CN102603854A - Method for extracting asiaticoside from asiatic pennywort herb - Google Patents
Method for extracting asiaticoside from asiatic pennywort herb Download PDFInfo
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- CN102603854A CN102603854A CN2011100262176A CN201110026217A CN102603854A CN 102603854 A CN102603854 A CN 102603854A CN 2011100262176 A CN2011100262176 A CN 2011100262176A CN 201110026217 A CN201110026217 A CN 201110026217A CN 102603854 A CN102603854 A CN 102603854A
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Abstract
The invention relates to a method for extracting asiaticoside from asiatic pennywort herb. The method comprises the following steps of: slicing an asiatic pennywort herb raw material; adding 15-20 times of acid water for percolating and extracting; filtering an extracting solution, and adding into an ultrafiltration system for performing ultrafiltration; adding a permeate liquid into a nanofiltration membrane system for performing nanofiltration; collecting a concentrated solution, adding water for saturating, and extracting by n-butyl alcohol for 2-3 times; adding active carbon into an extraction liquid, preserving heat at the temperature of 80 DEG C, and decolorizing; adding an appropriate amount of ethyl acetate into a decolorized liquid; standing for crystalizing; and drying a crystal to obtain a product. The method for producing asiaticoside has low energy consumption and low pollution; and an obtained product has high content, and the method is suitable for industrial production.
Description
Technical field:
The present invention relates to a kind of method of from Herba Centellae, extracting Centella Selected Triterpenes, especially a kind of method that adopts membrane separation technique to extract Centella Selected Triterpenes.
Background technology:
Herba Centellae is dry herb or the whole herb with root of dicotyledons umbelliferae Umbelliferae Herba Centellae Centella asiatica (L.) Urban.It has clearing heat and detoxicating, and is inducing diuresis and reducing edema.Be Oriental's long-lived medicine, can refresh oneself by beneficial brain.Research show have nourishing, anti-inflammatory, healing wound, diuresis defaecation and calm effect.Also effective in cure to leprosy, ulcer, blood purification and immunizing power there are activation, because of it can stimulate the replacement of deep skin cell.It is neural nourishing agent, and the ability memory alleviates mental fatigue: also can be hypotensive, and treatment hepatopathy etc.
Centella Selected Triterpenes is the Herba Centellae pharmaceutical compound, is the triterpenes saponin(e, is amorphous pale yellow powder, and bitter has and draws moistly, in water, ethanol, be prone to dissolve, with ether, chloroform in insoluble, the wound healing of promotion effect is arranged.Centella Selected Triterpenes is used to treat wound, operation wound, and burn, keloid and scleroderma etc., Recent study is found also antitumor with regard to having, the antioxygenation of Centella Selected Triterpenes.Accumulated snow saponin(e staple is centella asiatica glucoside, terminoloside and asiaticoside, and molecular weight is between 800-1000.
It is existing that from Herba Centellae, to extract the Centella Selected Triterpenes method more, as:
Patent " purposes of Total Of Triterpenes depression ", this patent disclosed method are methyl alcohol or the aqueous ethanolic solution immersion Herba Centellaes with 5%～95%, freezing extracting solution; Filtration under diminished pressure is removed throw out, gets filtrate decompression and concentrates the adsorptive macroporous resin adsorption; The zero(ppm) water wash-out is removed impurity; Again with 5%～95% methyl alcohol or aqueous ethanolic solution wash-out, obtain the elutriant concentrating under reduced pressure and dissolve thick thing, the ETHYLE ACETATE crystallization to the methyl alcohol or the aqueous ethanolic solution of thick thing 5%～95%; Be evaporated to driedly, obtain settled powder grass general glycoside.
Patent " method of the NSC 166063 extract of asiaticoside and terminoloside is rich in preparation "; This patent disclosed method is the over-ground part through alcohol property solvent extraction NSC 166063, and alcoholic solution is through resin anion(R.A), and the elutriant that obtains extracts through liquid/liquid and carries out the selectivity degreasing; The water of condensed skimmed-pure phase; And continuous filtration obtains water, and water is continuously through resin cation(R.C.), and passes through resin anion(R.A) subsequently; Stablize the water that obtains through adding alcohol, and obtain comprising the miscellany of asiaticoside, terminoloside and Centella Selected Triterpenes.
Patent " water soluble extract and the separation method thereof of the centella asiatica glucoside of self asiatic and the centella asiatica glucoside of hydroxyl and carboxyl centella asiatica glucoside ", this patent disclosed method are that aqueous alcohol solutions is extracted, and obtain extract solution, then, it are handled with halide solvent.Extract its water layer with higher alcohols.Then use buck, wash the extract in the alcohol layer several times with moisture then, vacuum concentration is used the ETHYLE ACETATE crystallization.
Patent " process for extracting of asiatic centella total saponins and the application in field of medicaments thereof ", this patent disclosed method are to take by weighing the Herba Centellae herb, and the ethanol of adding 40%～80% extracts in the ultrasonic extraction device; With extracting solution concentrate liquid concentrator: utilize cavitation suspension extraction equipment to use earlier chloroform extraction again; The part of fetching water is used ethyl acetate extraction again, and water intaking part is again used at last n-butanol extraction, gets propyl carbinol and partly carries out reduced-pressure backflow; Drying promptly obtains asiatic centella total saponins.
Patent " a kind of Asiaticoside and preparation method thereof "; This patent disclosed method is to be raw material with the Herba Centellae; Water or low-carbon alcohol are extracted, and what extracting solution made through column chromatographic isolation and purification, resin decolorization, crystallization, recrystallization, drying is the extract of staple with the Asiaticoside.
Patent " a kind of method of utilizing macroporous adsorbent resin to prepare asiatic centella total saponins "; The open method of this patent is: 1) add aqueous ethanolic solution in the Herba Centellae hay and soak, extract; Extracting solution merges, and concentrating under reduced pressure is removed ethanol, and liquid concentrator dilute with water after-filtration gets the asiatic centella total saponins aqueous solution; 2) the pretreated macroporous adsorbent resin of in chromatography column, packing into; 3) the total saponins aqueous solution is crossed resin column, and total saponins penetrates to the effluent; 4) use the water washing resin post, then with organic solvent-water mixed flow phase wash-out, elutriant merges behind thin-layer chromatographic analysis, gets the total saponins product through concentrated, crystallization, vacuum-drying again.
As stated, mostly existing technology is to adopt ethanol-extracted, macroporous resin purification or the extraction of multiple organic reagent, and energy consumption is high, and is seriously polluted, do not meet current yield-power demand for development.
Summary of the invention:
The technical problem that the present invention will solve provides a kind of method of from Herba Centellae, extracting Centella Selected Triterpenes, and it is low that this method adopts membrane sepn to cut down the consumption of energy, less pollution.
In order to solve the problems of the technologies described above, technical scheme of the present invention is following:
A kind of method of from Herba Centellae, extracting Centella Selected Triterpenes is characterized in that this method comprises the following steps: a Herba Centellae raw material section, adds 15-20 and doubly measures the extraction of sour water diacolation; Extracting solution filters and adds the ultrafiltration membrane system ultrafiltration, sees through liquid and adds the nanofiltration of nf membrane system again, collects liquid concentrator and adds water-saturated n-butanol extraction 2-3 time; Extraction liquid adds 80 ℃ of insulation decolourings of gac; Destainer adds an amount of ETHYLE ACETATE, places crystallization, and crystallisate is drying to obtain product.
Described sour water is hydrochloric acid or the aqueous sulfuric acid of pH3-4.
Optional tubular type of described ultra-filtration membrane or hollow organic membrane, molecular weight cut-off 3000-10000.
Optional tubular type of described nf membrane or hollow organic membrane, molecular weight cut-off is not more than 600.
The present invention adopts the sour water soaking and extracting, and energy consumption is low, reduces the stripping of flavonoid and fat-soluble component simultaneously; Ultra-filtration membrane and nf membrane are filtered; The sour water mother liquor reaches can do extraction solution again through liquid, and technology has been accomplished recycle, has reduced pollution and has reduced energy consumption.
The present invention adopts n-butanol extraction ETHYLE ACETATE crystallization method, and than adopting ethyl acetate extraction to adopt n-butanol extraction simple to operate more earlier, the product content that obtains is higher, to have reduced the consumption of ETHYLE ACETATE, has reduced production cost.
To combine embodiment to further specify the present invention below, but the scope that the present invention requires to protect is not limited to following embodiment.
Embodiment:
Embodiment 1:
10kg is got in the section of Herba Centellae raw material, and the sulfuric acid water diacolation that adds 20 times of amount pH4 extracts diacolation 24 hours; Extracting solution filters the hollow cellulose ultrafiltration membrane system ultrafiltration that adds molecular weight cut-off 3000, intake pressure control 0.5-0.8mpa, and normal temperature filters, and adds the suitable quantity of water dialysis; See through liquid and add the nanofiltration of molecular weight cut-off 600 hollow cellulose nf membrane systems again, collect liquid concentrator and add water-saturated n-butanol extraction 2 times, extraction liquid adds 80 ℃ of insulation decolourings of 1% gac, destainer filtering gac; Add an amount of ETHYLE ACETATE to there being deposition to separate out, place crystallization, the crystallisate drying under reduced pressure; Get the Herba Centellae product, content 93.1%, yield 85.2%.
Embodiment 2:
10kg is got in the section of Herba Centellae raw material, and the salt sour water diacolation that adds 20 times of amount pH3 extracts diacolation 16 hours; Extracting solution filters the hollow cellulose ultrafiltration membrane system ultrafiltration that adds molecular weight cut-off 3000, intake pressure control 0.5-0.8mpa, and normal temperature filters, and adds the suitable quantity of water dialysis; See through liquid and add the nanofiltration of molecular weight cut-off 600 hollow cellulose nf membrane systems again, collect liquid concentrator and add water-saturated n-butanol extraction 3 times, extraction liquid adds 80 ℃ of insulation decolourings of 2% gac, destainer filtering gac; Add an amount of ETHYLE ACETATE to there being deposition to separate out, place crystallization, the crystallisate drying under reduced pressure; Get the Herba Centellae product, content 94.6%, yield 83.2%.
Embodiment 3:
10kg is got in the section of Herba Centellae raw material, and the salt sour water diacolation that adds 20 times of amount pH4 extracts diacolation 20 hours; Extracting solution filters the hollow cellulose ultrafiltration membrane system ultrafiltration that adds molecular weight cut-off 6000, intake pressure control 0.4-6mpa, and normal temperature filters, and adds the suitable quantity of water dialysis; See through liquid and add the nanofiltration of molecular weight cut-off 600 hollow cellulose nf membrane systems again, collect liquid concentrator and add water-saturated n-butanol extraction 2 times, extraction liquid adds 80 ℃ of insulation decolourings of 0.5% gac, destainer filtering gac; Add an amount of ETHYLE ACETATE to there being deposition to separate out, place crystallization, the crystallisate drying under reduced pressure; Get the Herba Centellae product, content 90.7%, yield 87.3%.
Claims (4)
1. a method of from Herba Centellae, extracting Centella Selected Triterpenes is characterized in that this method comprises the following steps: a Herba Centellae raw material section, adds 15-20 and doubly measures the extraction of sour water diacolation; Extracting solution filters and adds the ultrafiltration membrane system ultrafiltration, sees through liquid and adds the nanofiltration of nf membrane system again, collects liquid concentrator and adds water-saturated n-butanol extraction 2-3 time; Extraction liquid adds 80 ℃ of insulation decolourings of gac; Destainer adds an amount of ETHYLE ACETATE, places crystallization, and crystallisate is drying to obtain product.
2. the method for from Herba Centellae, extracting Centella Selected Triterpenes as claimed in claim 1 is characterized in that described sour water is hydrochloric acid or the aqueous sulfuric acid of pH3-4.
3. the method for from Herba Centellae, extracting Centella Selected Triterpenes as claimed in claim 1 is characterized in that optional tubular type of described ultra-filtration membrane or hollow organic membrane, molecular weight cut-off 3000-10000.
4. the method for from Herba Centellae, extracting Centella Selected Triterpenes as claimed in claim 1 is characterized in that optional tubular type of described nf membrane or hollow organic membrane, and molecular weight cut-off is not more than 600.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2011100262176A CN102603854A (en) | 2011-01-25 | 2011-01-25 | Method for extracting asiaticoside from asiatic pennywort herb |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2011100262176A CN102603854A (en) | 2011-01-25 | 2011-01-25 | Method for extracting asiaticoside from asiatic pennywort herb |
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| CN102603854A true CN102603854A (en) | 2012-07-25 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106366152A (en) * | 2016-08-25 | 2017-02-01 | 桂林益天成生物科技有限公司 | Method of extracting asiaticoside from centella asiatica |
| CN107098947A (en) * | 2017-04-28 | 2017-08-29 | 南宁馨艺荣生物科技有限公司 | A kind of technique that Asiaticoside is extracted from centella |
| CN114014904A (en) * | 2021-11-19 | 2022-02-08 | 湘南学院 | Method for rapidly preparing high-content asiaticoside from asiatic pennywort herb raw material |
Citations (6)
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| US3366669A (en) * | 1963-08-28 | 1968-01-30 | Ratsimamanga Albert Rakoto | Hemisuccinates and salts of the hemisuccinates of asiatic acid |
| CA2164050C (en) * | 1994-12-20 | 2005-02-08 | Suk Hyung Cho | Cosmetic compositions containing betulinic acid |
| EP1569672A1 (en) * | 2002-12-10 | 2005-09-07 | Bayer Consumer Care AG | Method for preparing a centella asiatica extract rich in madecassoside and in terminoloside |
| CN1990500A (en) * | 2005-12-30 | 2007-07-04 | 杨光 | Liver-fibrosis-resistant asiatic centella triterpenoid saponin and its preparation process |
| CN101200487A (en) * | 2007-11-27 | 2008-06-18 | 浙江大学 | Method for preparing asiatic centella total saponins by using macroporous adsorption resin |
| CN101323637A (en) * | 2008-07-29 | 2008-12-17 | 卢照凯 | Asiaticoside and preparation thereof |
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2011
- 2011-01-25 CN CN2011100262176A patent/CN102603854A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3366669A (en) * | 1963-08-28 | 1968-01-30 | Ratsimamanga Albert Rakoto | Hemisuccinates and salts of the hemisuccinates of asiatic acid |
| CA2164050C (en) * | 1994-12-20 | 2005-02-08 | Suk Hyung Cho | Cosmetic compositions containing betulinic acid |
| EP1569672A1 (en) * | 2002-12-10 | 2005-09-07 | Bayer Consumer Care AG | Method for preparing a centella asiatica extract rich in madecassoside and in terminoloside |
| EP1569672B1 (en) * | 2002-12-10 | 2009-08-19 | Bayer Consumer Care AG | Use of a centella asiatica extract rich in madecassoside and in terminoloside |
| CN1990500A (en) * | 2005-12-30 | 2007-07-04 | 杨光 | Liver-fibrosis-resistant asiatic centella triterpenoid saponin and its preparation process |
| CN101200487A (en) * | 2007-11-27 | 2008-06-18 | 浙江大学 | Method for preparing asiatic centella total saponins by using macroporous adsorption resin |
| CN101323637A (en) * | 2008-07-29 | 2008-12-17 | 卢照凯 | Asiaticoside and preparation thereof |
Non-Patent Citations (2)
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| 《南京工业大学学报（自然科学版）》 20090531 韩伟等 "酶法提取积雪草苷" 第18-22页 第31卷, 第3期 * |
| 韩伟等: ""酶法提取积雪草苷"", 《南京工业大学学报（自然科学版）》, vol. 31, no. 3, 31 May 2009 (2009-05-31), pages 18 - 22 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106366152A (en) * | 2016-08-25 | 2017-02-01 | 桂林益天成生物科技有限公司 | Method of extracting asiaticoside from centella asiatica |
| CN106366152B (en) * | 2016-08-25 | 2018-01-19 | 桂林益天成生物科技有限公司 | The method that asiaticosid is extracted from centella |
| CN107098947A (en) * | 2017-04-28 | 2017-08-29 | 南宁馨艺荣生物科技有限公司 | A kind of technique that Asiaticoside is extracted from centella |
| CN114014904A (en) * | 2021-11-19 | 2022-02-08 | 湘南学院 | Method for rapidly preparing high-content asiaticoside from asiatic pennywort herb raw material |
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Application publication date: 20120725 |