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Method for extracting and separating picroside I and picroside II

A technology of berberine and berberine, applied in chemical instruments and methods, preparation of sugar derivatives, sugar derivatives, etc., can solve the problems of slow separation speed and low efficiency

Active Publication Date: 2017-05-31
山东康裕生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The polarity of berberine I and berberine II is similar, and it is difficult to separate the two by traditional extraction methods. Most of the current technologies are column chromatography methods, which are slow in separation speed and low in efficiency.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] (1) Take 50g of Tibetan Hu Huanglian medicinal materials and crush;

[0014] (2) Preparation of Rhizoma Rhizoma rhizoma extract: ultrasonically extract the above medicinal powder for 30 minutes, the extraction solvent is 10 times the amount of 75% ethanol, and the extract is allowed to stand for 8 hours and filtered to obtain a continuous filtrate of Rhizoma Rhizoma Rhizoma Rhizoma;

[0015] (3) Removal of impurities: the continuous filtrate of Hu Huang, the solvent was recovered under reduced pressure at 80 °C, concentrated into a fluid extract, adsorbed with 10 g of polyamide, and dried. Put on a polyamide chromatography column, wash the polyamide column with water until it is nearly colorless, and the molish reaction is negative, use a mixed solvent of 4 times the column bed volume (ethyl acetate-methanol-water-formic acid=40:23:30:7 ) eluting, collecting the eluate, recovering the solvent, concentrating to dryness, and dissolving with ethanol to obtain a mixed solut...

Embodiment 2

[0018] (1) Take 50g of Tibetan Hu Huanglian medicinal materials and crush;

[0019] (2) Preparation of Rhizoma Rhizoma rhizoma extract: ultrasonically extract the above-mentioned medicinal powder for 45 minutes, the extraction solvent is 15 times the amount of 85% ethanol, and the extract is allowed to stand for 5 hours and filtered to obtain a continuous filtrate of Rhizoma Rhizoma Rhizoma Rhizoma;

[0020] (3) Removal of impurities: the continuous filtrate of Hu Huang, the solvent was recovered under reduced pressure at 60 °C, concentrated into a fluid extract, adsorbed with 15 g of polyamide, and dried. Put on a polyamide chromatography column, wash the polyamide column with water until it is nearly colorless, and the molish reaction is negative, use a mixed solvent of 7 times the column bed volume (ethyl acetate-methanol-water-formic acid=60:22:15:3 ) eluting, collecting the eluate, recovering the solvent, concentrating to dryness, and dissolving with ethanol to obtain a m...

Embodiment 3

[0023] (1) Take 50g of Tibetan Hu Huanglian medicinal materials and crush;

[0024] (2) Preparation of rhizoma rhizoma extract: ultrasonically extract the above-mentioned medicinal powder for 40 minutes, the extraction solvent is 12 times the amount of 90% ethanol, and the extract is left to stand for 10 hours and filtered to obtain a continuous filtrate of rhizoma rhizoma rhizoma;

[0025] (3) Removal of impurities: the continuous filtrate of Huhuang, the solvent was recovered under reduced pressure at 70°C, concentrated into a liquid extract, adsorbed with 20g of polyamide, and dried. Put on a polyamide chromatography column, wash the polyamide column with water until it is nearly colorless, and the molish reaction is negative, use a mixed solvent of 5 times the column bed volume (ethyl acetate-methanol-water-formic acid=40:30:23:7 ) eluting, collecting the eluate, recovering the solvent, concentrating to dryness, and dissolving with ethanol to obtain a mixed solution of pic...

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PUM

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Abstract

The invention relates to a process method for extracting, separating and purifying picroside I and picroside II from rhizoma picrorhizae. The method comprises the following steps: (1) performing ultrasonic extraction on rhizoma picrorhizae powder to obtain a liquor A; (2) standing the liquor A, then filtering, recovering solvent from the filtrate under reduced pressure, concentrating to obtain a rhizoma picrorhizae fluid extract, adsorbing and mixing with polyamide, drying, passing through a polyamide chromatographic column, and eluting with ethyl acetate-methanol-water-formic acid mixed solvent; and (3) recovering solvent from the eluate, concentrating to dry, dissolving with ethanol, and adding neutral lead acetate precipitant to separate picroside I and picroside II. The method provided by the invention is low in cost, high in yield, simple in process and suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to a method for separating picroside I and picroside II from extracts from the traditional Chinese medicine Rhizoma Rhizoma Rhizoma Rhizoma, and belongs to the technical field of medicine. Background technique [0002] Huanglian is a traditional Chinese medicine in my country. Huanglian is the dry rhizome of the perennial herb of Scrophulariaceae. It is cold in nature and bitter in taste. It has the functions of clearing heat, dehumidification, improving eyesight, nourishing liver, benefiting gallbladder and killing insects. It is mainly used for tuberculosis and fever. Cough, damp-heat diarrhea, infantile malnutrition, red eyes and other diseases. The main chemical constituents are iridoids, cucurbitacins, phenethyl glucosides and phenolic glycosides, and also contain a very small amount of mannitol, picrosidenol, picrosterol, vanilla acetone and aromatic acids, etc. Among them, Picroside I (Picroside I) and Picroside II (Picrosi...

Claims

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Application Information

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IPC IPC(8): C07H17/04C07H1/08
CPCC07H1/08C07H17/04
Inventor 刘冬燕刘培冉贺灵剑刘文卉黄珊珊纪德选乔田斌张志东孙士青
Owner 山东康裕生物科技有限公司
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