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Preparation method of hydroxyl asiaticoside

A technology of madecassoside and centella asiatica, which is applied in the field of preparation of madecassoside, can solve the problems of high production cost and high price of high performance liquid chromatography, and achieves the advantages of reduced cost, high purity and reduced production cost. Effect

Active Publication Date: 2011-01-19
GUILIN NATURAL INGREDIENTS CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method can obtain high-purity madecassoside single product, it uses the asiaticoside extract with a weight content of 30 to 97% as a raw material for separation and purification, and a certain amount must be extracted from centella asiaticoside first. content of asiaticoside extract; in addition, the price of equipment used in this method for preparative high-performance liquid chromatography is relatively high, resulting in high production costs of products

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 1) Take Centella asiatica, crush it, put it in an extraction tank, add 65% ethanol 10 times the weight of the raw material for reflux extraction, control the temperature at 90°C, reflux the first time for 90 minutes, filter out the liquid medicine, and then add 10 times the raw material 65% ethanol by weight, reflux extraction for 30min, and combine the extracts;

[0028] 2) The extract is filtered with an alumina ceramic membrane with a pore size of 0.25 μm, then subjected to D101 macroporous resin column chromatography, and the resin column is washed with water until the effluent is clear. Wash the column with 70% ethanol of the volume of the resin column bed, collect the 70% ethanol eluate, concentrate under reduced pressure to extract;

[0029] 3) The extract is used for 95% ethanol precipitation with 10 times its weight, suction filtration, and the filtrate is added with water to make the ethyl alcohol therein

[0030] Alcohol content is 70%, enter activated carbo...

Embodiment 2

[0034] 1) Take Centella asiatica, pulverize it, put it in an extraction tank, add 80% ethanol 12 times the weight of the raw material to reflux for extraction for 90 minutes, control the temperature at 95°C, and collect the extract;

[0035] 2) The extract is filtered with an alumina ceramic membrane with a pore size of 0.5 μm, then enters the AB-8 macroporous resin column chromatography, washes the resin column with water until the effluent is clear, and then uses 40% ethanol and 1.5 times the volume of the resin column bed successively. Wash the column with 75% ethanol 3 times the volume of the resin column bed, collect the 75% ethanol eluate, and concentrate under reduced pressure to extract;

[0036] 3) The extract is used for alcohol precipitation with 100% ethanol 8 times its weight, suction filtration, adding water to the filtrate to make the ethanol content therein to 75%, then entering a neutral alumina resin column for decolorization, and collecting the effluent;

[...

Embodiment 3

[0040] 1) Take Centella asiatica, crush it, put it in an extraction tank, add 70% ethanol 10 times the weight of the raw material for reflux extraction, control the temperature at 100°C, reflux the first time for 60 minutes, filter out the medicinal solution, and then add 8 times the raw material 70% ethanol by weight, reflux extraction for 30 minutes, filter out the medicinal solution, add 70% ethanol 6 times the weight of raw materials for the third time, reflux extraction for 30 minutes, and combine the extracts;

[0041] 2) The extract is filtered with an alumina ceramic membrane with a pore size of 1 μm, and then subjected to D130 macroporous resin column chromatography, and the resin column is washed with water until the effluent is clear, and then 2.5 times the volume of the resin column bed volume 30% ethanol and 2 times the resin Wash the column with 70% ethanol of the column bed volume, collect the 70% ethanol eluate, concentrate under reduced pressure to extract;

...

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Abstract

The invention discloses a preparation method of hydroxyl asiaticoside. Centella serves as raw material and is heated, reflowed and extracted by ethanol; the obtained extract enters a macroporous resin column for chromatography after filtered by a ceramic membrane; the resin column is washed by water and is extracted until effluent is clear; the column is successively washed by 30-40% of ethanol and 70-80% of ethanol, and 70-80% of ethanol eluate is collected and concentrated into extract; the extract is performed with alcohol precipitation by 90-100% of ethanol and filtered; the content of ethanol in the filtrate is regulated to 70-80%; then a decoloring resin column is decolored to collect effluent; the effluent is concentrated so that ethanol content in the effluent is 10-15%, and devitrification and filteration are carried out; mother liquor enters the macroporous resin column for chromatography; the resin column is washed by water until the effluent is clear; then, the column is washed by 10-20% of ethanol and 35-45% of ethanol successively; and 35-45% of ethanol eluate is collected, concentrated and dried to obtain the hydroxyl asiaticoside. Compared with the prior art, the method of the invention has simple operation, low production cost and high product purity.

Description

technical field [0001] The invention relates to a preparation method of madecassoside, which belongs to the technical field of extraction of medicinal active ingredients. Background technique [0002] Centella asiatica is the whole herb or rooted whole plant of Centella asiatica, a dicotyledonous plant Umbelliferae. It has the effects of clearing away heat and dampness, reducing swelling and detoxification; Injury etc. Centella asiaticoside is the active ingredient of Centella asiatica, and madecassoside is one of the main components of asiaticoside. Studies have found that madecassoside has good antidepressant medicinal properties and is a promising natural antidepressant. [0003] Currently, there are not many methods for extracting and isolating madecassoside from Centella asiatica, specifically: [0004] 1. The invention patent with the publication number CN1377649 discloses a method for preparing madecassoside. Specifically, after dissolving total asiaticoside in met...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J63/00
Inventor 孙步祥梁远盛宋云飞张志朋汤凌志
Owner GUILIN NATURAL INGREDIENTS CORP
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