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Purification method of fangchinoline

A technology of tetrandrine and its purification method, which is applied in the field of refining tetrandrine by ODS reversed-phase silica gel method, can solve the problems of large solvent consumption, etc., and achieve the effects of high product purity, easy operation, and simple operation of process steps

Inactive Publication Date: 2012-08-29
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

This method also uses two extractions, the solvent consumption is large, and the toxic organic solvent benzene is used in the preparation process. This method only produces the crude tetrandrine

Method used

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  • Purification method of fangchinoline

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Take 1 kg of Fangji medicinal material powder, add 5 L of 40% methanol solution to reflux and extract twice, extract for 1 hour each time, recover the solvent from the extract until it has no alcohol smell, add hydrochloric acid to adjust the pH to 2, filter the acid solution, add sodium hydroxide to adjust to pH9, add 1 times the amount of chloroform for extraction, let stand to separate layers, release the chloroform layer, then take 450g of ODS silica gel to pack into the column, take another 50g of ODS silica gel and chloroform layer to mix the sample, evaporate the solvent, put it on the column, and elute with 60% methanol aqueous solution , collected the eluent, concentrated and dried to obtain 3.8 g of the product, with a content of 99.1%.

Embodiment 2

[0023] Take 1 kg of Fangji medicinal material powder, add 12L of 70% ethanol solution to reflux extraction 4 times, extract 3 hours each time, recover the solvent from the extract until it has no alcohol smell, add sulfuric acid to adjust the pH to 4, filter the acid solution, add potassium hydroxide to adjust to pH 9, add 3 times the amount of chloroform for extraction, let stand to separate layers, release the chloroform layer, then take 1000g ODS silica gel to pack into the column, take another 125g ODS silica gel and chloroform layer to mix the sample, evaporate the solvent, put it on the column, and elute with 55% acetonitrile aqueous solution , collected the eluent, concentrated and dried to obtain 3.5 g of the product, with a content of 99.3%.

Embodiment 3

[0025] Take 5 kg of Fangji medicinal material powder, add 40 L of 50% ethanol solution to reflux and extract 3 times, extract for 2 hours each time, recover the solvent from the extract until it has no alcohol smell, add formic acid to adjust the pH to 3, filter the acid solution, and add sodium hydroxide to adjust to pH 10, add 2 times the amount of chloroform for extraction, let stand to separate layers, release the chloroform layer, then take 3kg ODS silica gel to pack into the column, take another 300g ODS silica gel and chloroform layer to mix the sample, evaporate the solvent, put it on the column, and elute with 58% methanol aqueous solution , collected the eluate, concentrated and dried to obtain 18.7 g of the product, with a content of 98.7%.

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PUM

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Abstract

The invention relates to a purification method of fangchinoline. The method comprises the following specific steps: (1) refluxing or quenching and extracting fangchinoline medical powder by utilizing an alcohol solution, recovering solvents from the extracting solution until no alcohol flavor exists, and acidifying until the solution is acidic; and (2) performing alkaline regulation on the acidic solution, extracting with chloroform, filtering the extract through an ODS (Ozone Depleting Substance) silicagel column by a dry method, eluting with a methanol-water or acetonitrile-water mixed solvent, recovering solvents from the eluent and drying to obtain the fangchinoline. The purification method has the advantages of low energy consumption, low preparation period and high product purity.

Description

Technical field: [0001] The invention belongs to the field of natural product separation, and in particular relates to a method for refining tetrandrine by adopting an ODS reverse-phase silica gel method. Background technique: [0002] Fangji is the root tuber of Stephania tetrandra S. Moore, a plant belonging to the genus Fangji. It is a rheumatism-dispelling, antipyretic and analgesic drug, and it is mainly used for edema, dysuria, rheumatic joint pain, and hypertension. [0003] Tetrandrine contains alkaloids, flavonoids, polysaccharides and other ingredients, the active ingredient is alkaloids, the total alkaloid content can reach 2.3%, of which tetrandrine (tetrandrine) is about 1%, and tetrandrine (fangchinoline) is about 1%. 0.5%. Modern pharmacological studies have shown that Fangji alkaloids have analgesic, anti-inflammatory, antihypertensive, antibacterial, antitumor, and striated muscle relaxation effects. [0004] Tetrandrine: alias fangchinoline, nortetradine,...

Claims

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Application Information

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IPC IPC(8): C07D491/147
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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