Method for purifying asiatic acid in asiatic pennywort herb

A technology of asiatic acid and centella asiatica, which is applied in the field of enzymatic extraction and macroporous resin purification of asiatic acid, can solve the problems of low extraction rate, low content, long extraction time, etc., achieve mild conditions and reduce pollution , cost reduction effect

Inactive Publication Date: 2012-05-09
苏州宝泽堂医药科技有限公司
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

Such as the patent (application number 200810163172.5) "a method for preparing asiatic acid by hydrolysis of asiaticoside", the method disclosed in this patent is to prepare asiatic acid by hydrolysis of asiaticoside, although the process is simple, the extraction low rate, low content
However, the traditional method of directly extracting Asiatic acid from Centella asiatica often takes a long time to extract, requires a large amount of solvent, and the extraction rate is low, and the content is not very high

Method used

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  • Method for purifying asiatic acid in asiatic pennywort herb

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Embodiment 1

[0022] Take Centella asiatica and crush it to 60 mesh, weigh 1kg, add appropriate amount of hydrochloric acid aqueous solution (pH5) to moisten, add 10g of cellulase, mix well, and naturally enzymatically hydrolyze for 3 days, then use 7L of 90% ethanol solution to reflux extract the raw material for enzymolysis for 1 hour , extracted 3 times, the extract was filtered to recover ethanol under reduced pressure, added 2L petroleum ether to shake, transferred to a separatory funnel, removed the petroleum ether layer, released and centrifuged to obtain 53g of crude extract, dissolved in absolute ethanol, filtered, and added 50g of NKA to the filtrate -2 macroporous resin resins, recycle ethanol. Take 50g of NKA-2 macroporous resin to pack into a column, add the dry sample to the upper part of the resin column, take 1.5L of 40% ethanol solution to elute the impurities, and then take 2L of 90% ethanol solution to elute the active ingredients, recover under reduced pressure to 40% eth...

Embodiment 2

[0024] Take centella asiatica and crush it to 10 meshes, weigh 1kg, add appropriate amount of sulfuric acid aqueous solution (pH6) to moisten, add 4g of β-glucomerase and mix well, natural enzymolysis for 5 days, enzymolysis raw materials are extracted with 10L of 70% methanol solution under reflux 2 hours, extracted twice, the extract was filtered to recover ethanol under reduced pressure, added 3L petroleum ether to shake, transferred to a separatory funnel, removed the petroleum ether layer, released and centrifuged to obtain 65g of crude extract, dissolved in absolute ethanol, filtered, and the filtrate Add 70g of NKA-9 macroporous resin to recover ethanol. Take 50g of NKA-9 macroporous resin and put it into a column, add the dry sample to the upper part of the resin column, take 4L of 20% ethanol solution to elute the impurities, then take 3L of 70% ethanol solution to elute the active ingredients, recover under reduced pressure to 30% ethanol, place for crystallization, a...

Embodiment 3

[0026] Take centella asiatica and crush it to 40 mesh, weigh 1kg, add appropriate amount of citric acid aqueous solution (pH4) to moisten, add 8g of amylase and mix well, and naturally enzymatically hydrolyze for 4 days. , the extract is filtered to recover ethanol under reduced pressure, add 1L of petroleum ether to shake, transfer to a separatory funnel, remove the petroleum ether layer, release and centrifuge to obtain 45g of crude extract, dissolve with absolute ethanol, filter, add 50g X-5 large to the filtrate Hole resin resin, recovery ethanol. Take 50g of X-5 macroporous resin to pack into a column, put the dry sample into the upper part of the resin column, take 3L of 30% ethanol solution to elute impurities, and then take 2.5L of 80% ethanol solution to elute active ingredients, recover under reduced pressure to 40% ethanol, place for crystallization, Filtrate to obtain 12 g of crystals, dissolve the crystals under reflux with anhydrous methanol, let the crystals sta...

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Abstract

The invention provides a method for purifying asiatic acid in asiatic pennywort herb. The method comprises the following steps of: adding a biological enzyme into an asiatic pennywort herb medicinal material serving as a raw material for performing natural enzymolysis; extracting a zymolyte with 70-99 percent alcohol solution for 1-3 times; recovering ethanol from an extracting solution under reduced pressure; adding petroleum ether into a concentrated solution for degreasing; dissolving a crude extract and adding macroporous resin for mixing; loading onto a macroporous resin column with a dry method; eluting with ethanol solutions of different concentrations; concentrating and crystalizing; refluxing, dissolving and recrystallizing a crystal with methanol and acetone; and drying to obtain a product. The method has the advantages of easiness for process operation, resin recyclability, and high content, high yield and low cost of the obtained product, and is suitable for industrial production.

Description

Technical field: [0001] The invention relates to a method for extracting asiatic acid from centella asiatica, in particular to a method for extracting asiatic acid by enzymatic extraction and macroporous resin. Background technique: [0002] Asiatic acid, ursane-type pentacyclic triterpene acids. [0003] Molecular formula: C 48 h 78 o 5 . [0004] [0005] Asiatic acid is insoluble in petroleum ether and water, soluble in methanol, ethanol, butanol, butanone, slightly soluble in acetone, slightly soluble in benzene, chloroform, ether and other organic solvents. [0006] Centella asiatica is the dry whole herb of the Umbelliferae plant Centella asiatica, also known as Luodeda, Bengdawan, and Banbianqian. It has been used as a medicinal plant in my country for more than 2,000 years, and it is included in the "Chinese Pharmacopoeia" commonly used traditional Chinese medicine. Centella asiatica resources are very rich in China, almost all over the south of the Yangtze R...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J63/00
Inventor 李法庆杨成东刘东锋
Owner 苏州宝泽堂医药科技有限公司
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