Method for extracting asiaticoside and madecassoside from centella

A technology of madecassoside and asiaticoside, which is applied in the field of extraction and separation of medicinal active ingredients, can solve the problems of high cost, complicated process, and complicated operation, and achieve low cost, simple process, and strong operability Effect

Inactive Publication Date: 2015-05-06
GUANGZHOU HANFANG PHARMA
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  • Description
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Problems solved by technology

[0003] At present, there are not many methods for simultaneously preparing high-purity asiaticoside and madecassoside from Centella asiatica. Patent CN 102477063 discloses a preparation-type high-efficiency A method for separating asiaticoside B and madecassoside in centella asiatica extract by liquid chromatography, adding cyclodextrin to the mobile phase, and then extracting with an organic solvent to remove the cyclodextrin in the solvent to obtain a pure product , the method is complex in operation, high in cost, and difficult for industrial production
Patent CN 102532244 A discloses a method for preparing high-purity asiaticoside. The pure product of asiaticoside is obtained through extraction, decolorization and recrystallization. Extraction, the amount of organic solvent is large, which is easy to cause secondary pollution
Patent CN 101948501 A discloses a preparation method of madecassoside. The extract is subjected to macroporous resin column layer, activated carbon decolorization, crystallization, and macroporous resin chromatography to finally obtain madecassoside with a purity of more than 98%. , the process cycle is long, the process is complicated, and the cost is high

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  • Method for extracting asiaticoside and madecassoside from centella

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Preparation of the crude product of Centella asiatica: 500g of Centella asiatica is pulverized, and in the extraction tank, add 70% ethanol (v / v) of 10 times the weight of the raw material for microboiling and reflux extraction, extract for the first time for 120min, filter out the medicinal liquid, Then add 70% ethanol (v / v) of 10 times the weight of raw materials, reflux extraction for 60min, and combine the extracts;

[0026] The extract was concentrated under reduced pressure to a density of 1.05 g / ml, diluted with 4 times of water, and centrifuged to obtain the upper column solution a, which was put into a D101 macroporous resin column, washed with water until the eluate was nearly colorless, and then used for 3 columns with a volume of 20 % ethanol (v / v) and 4 column volumes of 50% ethanol (v / v) were eluted, the 50% ethanol (v / v) eluate was collected, concentrated under reduced pressure to a density of 1.03 g / ml, and 3% activated carbon was added Decolorize, and f...

Embodiment 2

[0030] Preparation of the crude product of Centella asiaticoside: 500g of Centella asiatica is pulverized, and in the extraction tank, add 70% ethanol (v / v) of 12 times the weight of the raw material for microboiling and reflux extraction, extract for the first time for 90min, filter out the medicinal liquid, Then add 70% ethanol (v / v) of 10 times the weight of raw materials, reflux extraction for 90min, and combine the extracts;

[0031] The extract was concentrated under reduced pressure to a density of 1.10 g / ml, diluted with 6 times of water, and centrifuged to obtain the upper column solution a, which was put into a D130 macroporous resin column, washed with water until the eluent was nearly colorless, and then used for 4 columns with a volume of 20 % ethanol (v / v) and 5 column volumes of 50% ethanol (v / v) were eluted, the 50% ethanol (v / v) eluate was collected, concentrated under reduced pressure to a density of 1.04 g / ml, and 3% activated carbon was added Decolorize, an...

Embodiment 3

[0035] Preparation of the crude product of Centella asiatica: 500g of Centella asiatica is pulverized, and in the extraction tank, add 70% ethanol (v / v) of 10 times the weight of the raw material for microboiling and reflux extraction, extract for the first time for 120min, filter out the medicinal liquid, Then add 70% ethanol (v / v) of 8 times the weight of raw materials, reflux extraction for 60min, and combine the extracts;

[0036] The extract was concentrated under reduced pressure to a density of 1.15 g / ml, diluted with 8 times of water, and centrifuged to obtain the upper column liquid a, which was put into a D101 macroporous resin column, washed with water until the eluate was nearly colorless, and then used for 3 columns with a volume of 20 % ethanol (v / v) and 5 column volumes of 60% ethanol (v / v) were eluted, the 60% ethanol (v / v) eluate was collected, concentrated under reduced pressure to a density of 1.05 g / ml, and 3% activated carbon was added Decolorize, and filt...

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Abstract

The invention discloses a method for extracting asiaticoside and madecassoside from centella. The method comprises the following operation steps: (1) adding a 50%-90% ethanol solution (v / v) into dry centella, extracting, after filtering an extracting solution, carrying out reduced pressure concentration to remove ethanol, adding water to dilute concentrated liquid, and carrying out centrifugal filtration to obtain a centella total saponin water solution; (2) filtering the centella total saponin water solution by virtue of a resin column, respectively washing the resin column by virtue of water, 15%-30% ethanol (v / v) and 50%-80% ethanol (v / v), and fractionally collecting eluant; and (3) concentrating eluant of 50%-80% ethanol (v / v), adding activated carbon, carrying out decolonization to obtain column loading liquid, filtering the column loading liquid, adding the column loading liquid in a preparative chromatography, fractionally collecting eluant containing madecassoside and asiaticoside by taking methanol / water as a moving phase, and concentrating and drying to obtain purified products. The method has the beneficial effects that the technical process is simple, the operability is strong, the extraction efficiency is high, and the purities of the prepared asiaticoside and madecassoside are high; the method is applicable to industrial production.

Description

technical field [0001] The invention belongs to the technical field of extraction and separation of medicinal active ingredients, and in particular relates to a method for the extraction, separation and preparation of high-purity asiaticoside and madecassoside. Background technique [0002] Centella asiatica is the dry or rooted whole grass of the dicotyledon Umbelliferae. Widely distributed in various places south of the Yangtze River Basin, it is a commonly used Chinese herbal medicine in folk areas in Guangdong, and its use history has reached more than 2,000 years. Modern medical research shows that asiaticosides have the efficacy of treating depression, skin trauma, gastric ulcer, infectious hepatitis, skin diseases and epidemic cerebrospinal meningitis and other diseases. The main active ingredient of Centella asiatica is total asiaticoside, including asiaticoside, madecassoside and asiaticoside B and other triterpenoids. Among them, asiaticoside has been widely used...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J63/00
CPCC07J63/008
Inventor 李宇杨丽段迪钟鸣傅玉萍袁诚李金华
Owner GUANGZHOU HANFANG PHARMA
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