarse tripterygium extractive. The said process has short extraction period, reduced organic solvent throwing amount, low power consumption for recovering organic solvent, less damage to the effective components of tripterygium, high extraction rate of the effective components and high product quality.
Description
Technical field
The present invention relates to the preparation technology of Chinese medicinal materials extract, specifically a kind of preparation method of trypterygine crude extract.
Background technology
The Chinese medicinal materials trypterygine is the Celastraceae tripterygium plant, is used for the treatment of that kind of an immunological disease has significant curative effect surplus rheumatoid arthritis, chronic nephropathy, the lupus erythematosus etc. 30, and main component is the diterpenes component based on triptolide.The extraction process of prepared from active ingredients of tripterygium wilfordii has water extraction and alcohol precipitation method, alcohol extracting, ethyl acetate extraction method etc.Water extraction and alcohol precipitation method: the clean medicinal material of trypterygine decocts secondary with the tap water of about 25 times of medicinal material amounts, and the aqueous solution of gained adds alcohol after concentrating, and reclaims ethanol afterwards, uses chloroform extraction three times, and the extraction liquid vacuum is drained the crude extract that promptly gets trypterygine.This explained hereafter efficient is low, and the flow process complexity needs a large amount of equipment, and floor space is big, and energy consumption is big, extraction yield low (3-5 ‰), and operator at high temperature work the scald accident take place easily.Ethanol extraction method: the ethanol that the clean medicinal material of trypterygine adds about 10 times of medicinal material amounts comes diacolation, and percolate is used chloroform extraction three times after reclaiming ethanol, and extraction liquid is pumped into dry product after reclaiming chloroform.The shortcoming of this technology be alcoholic acid feed intake big and loss big, production efficiency extremely low (the diacolation process needs about 48 hours) is not suitable for scale operation.The ethyl acetate extraction method: the clean medicinal material of trypterygine soaks into ethanol or thermal backflow is extracted, extracting solution reclaims behind the ethanol with ethyl acetate extraction repeatedly, then the ethyl acetate in the extraction liquid is reclaimed, the concentrated solution chloroform extraction of gained, the chloroform extraction liquid of gained is pumped into medicinal extract after reclaiming chloroform.The trypterygine crude extract interest rate higher (about 12 ‰) that this technology is extracted, but composition is more assorted, thereby contained activity is also lower in the composition, is unfavorable for step mask work down.The common ground of above-mentioned three kinds of technologies is that the extraction time of prepared from active ingredients of tripterygium wilfordii is long, and production efficiency is low.
Summary of the invention
Technical problem to be solved by this invention is the defective that overcomes above-mentioned prior art, and the preparation method of a kind of extraction yield height, extraction time weak point, raw material less investment, energy consumption is little, floor space is little trypterygine crude extract is provided.
Technical scheme of the present invention is such: the preparation method of trypterygine crude extract, be characterized in that the clean medicinal material of trypterygine carries out dynamic countercurrent low temperature cover with organic solvent and carries, complete until extracts active ingredients, the extracting solution concentrating under reduced pressure, use the organic solvent extraction concentrated solution, the extraction liquid normal pressure vacuumizes into dry product after reclaiming organic solvent, promptly gets the crude extract of trypterygine.The used dynamic countercurrent extracting method of the present invention makes ethanol enter in the cell of medicinal material fast and dissolves effective constituent, reach balance rapidly, strengthened mass transfer power, shorten extraction time, reduce the input amount of organic solvent, reduce and reclaim the required energy consumption of organic solvent, reduced equipment, floor space is few.Extract at low temperature of the present invention has been avoided extracting solution, and long-time high temperature is to the destruction of prepared from active ingredients of tripterygium wilfordii in the decocting and concentrating process (water extraction and alcohol precipitation method), and the quality that has improved the extraction yield of prepared from active ingredients of tripterygium wilfordii and extract is good.
The preparation method of described trypterygine crude extract, organic solvent is methyl alcohol or ethanol.
The preparation method of described trypterygine crude extract, the step that dynamic countercurrent low temperature cover is carried is: be respectively charged into after wetting the clean medicinal material coarse powder of trypterygine in the extraction column of the closed polyphone of 4-12 root with ethanol, again medicinal material is pressurizeed for some time after taking the air in all extraction columns away or taking air away, impel ethanol rapid osmotic medicinal material, optional one is initial extraction column, feed ethanol, make ethanol under 0-50 ℃, carry out countercurrent extraction with recycle pump, the soup of gained enters successively in the closed with it extraction column of contacting and carried out same countercurrent extraction 20-50 minute, and effusive soup is as extracting solution behind 4 extraction columns of will flowing through at least; In the extraction column of initial extraction column back, add ethanol successively, repeat the aforesaid operations step, after the extraction fully, united extraction liquid.The discharging charging again more together of all extraction columns is carried out next round and is extracted.
The preparation method of described trypterygine crude extract, used alcohol concn is 40-80%, and its consumption is 1-4 a times of medicinal material amount, and the vacuum tightness during draws air is 0.06-0.09Mpa, and the pressure during pressurization is 0.02-0.03Mpa, be 10-30 minute clamping time.
The preparation method of described trypterygine crude extract, organic solvent is chloroform or methylene dichloride; The relative density of the concentrated solution that obtains is 1.00-1.10 (40 ℃).
The production comparison sheet of dynamic countercurrent extraction method of the present invention and water extract-alcohol precipitation extraction method (the medicinal material amount of input is 100kg):
| Classification | Water extraction and alcohol precipitation method | The present invention | |
| Plant area | ??100m 2(floor height 8m) | ??25m 2(floor height 8m) | |
| Energy consumption | Coal | 0.6 ton | 0.12 ton |
| Electricity | 121 degree | 35 degree | |
| Water | 5 tons | 1.1 ton (usefulness of mainly clearing out a gathering place) | |
| Solvent | Chloroform | Loss 8.2kg | Loss 8kg |
| 95% ethanol | Loss 40kg | Loss 23kg | |
| Extract yield | ????3-5‰ | ????9-13‰ | |
| Extraction time | About 48 hours | About 16-26 hour | |
The present invention compares with water extraction and alcohol precipitation method and has the following advantages: 1, extraction yield height, extraction time are short and quality extract is good, extraction yield is at 9-13 ‰, extraction time is 16-26 hour, thereby has improved production efficiency 2, starting material less investment loss is little, the ethanol consumption be dose 2-5 doubly; 3, needn't carry out decoction and vaporize water solution process in the water extract-alcohol precipitation extraction method, cut down the consumption of energy significantly; 4, simplify technical process, thereby reduced use equipment and floor space; 5, improved work situation, avoided under high-temperature, working and the scald accident that takes place.
Embodiment
Embodiment 1
The clean medicinal material coarse powder 420kg of trypterygine stirs with 80% ethanol, it is moistening fully that medicinal material is obtained, medicinal material after moistening is packed in the extraction column, and airtight extraction column is opened vacuum pump and is extracted air in the extraction column, vacuum degree control is at 0.08Mpa, feed an amount of ethanol medicinal material just is submerged, logical afterwards pressurized with compressed air 10 minutes is pressed to being 0.02Mpa, carry out dynamic countercurrent low temperature cover then and propose operation, extract temperature at 25 ℃.
The device that used dynamic countercurrent low temperature cover is carried is the extraction column of 6 closed polyphones.In the 1st extraction column, add 80% ethanol 110kg, the ON cycle pump, allow ethanol pass medicinal material from bottom to top and carry out countercurrent extraction, required time is 40 minutes, the soup of emitting enters the 2nd extraction column and carries out countercurrent extraction up to the 5th post, from the 5th effusive soup of post as No. the 1st extracting solution; In the 2nd extraction column, add ethanol 110kg, allow ethanol pass medicinal material from bottom to top and carry out countercurrent extraction, required time is 40 minutes, and the soup of emitting enters the 3rd extraction column and carries out countercurrent extraction up to the 6th post, from the 6th effusive soup of post as No. the 2nd extracting solution; In the 3rd extraction column, add ethanol 110kg, allow ethanol pass medicinal material from bottom to top and carry out countercurrent extraction, required time is 40 minutes, the soup of emitting enters the 4th, 5,6 extraction column successively and carries out countercurrent extraction, enter the 1st post again from the 6th effusive soup of post, from the 1st effusive soup of extraction column as No. the 3rd extracting solution; In the 4th extraction column, add ethanol 110kg, allow ethanol pass medicinal material from bottom to top and carry out countercurrent extraction, required time is 40 minutes, the soup of emitting enters the 5th, 6 extraction column successively and carries out countercurrent extraction, enter the 1st, 2 post again from the 6th effusive soup of post, from the 2nd effusive soup of extraction column as the 4th extracting solution; In the 5th extraction column, add ethanol 110kg, allow ethanol pass medicinal material from bottom to top and carry out countercurrent extraction, required time is 40 minutes, the soup of emitting enters the 6th extraction column successively and carries out countercurrent extraction, effusive soup enters the 1st, 2,3 post again, from the 3rd effusive soup of extraction column as the 5th extracting solution; In the 6th extraction column, add ethanol 110kg, allow ethanol pass medicinal material from bottom to top and carry out countercurrent extraction, required time is 40 minutes, and the soup of emitting enters the 1st, 2,3,4 post again, as No. the 6th extracting solution, merge the extracting solution of gained from the 4th effusive soup of extraction column.5 extraction columns of flowing through after so each ethanol adds flow out as extracting solution, and 6 extraction columns have all carried out five times and extracted, and have just finished a wheel operation, and the time of finishing 6 posts is 22.5 hours.The discharging charging again more together of all extraction columns is carried out next round and is extracted.
Determine to extract whether fully with the leaching yield of thin layer chromatography, the refractive index of surveying extracting solution or medicinal material, extracting solution after merging is carried out underpressure distillation, and (vapor pressure is 0.15Mpa, vacuum tightness is at 0.08Mpa), reclaim ethanol, the relative density of the concentrated solution of gained is 1.04 (40 ℃).Concentrated solution shifts three times with chloroform extraction in extraction kettle, and extraction liquid reclaims chloroform under normal pressure, vacuumize into loose, the dried shape dry product of foam afterwards, is the crude extract of trypterygine, and extract yield is 10.8 ‰.
Embodiment 2
Embodiment 2 is that with the difference of embodiment 1 time of pressurizeing is 30 minutes, and extracting the used time is 50 minutes, extracts temperature at 30 ℃, used organic solvent is a methyl alcohol, its total consumption is 840kg, and used extraction agent is a methylene dichloride, and extract yield is 12.6 ‰.
Embodiment 3
Embodiment 3 is that with the difference of embodiment 1 used extraction column is 12, and the medicinal material amount of adding is 840kg, and used alcohol concn is 60%, and total consumption is 1680kg, 11 extraction columns of flowing through after each ethanol adds, and extract yield is 11.5 ‰.
Claims (5)
1, the preparation method of trypterygine crude extract, it is characterized in that the clean medicinal material coarse powder of trypterygine is carried out dynamic countercurrent low temperature cover with organic solvent to be carried, complete until extracts active ingredients, the extracting solution concentrating under reduced pressure, use the organic solvent extraction concentrated solution, extraction liquid vacuumizes into dry product after reclaiming organic solvent, is the trypterygine crude extract.
2, the preparation method of trypterygine crude extract according to claim 1 is characterized in that described organic solvent is methyl alcohol or ethanol.
3, the preparation method of trypterygine crude extract according to claim 2, it is characterized in that the step that described dynamic countercurrent low temperature cover is carried is: be respectively charged into after wetting the clean medicinal material coarse powder of trypterygine in the extraction column of the closed polyphone of 4-12 root with ethanol, again medicinal material is pressurizeed for some time after taking the air in all extraction columns away or taking air away, optional one is initial extraction column, feed ethanol, with recycle pump ethanol was carried out countercurrent extraction 20-50 minute under 0-50 ℃, the soup of gained enters successively in the closed with it extraction column of contacting and carries out same countercurrent extraction, and effusive soup is as extracting solution behind 4 extraction columns of will flowing through at least; Add ethanol at the extraction column that is positioned at initial extraction column back successively, repeat the aforesaid operations step, after the extraction fully, united extraction liquid.
4, the preparation method of trypterygine crude extract according to claim 3, it is characterized in that described alcohol concn is 40-80%, its consumption is 1-4 a times of medicinal material amount, vacuum tightness during draws air is 0.06-0.09Mpa, pressure during pressurization is 0.02-0.03Mpa, and be 10-30 minute clamping time.
5, the preparation method of trypterygine crude extract according to claim 4 is characterized in that described organic solvent is chloroform or methylene dichloride, and the relative density of described concentrated solution is 1.00-1.10 (40 ℃).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02155133 CN1250552C (en) | 2002-12-10 | 2002-12-10 | Prepn process of tripterygium extractive |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02155133 CN1250552C (en) | 2002-12-10 | 2002-12-10 | Prepn process of tripterygium extractive |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1506365A true CN1506365A (en) | 2004-06-23 |
| CN1250552C CN1250552C (en) | 2006-04-12 |
Family
ID=34235739
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 02155133 Expired - Lifetime CN1250552C (en) | 2002-12-10 | 2002-12-10 | Prepn process of tripterygium extractive |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1250552C (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102008536A (en) * | 2010-12-02 | 2011-04-13 | 吴江迪星科技有限公司 | Tripterygium wilfordii hook extract cataplasm and preparation method thereof |
| CN103041614A (en) * | 2012-11-30 | 2013-04-17 | 广东医学院 | Device and method for extracting and concentrating traditional Chinese medicine |
| CN103242414A (en) * | 2013-05-17 | 2013-08-14 | 成都彼斯特生物科技有限公司 | Method for separating and purifying tripterine from medicinal material celastrus orbiculatus |
| CN103919835A (en) * | 2014-03-25 | 2014-07-16 | 浙江中医药大学 | Method for preparing tripterygium wilfordii extract by using triterpenes as main components and pharmaceutical application of tripterygium wilfordii extract |
| CN115894602A (en) * | 2022-12-24 | 2023-04-04 | 浙江得恩德制药股份有限公司 | Extraction of triptolide from tripterygium wilfordii |
-
2002
- 2002-12-10 CN CN 02155133 patent/CN1250552C/en not_active Expired - Lifetime
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102008536A (en) * | 2010-12-02 | 2011-04-13 | 吴江迪星科技有限公司 | Tripterygium wilfordii hook extract cataplasm and preparation method thereof |
| CN102008536B (en) * | 2010-12-02 | 2012-05-23 | 吴江迪星科技有限公司 | Tripterygium wilfordii hook extract cataplasm and preparation method thereof |
| CN103041614A (en) * | 2012-11-30 | 2013-04-17 | 广东医学院 | Device and method for extracting and concentrating traditional Chinese medicine |
| CN103242414A (en) * | 2013-05-17 | 2013-08-14 | 成都彼斯特生物科技有限公司 | Method for separating and purifying tripterine from medicinal material celastrus orbiculatus |
| CN103242414B (en) * | 2013-05-17 | 2015-09-30 | 成都彼斯特生物科技有限公司 | A kind of method from Stem of Oriental Bittersweet medicinal material separation and purification Tripterine |
| CN103919835A (en) * | 2014-03-25 | 2014-07-16 | 浙江中医药大学 | Method for preparing tripterygium wilfordii extract by using triterpenes as main components and pharmaceutical application of tripterygium wilfordii extract |
| CN103919835B (en) * | 2014-03-25 | 2017-06-27 | 浙江中医药大学 | The preparation method and its pharmaceutical applications of the triperygium wilfordii extractive with triterpenes as main component |
| CN115894602A (en) * | 2022-12-24 | 2023-04-04 | 浙江得恩德制药股份有限公司 | Extraction of triptolide from tripterygium wilfordii |
| CN115894602B (en) * | 2022-12-24 | 2024-05-14 | 浙江得恩德制药股份有限公司 | Extraction of triptolide from Tripterygium wilfordii |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1250552C (en) | 2006-04-12 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101810658B (en) | Method for removing residual pesticide from ginseng | |
| CN104628739A (en) | Extraction technology of artemisinin | |
| CN109320431A (en) | A method of N-METHYLFORMAMIDE and diethylene glycol monomethyl ether in recycling paint stripper waste liquid | |
| CN1250552C (en) | Prepn process of tripterygium extractive | |
| CN102443036A (en) | Method for purifying asiatic acid in asiatic pennywort herb | |
| CN102000445B (en) | Process for producing pyrethrum through subcritical continuous extraction | |
| CN103215073A (en) | Production method for extracting lignite wax from brown coal | |
| CN101982471A (en) | Technological process for extracting aucubin from fruits of eucommia ulmoides oliver | |
| CN100509829C (en) | Producing process of icariin | |
| CN103497170A (en) | Method for extracting procyanidine in receptaculum nelumbinis in full low temperature process | |
| CN105348334B (en) | A kind of method for extracting day sesame oil and Gastrodin simultaneously from rhizoma Gastrodiae | |
| CN100410258C (en) | New super critical CO2 extraction process | |
| CN101375975A (en) | Novel method for preparing grape seed extract | |
| CN102091107B (en) | Method for extracting total triterpene of centella asiatica by enzymic process | |
| CN102911150B (en) | Process for preparing oligomeric proantho cyanidins by peanut skin | |
| CN102389510A (en) | Dioscorea nipponica Makino saponin extraction method | |
| CN107903296A (en) | The extracting method of madecassoside | |
| CN209173420U (en) | A kind of recyclable device for paint stripper waste liquid | |
| CN112608312A (en) | Optimized process for supercritical extraction of matrine | |
| CN101244159A (en) | Novel method for preparing vine seed extract | |
| CN1450061A (en) | Process for extracting Isofraxidin | |
| CN101138389B (en) | Method of comprehensive utilization of waste liquor produced in the refining process of puerarin | |
| CN104031102A (en) | Method for extracting shanzhiside methyl ester from phlomis umbrosa | |
| CN110179841A (en) | A kind of industrial extraction method of high level of water soluble asiaticoside | |
| CN109646491A (en) | A kind of extracting method of spire banyan dry extract, pithecellobium clypearia dry extract |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CP01 | Change in the name or title of a patent holder | ||
| CP01 | Change in the name or title of a patent holder |
Address after: 312560 No. 2 National Road East, Xinchang, Zhejiang Patentee after: ZHEJIANG DND PHARMACEUTICAL CO.,LTD. Address before: 312560 No. 2 National Road East, Xinchang, Zhejiang Patentee before: ZHEJIANG DND PHARMACEUTICAL CO.,LTD. |
|
| CX01 | Expiry of patent term | ||
| CX01 | Expiry of patent term |
Granted publication date: 20060412 |