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Preparation method of skimmin

A technology of linoside and methanol, applied in the field of medicine, can solve problems such as difficult industrialization, and achieve the effects of short production cycle, large sample load and good separation degree.

Inactive Publication Date: 2013-02-06
苏州宝泽堂医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chen Yu et al. used 95% ethanol extraction, sequential extraction with various organic solvents, and repeated silica gel column chromatography and gel column chromatography to separate and obtain innoside. This method is only suitable for a small amount of preparation in the laboratory and is not easy for industrialization.

Method used

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  • Preparation method of skimmin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Use 65% acetone 3 times in a flash extractor at room temperature with 20 kg of the whole plant of Rhizoma chinensis, 20 minutes each time, combine the extracts, concentrate under reduced pressure to extract, and use a mixed solution of ethyl acetate-methanol with a ratio of 10:1 Perform 18-stage countercurrent extraction, combine the extracts, recover the solvent under reduced pressure, disperse the obtained extract with water, absorb through a polyamide resin column, elute with 50% ethanol solution, collect 3 times the column volume eluate, and recover ethanol under reduced pressure , concentrated crude product. Weigh 200-300 mesh of activated silica gel and add it to a stainless steel chromatography column with an inner diameter of 60 mm and a diameter-to-height ratio of 1:12. The above-mentioned crude product is added to methanol sonication to dissolve it completely. : 15) the mixed solution was eluted, the fractions were collected in sections, monitored by TLC, the ...

Embodiment 2

[0021] Use 50% acetone 3 times with 50% acetone in a flash extractor at room temperature for 20 kg of the whole plant of Rhizoma chinensis, 30 minutes each time, combine the extracts, concentrate under reduced pressure to extract, and use a mixed solution of ethyl acetate-methanol with a ratio of 10:1 Carry out 17 stages of countercurrent extraction, combine extracts, recover solvent under reduced pressure, add water to disperse the obtained extract, absorb through polyamide resin column, elute with 60% ethanol solution, collect 2 times column volume eluate, recover ethanol under reduced pressure , concentrated crude product. Weigh 200-300 mesh activated silica gel and add it to a stainless steel chromatographic column with an inner diameter of 200 mm and a diameter-to-height ratio of 1:10. Add the above-mentioned crude product to methanol sonication to dissolve it completely, inject the sample with a pump, and use methanol-dichloromethane (1 : 15) the mixed solution was elute...

Embodiment 3

[0023] Use 80% acetone 3 times in a flash extractor at room temperature with 20 kg of the whole plant of Rhizoma chinensis, 20 minutes each time, combine the extracts, concentrate under reduced pressure to extract, and use a mixed solution of ethyl acetate-methanol with a ratio of 10:1 Carry out 15 stages of countercurrent extraction, combine the extracts, recover the solvent under reduced pressure, disperse the obtained extract with water, absorb through a polyamide resin column, elute with 45% ethanol solution, collect 6 times the column volume eluate, and recover ethanol under reduced pressure , concentrated crude product. Weigh 200-300 mesh of activated silica gel and add it to a stainless steel chromatography column with an inner diameter of 180 mm and a diameter-to-height ratio of 1:20. The above-mentioned crude product is added to methanol sonication to dissolve it completely. : 15) the mixed solution was eluted, the fractions were collected in sections, monitored by TL...

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Abstract

The invention relates to a preparation method of skimmin. The method comprises technical steps of: creeping dichondra complete herb is subjected to tissue breaking and extraction 3 times by using acetone; an extraction liquid is subjected to reduced-pressure concentration, such that an extraction paste is obtained; multi-stage countercurrent extraction is carried out by using an ethyl acetate-methanol mixed solvent with a ratio of 10:1; extraction liquids are combined; the solvent is subjected to reduced-pressure recovery; the obtained material is processed by using a polyamide resin column; an obtained elution liquid is concentrated, such that a crude product is obtained; the product is fed into a medium-pressure chromatography column with silica gel of 200-300 meshes; a methanol-dichloromethane mixed solvent system is adopted; elution liquids at target component fragments are collected; the elution liquid is filtered and concentrated, and is subjected to low-temperature drying, such that skimmin is obtained. The skimmin preparation method provided by the invention has the advantages of high product purity and suitability for industrialized enlargement.

Description

technical field [0001] The invention belongs to the technical field of medicine, and in particular relates to a method for extracting, separating and preparing inininin from Rhizoma chinensis. Background technique [0002] Skimmin is a coumarin compound, also known as 7-O-β-D-glucopyranosyloxycoumarin, mp.220-221℃, white needle-like crystal, molecular weight 324.28274 ;Molecular formula C 15 h 16 o 8 , the molecular structure formula is: [0003] [0004] Inherin is widely distributed in various plants and citrus fruits, and has activity in the treatment of renal insufficiency. At present, Benazepril and Losartan are the main drugs for clinical treatment of renal insufficiency, but they mainly rely on imports, are expensive, and have serious side effects, such as hyperkalemia, severe cough, and weak blood pressure lowering effect. In the pharmacological test, innoside has similar efficacy and strength to the above-mentioned synthetic drugs: in the mouse kidney injury...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/075C07H1/08
Inventor 李法庆刘东锋
Owner 苏州宝泽堂医药科技有限公司
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