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Method for separating total flavonoid glucuronide and total phenylethanoid glycoside in Callicarpa kwangtungensis Chun

A technology for the separation of glucuronides and glucuronides, which is applied in the field of separation of total flavonoid glucuronides and total phenylethanol glycosides in Guangdong Zizhu, and can solve the problem of the importance of total flavone glucuronides and the insufficient purity of total phenylethanol glycosides , mixed with other problems, to achieve excellent water solubility, light yellow color, easy to operate

Active Publication Date: 2015-07-29
JIANGSU KANION PHARMA CO LTD +2
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by the present invention is to overcome the fact that other impurities are mixed in the extraction results of the total phenylethanol glycosides in Guangdong purple pearl in the prior art, and the total flavonoid glucuronides present in the impurities are not paid enough attention , and the defect that the purity of total phenylethanol glycosides is not high enough, and a kind of separation method of total flavonoid glucuronide and total phenylethanol glycosides in Guangdong Zizhu is provided

Method used

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  • Method for separating total flavonoid glucuronide and total phenylethanoid glycoside in Callicarpa kwangtungensis Chun
  • Method for separating total flavonoid glucuronide and total phenylethanoid glycoside in Callicarpa kwangtungensis Chun
  • Method for separating total flavonoid glucuronide and total phenylethanoid glycoside in Callicarpa kwangtungensis Chun

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] In this example, the steps for separating and enriching total flavone glucuronides and total phenylethanol glycosides from Guangdong Zizhu are as follows:

[0053] (1) Take the aboveground parts of Guangdong Zizhu and dry them, crush them through a 30-mesh sieve, add water 10 times the mass of the powder, reflux and extract twice, each time for 2 hours, filter, combine the extracts, and concentrate under reduced pressure to a crude drug content of 10g / mL Concentration, get concentrated solution;

[0054] (2) AB-8 macroporous adsorption resin is applied to the concentrated solution, the sample volume is 2 times the column volume, and the impurity is eluted with 5 times the column volume of water, and then 4 times the column is eluted with 20% ethanol aqueous solution with a volume percent concentration Volume, flow rate 5BV / h, the eluate is concentrated under reduced pressure to no alcohol smell, and freeze-dried to obtain the total flavonoid glucuronide part, wherein th...

Embodiment 2

[0062] In this example, the steps for separating and enriching total flavone glucuronides and total phenylethanol glycosides from Guangdong Zizhu are as follows:

[0063] (1) Take the aboveground part of Guangdong purple pearl and dry it, crush it through a 10-mesh sieve, add 10 times the mass of the powder into an aqueous ethanol solution with a volume percentage concentration of 60%, and reflux for extraction twice, each time for 2 hours, filter, combine the extracts, and reduce Concentrate under pressure to the concentration of crude drug amount 1g / mL to obtain concentrated solution;

[0064] (2) Put the concentrated solution on D101 macroporous adsorption resin, the sample volume is 1 / 2 times the column volume, wash with 5 times the column volume of water to remove impurities, and then elute with 25% ethanol aqueous solution for 3 times Column volume, flow rate 3BV / h, concentrating the eluate under reduced pressure until it has no alcohol smell, and freeze-drying to obtain...

Embodiment 3

[0068] In this example, the steps for separating and enriching total flavone glucuronides and total phenylethanol glycosides from Guangdong Zizhu are as follows:

[0069] (1) Take the underground part of Guangdong Zizhu and dry it, crush it through a 10-mesh sieve, add 10 times the mass of the powder to 60% ethanol aqueous solution for reflux extraction twice, each time for 2 hours, filter, combine the extracts, reduce Concentrate under pressure to the concentration of crude drug amount 3g / mL to obtain concentrated solution;

[0070] (2) Put the concentrated solution on the D101 macroporous adsorption resin, the sample volume is 1 times the column volume, eluted with 4 times the column volume of water to remove impurities, and then eluted with 20% ethanol aqueous solution for 3 times the column volume Concentrate the eluent under reduced pressure at a flow rate of 3BV / h until there is no alcohol smell, freeze-dry to obtain the total flavonoid glucuronide fraction, wherein the ...

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Abstract

The present invention discloses a method for separating total flavonoid glucuronide and total phenylethanoid glycoside in Callicarpa kwangtungensis Chun. The method is as below: 1) mixing Callicarpa kwangtungensis Chun powder with water or aqueous ethanol, extracting and concentrating to obtain a concentrated liquid; 2) passing the concentrated liquid through a macroporous resin column, wherein the sampling volume is 1 / 5-2 times of the column volume, removing impurities by water of 4-6 times of the column volume, and eluting the macroporous adsorption resin column with 15-25% ethanol aqueous solution in the volume 3-5 times of the column volume to obtain total flavonoid glucuronide; 3) eluting the macroporous resin column with 35-45% ethanol aqueous solution in the volume 3-5 times of the column volume to obtain a total phenylethanoid glycoside crude product; and 4) passing the total phenylethanoid glycoside crude product through a polyamide resin column, wherein the maximum sampling volume is 1g / mL, and eluting with 5-30% ethanol aqueous solution in the volume 3-6 times of the column volume to obtain the total phenylethanoid glycoside. The separation method can effectively separate total flavonoid glucuronide and total phenylethanoid glycoside, and is simple, practical and applicable to industrial production.

Description

technical field [0001] The invention relates to a method for separating total flavonoid glucuronide and total phenylethanol glycoside in Guangdong purple pearl. Background technique [0002] Calliscarpa kwangtungensis Chun. is a plant of the genus Calliscarpa kwangtungensis Chun. It is mainly distributed in Jiangxi, Guangdong, Guangxi and Guizhou, and its resources are relatively rich. As a newly recorded variety in the 2010 edition of "Chinese Pharmacopoeia", it has the functions of astringing and stopping bleeding, dispelling blood stasis, clearing heat and detoxifying, and is mainly used clinically to treat gynecological inflammations such as cervical erosion and bleeding, vaginitis and cervicitis. Guangdong Zizhu is rich in phenylethanol glycosides, mainly including golden shicroside, forsythiaside B, verbascoside, 2′-acetyl forsythiaside B and 2′-acetyl caddiscoside (Brandioside); The content of flavonoids in Guangdong Zizhu is relatively low, mainly flavonoid glucuron...

Claims

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Application Information

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IPC IPC(8): A61K36/85C07H15/18C07H1/08
Inventor 胡晓杨义芳黄春跃李丽余婧
Owner JIANGSU KANION PHARMA CO LTD
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