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Method for preparing gentiopicroside

A technology of gentiopicroside and gentiopicroside, which is applied in the preparation of sugar derivatives, chemical instruments and methods, production of bulk chemicals, etc., can solve serious pollution, low gentiopicroside content, and unfavorable large-scale production operations, etc. question

Inactive Publication Date: 2010-05-12
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In the prior art, the extraction and separation method of gentiopicroside mainly adopts organic solvent method, etc., but the content of gentiopicroside obtained by these extraction processes is low, the pollution in the production process is serious, and it is unfavorable for large-scale production operations

Method used

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  • Method for preparing gentiopicroside

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Experimental program
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Effect test

Embodiment 1

[0021] Take 10Kg of Gentiana root and rhizome powder and add it to CO 2 In the supercritical extractor, methanol is used as the entrainer. The entrainer accounts for 2% of the total extraction solvent. The extraction pressure is 10MPa, the temperature is 30°C, and CO 2 Flow rate 1ml / g crude drug / min, extraction time 100min, to obtain the extract, adsorbed by AB-8 macroporous adsorption resin, eluted with 50% ethanol, collect 3 times the column volume of the eluate, recover the ethanol under reduced pressure and concentrate, Ethyl acetate-water-methanol (3:1:1) was added for crystallization, separated, washed, and dried to obtain 55.8 g of gentiopicroside. The purity was 98.6% by HPLC detection.

Embodiment 2

[0023] Take 10Kg of Gentiana root and rhizome powder and add it to CO 2 In the supercritical extractor, methanol is used as the entrainer, and the volume percentage of the entrainer in the total extraction solvent is 6%. The extraction pressure is 40MPa, the temperature is 60°C, and CO 2 The flow rate is 5ml / g crude drug / min, the extraction time is 250min, and the extract is obtained. The extract is adsorbed by H-103 macroporous adsorption resin and eluted with 80% ethanol. Collect 8 times the column volume of the eluate, recover the ethanol under reduced pressure and concentrate. Ethyl acetate-water-methanol (3:1:1) was added for crystallization, separated, washed, and dried to obtain 74.8 g of gentiopicroside. The purity was 98.1% by HPLC detection.

Embodiment 3

[0025] Take 10Kg of Gentiana root and rhizome powder and add it to CO 2 In the supercritical extractor, methanol is used as the entrainer, and the volume percentage of the entrainer in the total extraction solvent is 3%. The extraction pressure is 15MPa, the temperature is 45°C, and CO 2 The flow rate is 3ml / g crude drug / min, the extraction time is 150min, and the extract is obtained. It is adsorbed by D101 macroporous adsorption resin and eluted with 60% ethanol. Collect 5 times the column volume of the eluate, recover the ethanol under reduced pressure and concentrate, add acetic acid Ethyl ester-water-methanol (3:1:1) was crystallized, separated, washed, and dried to obtain 79.8 g of gentiopicroside. The purity was 99.4% by HPLC detection.

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Abstract

The invention relates to a method for preparing gentiopicroside with simple and convenient operation, small pollution and less equipment investment. The method comprises the following processing steps: adding gentiana manshurica root and rhizome powder into a CO2 supercritical fluid extractor; using methyl alcohol as entrainer which accounts for 2 to 6 percent of total extraction solvent in percentage by volume; and extracting the mixture under extracting pressure of between 10 and 40MPa, at the temperature of between 30 and 60 DEG C, and at a CO2 flow rate of between 1 and 5 ml / g crude drug / min for 100 to 250 minutes so as to obtain an extract; absorbing the extract by macroporous absorption resin; eluting the extract by 50 to 80 percent ethanol; collecting eluent of between 3 to 8 times of column volume; reclaiming the ethanol under reduced pressure and concentrating the ethanol; adding ethyl acetate-water-methanol (3:1:1) for crystallization. The gentiopicroside prepared by adopting the method has high purity, and is easy to realize industrial development.

Description

Technical field [0001] The invention relates to a method for preparing gentiopicrin, in particular to a method for extracting gentiopicrin from a plant. Background technique [0002] Gentiopicroside, synonym: Gentopicrin. Molecular formula: C 16 H 20 O 9 , Molecular weight: 356.329, CAS registration number: 20831-76-9, structural formula: [0003] [0004] Gentiopicrin is a natural compound with insecticidal and antimalarial activities, and it is widely present in many plants of the Gentiana family. [0005] The traditional Chinese medicine gentian is the dried roots and rhizomes of Gentiana manshurica Kitag., Gentiana scabraBge, Gentiana triflora pall or Gentiana rigescens Franch. It has the effects of clearing away heat and dampness, purging liver and gallbladder fire. The plants from all sources of gentian contain large amounts of gentiopicroside. [0006] In the prior art, the extraction and separation method of gentiopicrin mainly adopts organic solvent method, etc., but the c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/04C07H1/08
CPCY02P20/54
Inventor 刘东锋范淦彬杨成东
Owner NANJING ZELANG MEDICAL TECH
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