CN102617696B - Preparation method of asiaticoside - Google Patents
Preparation method of asiaticoside Download PDFInfo
- Publication number
- CN102617696B CN102617696B CN201210071147.0A CN201210071147A CN102617696B CN 102617696 B CN102617696 B CN 102617696B CN 201210071147 A CN201210071147 A CN 201210071147A CN 102617696 B CN102617696 B CN 102617696B
- Authority
- CN
- China
- Prior art keywords
- herba centellae
- total glycosides
- preparation
- centellae total
- aqueous ethanolic
- 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.)
- Active
Links
Landscapes
- Medicines Containing Plant Substances (AREA)
- Steroid Compounds (AREA)
Abstract
The invention discloses a preparation method of asiaticoside. The method comprises the following steps of: extracting a natural plant, i.e., asiatic centella serving as a raw material with water; adsorbing with macroporous resin; gradually eluting an ethanol aqueous solution; and decolorizing with active carbon to obtain high-yield and high-quality asiaticoside. The method is convenient to operate, and has extremely high yield, low cost and low pollution.
Description
Technical field
The invention belongs to Chinese medicinal plant bulk drug preparation technology, relate generally to a kind of method that extracts medicinal ingredients wherein taking Chinese medicinal plant as basic raw material, specially refer to the preparation method who extracts Herba Centellae total glycosides taking Herba Centellae as basic raw material.
Background technology
The conventional Chinese medicine that Herba Centellae [Centella asiatica (L.) Urban] is recorded for " Chinese Pharmacopoeia ", for the dry herb of umbelliferae Centella plant Herba Centellae, begin to be loaded in Shennong's Herbal, classify middle product as, there is effect of clearing heat and promoting diuresis, detoxify and promote the subsdence of swelling.
Herba Centellae total glycosides is to extract and separate the efficient part obtaining from the herb of Herba Centellae, contains multiple triterpene compound, mainly contains centella asiatica glucoside, asiaticoside and their homologue, and wherein the structural formula of centella asiatica glucoside, asiaticoside is as follows:
In the time that R1 is H, be centella asiatica glucoside, in the time that R1 is OH, be asiaticoside.Centella asiatica glucoside can effectively promote wound healing, asiaticoside to have anti-inflammatory and treatment rheumatic arthritis isoreactivity, is used for the treatment of clinically operation wound, burn, wound and keloid etc.
Summary of the invention
The object of the present invention is to provide a kind of processing condition to require simple, easy to operate, yield is high, with low cost, pollutes little Herba Centellae total glycosides preparation technology.Concrete operation method is:
A. Herba Centellae is thrown in extractor, with 20～25 times from the beginning moisture carry out micro-extraction of boiling for three times, each 2 hours, filter, united extraction liquid, concentrating under reduced pressure obtains concentrated solution.
B. concentrated solution is put into length-to-diameter ratio and be in the macroporous resin column of 2: 1～5: 1, then carry out gradient elution: first wash with water to effluent liquid water white transparency, use again 20% aqueous ethanolic solution wash-out to effluent liquid water white transparency, then use the aqueous ethanolic solution wash-out of 4 column volumes 75%, collect 75% ethanol water elution liquid, be evaporated to thick paste shape, add 5～8 times of 95% aqueous ethanolic solution at 70～80 DEG C, to make it dissolve, obtain lysate;
C. lysate is added to 10% gac, insulated and stirred decolouring 30min, filtered while hot, after filtrate decompression is concentrated, 80 ± 10 DEG C of heat-wind circulate dryings make Herba Centellae total glycosides.
The Herba Centellae total glycosides of preparation characterizes qualification by high performance liquid phase, consistent with the characterization data of 2010 editions European Pharmacopoeias, sees accompanying drawing 1, accompanying drawing 2.And by content and the extraction yield of high-efficient liquid phase chromatogram technique analysis Herba Centellae total glycosides.Wherein, the content of Herba Centellae total glycosides is 60-80%, more than the extraction rate reached to 90% of the total glycosides of asiaticoside.Efficient liquid phase chromatographic analysis condition used is: column length and model: Sapphire C 184.6 × 250mm, 5 μ m, column temperature: 30 DEG C, moving phase: acetonitrile-2mmol/L beta-cyclodextrin solution (24: 76), flow velocity: 1ml/min, detects wavelength: 205nm.
For fully extract the effective constituent of Herba Centellae in step a, the concentrated solution volume obtaining is 1L with the ratio of Herba Centellae weight: 1kg is advisable;
For fully adsorb the effective constituent of Herba Centellae in step b, in macroporous resin column, use the resin of nonpolar or low-pole as AB-8, HPD100, D101, its good separating effect, and can recycle, be convenient to industrialization and produce.
The present invention is taking natural phant Herba Centellae as starting raw material, and with water extraction, macroporous resin adsorption, aqueous ethanolic solution gradient elution, activated carbon decolorizing, can obtain high yield, high-quality Herba Centellae total glycosides.Tool of the present invention has the following advantages:
1, taking water as extracting solvent, cost is low, non-environmental-pollution;
2, taking macroporous resin as sorbent material, aqueous ethanolic solution is eluent, and cost is low, recoverable;
3, Herba Centellae total glycosides product yield is high, and quality is good, and production operation is simple.
Brief description of the drawings
Fig. 1 is Herba Centellae total glycosides high performance liquid phase spectrogram;
Fig. 2 is the data sheet that Herba Centellae total glycosides characterizes.
Embodiment
Below by embodiment, the present invention is further illustrated.
Embodiment 1
The present embodiment extracts the working method of Herba Centellae total glycosides to carry out according to following two steps:
The preparation of Herba Centellae total glycosides crude product: 0.5kg Herba Centellae is packed in 3L Erlenmeyer flask, add successively 4.5kg, 4kg, 4kg tap water, micro-lower each extraction 2 hours of boiling, united extraction liquid, is evaporated to 0.5L, injects the AB-8 macroporous resin column that 100g length-to-diameter ratio is 3: 1, first wash with water to colourless, use 20% aqueous ethanolic solution wash-out to colourless again, then use 4 column volumes, 75% aqueous ethanolic solution wash-out, flow velocity is 3BV/h.Collect 75% ethanol water elution liquid, be evaporated to thick paste shape, obtain Herba Centellae total glycosides crude product.
The preparation of Herba Centellae total glycosides finished product: after Herba Centellae total glycosides crude product is dissolved at 75 ± 5 DEG C with 5 times of 95% ethanol, add the processing of decolouring of 10% gac, filtered while hot.Gained filtrate decompression is concentrated, and 80 ± 10 DEG C obtain Herba Centellae total glycosides finished product for heat-wind circulate drying 4 ± 2h hour.
After testing, the content of Herba Centellae total glycosides is 77.14%, the extraction rate reached to 91.45% of the total glycosides of asiaticoside.
Embodiment 2
The present embodiment extracts the working method of Herba Centellae total glycosides to carry out according to following two steps:
The preparation of Herba Centellae total glycosides crude product: 0.5kg Herba Centellae is poured in 3L Erlenmeyer flask, add successively 4.5kg, 4kg, 4kg tap water, micro-lower each extraction 2 hours of boiling, united extraction liquid, is evaporated to 0.5L, injects the HPD100 macroporous resin column that 100g length-to-diameter ratio is 3: 1, first wash with water to colourless, use 20% aqueous ethanolic solution wash-out to colourless again, then use 4 column volumes, 75% aqueous ethanolic solution wash-out, flow velocity is 3BV/h.Collect 75% ethanol water elution liquid, be evaporated to thick paste shape, obtain Herba Centellae total glycosides crude product.
The preparation of Herba Centellae total glycosides finished product: after Herba Centellae total glycosides crude product is dissolved at 75 ± 5 DEG C with 5 times of 95% ethanol, add the processing of decolouring of 10% gac, filtered while hot.Gained filtrate decompression is concentrated, and 80 ± 10 DEG C obtain Herba Centellae total glycosides finished product for heat-wind circulate drying 4 ± 2h hour.
After testing, the content of Herba Centellae total glycosides is 76.32%, the extraction rate reached to 92.13% of the total glycosides of asiaticoside.
Embodiment 3
The preparation of Herba Centellae total glycosides crude product: 0.5kg Herba Centellae is poured in extractor, add successively 4.5kg, 4kg, 4kg tap water, micro-lower each extraction 2 hours of boiling, united extraction liquid, is evaporated to 0.5L, injects the D101 macroporous resin column that 100g length-to-diameter ratio is 3: 1, first wash with water to colourless, use 20% aqueous ethanolic solution wash-out to colourless again, then use 4 column volumes, 75% aqueous ethanolic solution wash-out, flow velocity is 3BV/h.Collect 75% ethanol water elution liquid, be evaporated to thick paste shape, obtain Herba Centellae total glycosides crude product.
The preparation of Herba Centellae total glycosides finished product: after Herba Centellae total glycosides crude product is dissolved at 75 ± 5 DEG C with 5 times of 95% ethanol, add the processing of decolouring of 10% gac, filtered while hot.Gained filtrate decompression is concentrated, and 80 ± 10 DEG C obtain Herba Centellae total glycosides finished product for heat-wind circulate drying 4 ± 2h hour.
After testing, the content of Herba Centellae total glycosides is 76.80%, the extraction rate reached to 91.50% of the total glycosides of asiaticoside.
Embodiment 4
The preparation of Herba Centellae total glycosides crude product: 10kg Herba Centellae is poured in extractor, add successively 90kg, 80kg, 80kg tap water, micro-lower each extraction 2 hours of boiling, united extraction liquid, is evaporated to 10L, injects the AB-8 macroporous resin column that 2000g length-to-diameter ratio is 3: 1, first wash with water to colourless, use 20% aqueous ethanolic solution wash-out to colourless again, then use 4 column volumes, 75% aqueous ethanolic solution wash-out, flow velocity is 3BV/h.Collect 75% ethanol water elution liquid, be evaporated to thick paste shape, obtain Herba Centellae total glycosides crude product.
The preparation of Herba Centellae total glycosides finished product: after Herba Centellae total glycosides crude product is dissolved at 75 ± 5 DEG C with 5 times of 95% ethanol, add the processing of decolouring of 10% gac, filtered while hot.Gained filtrate decompression is concentrated, and 80 ± 10 DEG C obtain Herba Centellae total glycosides finished product for heat-wind circulate drying 4 ± 2h hour.
After testing, the content of Herba Centellae total glycosides is 76.10%, the extraction rate reached to 92.16% of the total glycosides of asiaticoside.
Claims (2)
1. a preparation method for Herba Centellae total glycosides, is characterized in that, comprises the steps:
A. Herba Centellae is thrown in extractor, carry out micro-extraction of boiling for three times with the moisture from the beginning of 25 times of w/w, each 2 hours, filter, united extraction liquid, concentrating under reduced pressure obtains concentrated solution, and concentrated solution volume is 1L: 1kg with the ratio of Herba Centellae weight;
B. concentrated solution is put into length-to-diameter ratio and be in the macroporous resin column of 2: 1～5: 1, then carry out gradient elution: first wash with water to effluent liquid water white transparency, use again 20% aqueous ethanolic solution wash-out to effluent liquid water white transparency, then use the aqueous ethanolic solution wash-out of 4 column volumes 75%, collect 75% ethanol water elution liquid, be evaporated to thick paste shape, add 5～8 times of 95% aqueous ethanolic solution at 75 ± 5 DEG C, to make it dissolve, obtain lysate;
C. lysate is added to 10% gac, insulated and stirred decolouring 30min, filtered while hot, after filtrate decompression is concentrated, 80 ± 10 DEG C of heat-wind circulate dryings make Herba Centellae total glycosides.
2. the preparation method of a kind of Herba Centellae total glycosides according to claim 1, is characterized in that: wherein in the macroporous resin column described in step b, use AB-8, HPD100 or D101 resin.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210071147.0A CN102617696B (en) | 2012-03-16 | 2012-03-16 | Preparation method of asiaticoside |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210071147.0A CN102617696B (en) | 2012-03-16 | 2012-03-16 | Preparation method of asiaticoside |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102617696A CN102617696A (en) | 2012-08-01 |
| CN102617696B true CN102617696B (en) | 2014-10-22 |
Family
ID=46557947
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210071147.0A Active CN102617696B (en) | 2012-03-16 | 2012-03-16 | Preparation method of asiaticoside |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102617696B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104892719B (en) * | 2014-12-04 | 2016-09-21 | 陕西君碧莎制药有限公司 | A kind of preparation method of asiaticoside |
| CN104592341A (en) * | 2014-12-30 | 2015-05-06 | 广州白云山汉方现代药业有限公司 | Method for extracting asiaticoside and madecassoside from centella |
| CN110179841A (en) * | 2019-07-02 | 2019-08-30 | 江西青春康源制药有限公司 | A kind of industrial extraction method of high level of water soluble asiaticoside |
| CN115624514A (en) * | 2022-10-12 | 2023-01-20 | 杭州时光肌生物科技有限公司 | Preparation method of composite plant extract for improving facial redness |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1387868A (en) * | 2001-05-29 | 2003-01-01 | 中国人民解放军第二军医大学 | Prepn process and new use of general asiaticoside |
| CN101323637A (en) * | 2008-07-29 | 2008-12-17 | 卢照凯 | Asiaticoside and preparation thereof |
| CN101948501A (en) * | 2010-09-01 | 2011-01-19 | 桂林莱茵生物科技股份有限公司 | Preparation method of hydroxyl asiaticoside |
-
2012
- 2012-03-16 CN CN201210071147.0A patent/CN102617696B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1387868A (en) * | 2001-05-29 | 2003-01-01 | 中国人民解放军第二军医大学 | Prepn process and new use of general asiaticoside |
| CN101323637A (en) * | 2008-07-29 | 2008-12-17 | 卢照凯 | Asiaticoside and preparation thereof |
| CN101948501A (en) * | 2010-09-01 | 2011-01-19 | 桂林莱茵生物科技股份有限公司 | Preparation method of hydroxyl asiaticoside |
Non-Patent Citations (2)
| Title |
|---|
| 大孔树脂纯化积雪草总苷的工艺研究;黄怀鹏等;《中药材》;20080725;第31卷(第7期);1072-1075 * |
| 黄怀鹏等.大孔树脂纯化积雪草总苷的工艺研究.《中药材》.2008,第31卷(第7期),1072-1075. |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102617696A (en) | 2012-08-01 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104592341A (en) | Method for extracting asiaticoside and madecassoside from centella | |
| CN102617696B (en) | Preparation method of asiaticoside | |
| CN101982471B (en) | Technological process for extracting aucubin from fruits of eucommia ulmoides oliver | |
| CN102233013A (en) | Preparation method for total saponins of pulsatilla chinensis | |
| CN101524458A (en) | Extract of smilax glabra saponins and flavonoid and preparation method thereof | |
| CN102070683B (en) | Method for simultaneously preparing chemical reference substances of parishin, parishin B and parishin C | |
| CN104610401B (en) | A kind of method for extracting baicalin, baicalin and wogonin from Radix Scutellariae simultaneously | |
| CN103232515A (en) | Cyclocarya paliurus glucoside I preparation method | |
| CN102503996B (en) | Method for extracting active constituent from Swertia mussotii plant | |
| CN103242422A (en) | Method for extracting cyclocaric acid A from cyclocarya paliurus leaves | |
| CN103833805A (en) | Process for refining glycyrrhizinic acid in liquorice | |
| CN103951717B (en) | The method of benzoylpaeoniflorin and benzoyl lactone glucoside of Radix Paeoniae is prepared in a kind of extraction | |
| CN102895303A (en) | Resin purification method for extracting and separating total flavone of cyclocarya paliurus | |
| CN108743657A (en) | The preparation method of methods of glycosides in a kind of mussot swertia herb | |
| CN101974065A (en) | Method for extracting not less than 98% of oleanolic acid from glossy privet fruit | |
| CN102633860A (en) | Method for extracting ardisiacrispin A | |
| CN103819518A (en) | Preparation method for standardized extracts of eucommia ulmoides pinoresinol diglucoside | |
| CN102114063B (en) | Method for extracting and separating asiaticoside by countercurrent extraction combined with membrane separation | |
| CN102391330A (en) | Method for extracting liquiritin from liquorice | |
| CN101869605B (en) | Method for extracting and separating mulberry leaf flavone and alkaloid composite | |
| CN102234299A (en) | Separation method of hyperin | |
| CN108704007A (en) | A kind of preparation method of Radix Polygalae active ingredient | |
| CN1268512A (en) | Preparation method of scutellaria root extract | |
| CN105713006A (en) | Preparation method of oridonin | |
| CN108452069A (en) | A kind of method that microwave prepares paulownia root antineoplastic 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 | ||
| C53 | Correction of patent for invention or patent application | ||
| CB02 | Change of applicant information |
Address after: 510000 No. 663, Wenquan Avenue, Conghua hot spring town, Guangdong, Guangzhou Applicant after: Guangzhou Hanfang Pharmaceutical Co., Ltd. Address before: 510900 No. 663, Wenquan Avenue, Conghua hot spring town, Guangdong, Guangzhou Applicant before: Hanfang Modem Chinese Traditional Medicine Research Development Co., Ltd., Guang |
|
| COR | Change of bibliographic data |
Free format text: CORRECT: APPLICANT; FROM: HANFANG MODEM CHINESE TRADITIONAL MEDICINE RESEARCH DEVELOPMENT CO., LTD., GUANG TO: GUANGZHOU HANFANG PHARMACEUTICAL CO., LTD. |
|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |