Extraction and purification process method for forsythiaside A in fructus forsythiae leaves

A technology of forsythiaside and process method, which is applied in the field of extraction and purification of forsythiaside A, which can solve the problem of many impurities in forsythiaside A, increasing the difficulty and time of column chromatography, and the chromaticity of forsythiaside A Not good and other problems, to achieve the effect of improving the purity, raising the proposal rate, and reducing the difficulty

Inactive Publication Date: 2015-11-25
湖北济世药业有限责任公司 +1
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  • Summary
  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

In the prior art, forsythiaside A is obtained by extracting with an organic solvent and then purifying it on a silica gel column or column chromatography. For example, the invention patent with publication number CN101215302A discloses a preparation method of forsythiaside A, which is Use organic solvent to extract, and then use column chromatography to purify (refine) to obtain forsythiaside A; although this method achieves the purpose of extracting and purifying (refining) forsythiaside A, but after using organic solvent to extract, directly extract The extract is subjected to column chromatography, and the extract also contains fat-soluble pigments and water-soluble impurities, which not only increases the difficulty and time of subsequent column chromatography, but also has many impurities in the finally obtained forsythiaside A, and forsythiaside The chroma of glycoside A is not good

Method used

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Embodiment 1

[0010] Example 1: Take 50 g of dried forsythia leaves, add 0.8 Kg of 80% ethanol aqueous solution, heat and reflux for extraction three times, each time for 90 minutes, combine the three extracts, filter, and concentrate the filtrate at 60°C until it has no alcohol smell; Dissolve the concentrate in a certain amount of water to obtain an extract; then, adjust the pH value to 6, extract with petroleum ether to remove fat-soluble pigments, and then extract with saturated n-butanol to remove most of the water-soluble impurities, and extract the solvent by volume The dosage is 1 times that of the extract, extract 3 times, recover n-butanol, and obtain the forsythiaside A extract; dry the forsythiaside A extract on a 200-300 mesh silica gel column, and use ethyl acetate and methanol The mixed solution was eluted, wherein the volume ratio of ethyl acetate to methanol was 7:1, and the eluate was collected; thin-layer chromatography detection (by volume ratio, the developing solvent wa...

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Abstract

The invention provides an extraction and purification process method for forsythiaside A in fructus forsythiae leaves. Fat-soluble pigment and water-soluble impurities in forsythiaside A extract are removed as much as possible before purification, the difficulty of following forsythiaside A purification is lowered, the chromaticity of the final product forsythiaside A is good, the purity reaches 95%-99%, and the extraction rate reaches 3.5%-5.5%. According to the technical scheme, the method includes the steps that 1, extraction is conducted; 2, extraction is conducted, wherein water is added to concentrate obtained in the step 1 for dissolution, an extracting solution is obtained, then the pH value is adjusted to be 6, petroleum ether is added, the fat-soluble pigment is removed through extraction, and then, most of the water-soluble impurities are removed through extraction through water-saturated normal butanol, wherein the use amount of water-saturated normal butanol is 0.5-2 times that of the extracting solution according to the volume ratio, the number of extraction times is 2-4, normal butanol is recovered, and forsythiaside A extract is obtained; 3, chromatographic column refining (fed to a 200-300-mesh silicagel column) is conducted, and coarse crystal substances are obtained; 4, recrystallization is conducted, and a finished product is obtained. The main innovation of the method is shown in extraction in the step 2.

Description

technical field [0001] The invention relates to a process for extracting and purifying forsythiaside A from forsythia leaves. Background technique [0002] At present, the extraction and purification methods of forsythiaside A have been reported. In the prior art, forsythiaside A is obtained by extracting with an organic solvent and then purifying it on a silica gel column or column chromatography. For example, the invention patent with publication number CN101215302A discloses a preparation method of forsythiaside A, which is Use organic solvent to extract, and then use column chromatography to purify (refine) to obtain forsythiaside A; although this method achieves the purpose of extracting and purifying (refining) forsythiaside A, but after using organic solvent to extract, directly extract The extract is subjected to column chromatography, and the extract also contains fat-soluble pigments and water-soluble impurities, which not only increases the difficulty and time of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H15/18C07H1/08
Inventor 曹克红杨光义
Owner 湖北济世药业有限责任公司
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