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Method for separating and purifying desacetyl asperulosidic acid methyl ester

A technology of acetyl chlorophyll and methyl oxalate, applied in chemical instruments and methods, organic chemistry, preparation of sugar derivatives, etc., can solve the problems of unsuitability for industrialized production, long production cycle, large sample loss, etc., and shorten the preparation time. , No sample loss, the effect of improving the amount of preparation

Inactive Publication Date: 2012-02-01
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The above methods all use solid packing column chromatography repeatedly, the operation is cumbersome, the production cycle is long, the sample loss is large, the yield is low, the cost is high, and it is not suitable for industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Take 500g of Hedyotis diffusa whole herb and pulverize it into a coarse powder, extract it by microwave with 50% ethanol for 20min, repeat the extraction 6 times, and concentrate the extract after filtering to obtain the crude extract of Hedyotis diffusa;

[0016] Select n-heptane, dichloromethane, methanol and water as the solvent system, configure them in a separatory funnel at a volume ratio of 1:4:3:2, shake them fully, leave to stand for stratification, take the upper phase as the stationary phase, and the lower phase As the mobile phase, dissolve 100 mg of Hedyotis diffusa crude extract in 5 ml of the lower phase solution for later use, use a semi-preparative high-speed countercurrent chromatograph to separate at room temperature, take the stationary phase and pump it into the high-speed countercurrent chromatographic column, start the host, Adjust the rotation speed to 900rpm, pump in the mobile phase, wait for the liquid to flow out, adjust the flow rate to 2ml / m...

Embodiment 2

[0018] Take 500g of Hedyotis diffusa whole herb and pulverize it into a coarse powder, extract it by microwave with 50% ethanol for 20min, repeat the extraction 5 times, and concentrate the extract after filtering to obtain the crude extract of Hedyotis diffusa;

[0019] Select n-heptane, dichloromethane, methanol and water as the solvent system, arrange them in a separatory funnel according to the volume ratio of 0.5:5:4:3, shake fully, let stand to separate layers, take the upper phase as the stationary phase, and the lower phase As the mobile phase, dissolve 100 mg of Hedyotis diffusa crude extract in 5 ml of the lower phase solution for later use, use a semi-preparative high-speed countercurrent chromatograph to separate at room temperature, take the stationary phase and pump it into the high-speed countercurrent chromatographic column, start the host, Adjust the rotation speed to 900rpm, pump in the mobile phase, wait for the liquid to flow out, adjust the flow rate to 2ml...

Embodiment 3

[0021] Take 500 g of the whole Hedyotis diffusa herb and grind it into a coarse powder, extract it by microwave with 50% ethanol for 20 min, repeat the extraction 4 times, and concentrate the extract after filtering to obtain the crude extract of Hedyotis diffusa;

[0022] Select n-heptane, dichloromethane, methanol and water as the solvent system, arrange them in a separatory funnel at a volume ratio of 2:5:3:4, shake them fully, leave to stand and separate into layers, take the upper phase as the stationary phase, and the lower phase As the mobile phase, dissolve 100 mg of Hedyotis diffusa crude extract in 5 ml of the lower phase solution for later use, use a semi-preparative high-speed countercurrent chromatograph to separate at room temperature, take the stationary phase and pump it into the high-speed countercurrent chromatographic column, start the host, Adjust the rotation speed to 850rpm, pump in the mobile phase, wait for the liquid to flow out, adjust the flow rate to...

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Abstract

The invention relates to a method for separating and purifying desacetyl asperulosidic acid methyl ester by using a semipreparative high-speed countercurrent chromatograph. The method is characterized in that a solvent system is composed of n-heptane, dichloromethane, methanol and water; the solvent system is placed in a separating funnel and sufficiently shaken and then stands still for layering, the upper phase is used as a stationary phase, and the lower phase is used as a mobile phase; and herba oldenlandiae crude extract is dissolved in the lower-phase solution to prepare into a sample solution, the sample solution is detected by the high-speed countercurrent chromatograph and an ultraviolet spectrograph, fraction is collected according to the chromatographic peak, concentrated and dried to finally obtain high-purity desacetyl asperulosidic acid methyl ester. The method has the advantages that solid filler is not used; irreversible adsorption is not existed; a large amount of desacetyl asperulosidic acid methyl ester can be separated efficiently and rapidly by the method; the preparation process is simple and easy to operate; and the purification efficiency is high, thereby laying a solid foundation for extraction and utilization of active ingredients in herba oldenlandiae.

Description

technical field [0001] The invention belongs to the technical field of extracting effective components of traditional Chinese medicines, and relates to a method for separating and purifying methyl deacetylsylphine oxalate by using high-speed countercurrent chromatography. Background technique [0002] Deacetyl asperulosidic acid methyl ester (deacetyl asperulosidic acid methyl ester), alias deacetyl asperulosidic acid methyl ester, molecular formula: C 17 h 24 o 11 , the molecular weight is 404.366, deacetylated methyl oxalate is a white powder, easily soluble in methanol and water, is an iridoid compound isolated from gardenia, Hedyotis diffusa and other plants, iridoids Compounds are widely distributed in the plant kingdom and have significant pharmacological effects, such as geniposide, which has laxative and choleretic effects. It has been reported in the literature that methyl deacetylpyrrolate has a cathartic effect. [0003] Existing reports on the preparation of ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/04C07H1/08
Inventor 刘东锋郭琴
Owner NANJING ZELANG MEDICAL TECH
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