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Method for preparing specnuezhenide reference substance

A technology of privetin and reference substance, which is applied in the field of modernization of traditional Chinese medicine, and can solve the problem of low purity of privetin

Active Publication Date: 2017-05-10
上海诗丹德标准技术服务有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, the demand for privetin reference substance is increasing, but there are few domestic reports on the separation and purification of privetin. The purity of privetin is not high either. For example, the patent application with application number 201110337108.6 discloses “a preparation method of privet” and the patent application with application number 200910093290.8 discloses “a kind of privet-specific component Separation and purification process of privetin", the purity of privetin obtained in the two patents is only above 98%

Method used

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  • Method for preparing specnuezhenide reference substance
  • Method for preparing specnuezhenide reference substance

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] A. Raw material extraction: crush 1 kg of Ligustrum lucidum medicinal material into coarse powder, add 10 L of ethanol solution with a volume fraction of 50%, heat extraction twice at 60°C for 2 hours each time, cool to room temperature, suction filter, and combine the filtrates , concentrated to no alcohol smell, a total of 1000ml;

[0055] B. Enrichment of macroporous resin: Weigh 3KgD101 macroporous adsorption resin and pack it into a column, statically adsorb the concentrated solution of step A with macroporous resin for 16 hours overnight, and then use 3L of water and 20% ethanol solution of 2L column volume respectively Elute the impurities, then elute the target substance with 3L of 40% ethanol solution, collect the eluate, and concentrate to 100ml;

[0056] C. Silica gel column chromatography: mix the 100ml concentrated solution of step B with 150g of 100-200 mesh silica gel, dry and crush, take 2kg of 200-300 mesh silica gel, and wet-pack the column with ethyl ...

Embodiment 2

[0061] A. Raw material extraction: crush 5 kg of Ligustrum lucidum medicinal material into coarse powder, add 50 L of ethanol solution with a volume fraction of 55%, heat extraction at 60°C for 2 times, each time for 2 hours, cool to room temperature, suction filter, and combine the filtrates , concentrated to no alcohol smell, a total of 5000ml;

[0062] B. Macroporous resin enrichment: Weigh 18KgD101 macroporous adsorption resin and pack it into a column, use the concentrated solution of step A to statically adsorb the macroporous resin overnight for 18 hours, and then use 15L of water and 10L of column volume of 20% ethanol solution Elute the impurities, then elute the target substance with 15L of 40% ethanol solution, collect the eluate, and concentrate to 500ml;

[0063] C. Silica gel column chromatography: Mix 500ml of the concentrated solution of step B with 600g of 100-200 mesh silica gel, dry and crush, take 10kg of 200-300 mesh silica gel, and wet-pack the column wit...

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Abstract

The invention provides a method for preparing a specnuezhenide reference substance. The preparation method specifically comprises the following steps: (i) providing specnuezhenide alcohol extract; (ii), mixing the specnuezhenide alcohol extract and a solvent to obtain a first mixture, and performing column chromatography separation on the first mixture by virtue of an intermediate-pressure preparation column, thereby obtaining a crude specnuezhenide product; (iii) performing recrystallization on the crude specnuezhenide product by virtue of purified water; (iv) separating and drying crystals obtained in step (iii), so as to obtain the specnuezhenide reference substance. The method is stable in process, convenient to operate, high in separation efficiency, low in cost, economical and environment-friendly, and has relatively high economic value and academic value.

Description

technical field [0001] The invention belongs to the technical field of modernization of traditional Chinese medicine, and relates to a preparation method of a chemical reference substance of traditional Chinese medicine. Specifically, the invention relates to a method for rapidly separating a reference substance of privet privet from Chinese medicinal material Ligustrum lucidum. Background technique [0002] Ligustrum lucidum, also known as holly, is the dry and mature fruit of Ligustrum lucidumAit., a traditional solid medicine in my country. "Shen Nong's Materia Medica" lists it as the top grade, saying that it "tastes bitter and flat, mainly nourishes the middle, calms the five internal organs, nourishes the spirit, and eliminates all diseases." It has the effect of nourishing the liver and kidney, improving eyesight and black hair. It is used for liver and kidney yin deficiency, dizziness, tinnitus, weak waist and knees, and premature graying of beard and hair. Modern p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/04C07H1/08
CPCC07H1/08C07H17/04
Inventor 辛振强何小义余小青张田勇戴军旗
Owner 上海诗丹德标准技术服务有限公司
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