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A kind of preparation method of sinomenine

A sinomenine and drying technology, applied in the field of extraction and separation of traditional Chinese medicine, can solve the problem that the product purity is difficult to reach 98%, and achieve the effects of reducing the dissolution of impurities, high product purity and high efficiency

Inactive Publication Date: 2011-12-07
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method solves the problem of countercurrent extraction of toxic liquid benzene in the original process, but the product purity is difficult to reach more than 98%.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Grind the stems and leaves of dried Pueraria japonica, take 1 kg, add 1% hydrochloric acid or sulfuric acid aqueous solution to soak for 2 hours, ultrasonically treat for 30 minutes, filter to obtain the extract, adjust the pH to 7.5, add an ultrafiltration membrane with a molecular weight cut-off of 3000-10000 for ultrafiltration, and then Add a nanofiltration membrane with a molecular weight cut-off of 200-500 to obtain a concentrated solution, adjust the pH to 10, extract with chloroform, take the organic layer, recover chloroform, and dry to obtain a crude product; the crude product is dissolved in 95% ethanol to make a concentration of 50mg / ml The solution was filtered through a 0.45 μm microfiltration membrane to obtain a sample solution. The preparative column was filled with a C8 bonded phase, with a particle size of 10 μm, a column length of 15 cm, and a diameter of 7 cm. The six-way valve was used to inject samples, and the injection volume was 25 ml. , with ac...

Embodiment 2

[0022] Grind the stems and leaves of dried Pueraria japonica, take 1 kg, add 0.5% hydrochloric acid or sulfuric acid aqueous solution to soak for 8 hours, ultrasonically treat for 30 minutes, filter to obtain the extract, adjust the pH to 8.5, add an ultrafiltration membrane with a molecular weight cut-off of 3000-10000 for ultrafiltration, and then Add a nanofiltration membrane with a molecular weight cut-off of 200-500 to obtain a concentrated solution, adjust the pH to 9.5, extract with chloroform, take the organic layer, recover chloroform, and dry to obtain a crude product; the crude product is dissolved in 95% ethanol to make a concentration of 100mg The solution per ml was filtered through a 0.45 μm microfiltration membrane to obtain the sample solution. The preparative column was filled with C18 bonded phase, with a particle size of 20 μm, a column length of 10 cm, and a diameter of 1 cm. Six-way valve injection, injection volume 5ml, with acetonitrile-0.3% ethylenediam...

Embodiment 3

[0024] Grind the stems and leaves of dried Pueraria japonica, take 5kg, add 0.8% hydrochloric acid or sulfuric acid aqueous solution to soak for 6 hours, ultrasonically treat for 30 minutes, filter to obtain the extract, adjust the pH to 8, add ultrafiltration membrane ultrafiltration with a molecular weight cut-off of 3000-10000, and then Add a nanofiltration membrane with a molecular weight cut-off of 200-500 to obtain a concentrated solution, adjust the pH to 11, extract with chloroform, take the organic layer, recover chloroform, and dry to obtain a crude product; the crude product is dissolved in 75% ethanol to make a concentration of 80mg / ml The solution was filtered through a 0.45μm microfiltration membrane to obtain a sample solution. The preparative column was filled with C18 bonded phase, with a particle size of 15μm, a column length of 50cm, and a diameter of 10cm. Six-way valve injection was used, and the injection volume was 30ml. , using acetonitrile-0.3% ethylene...

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Abstract

The invention discloses a preparation method of sinomenine, which comprises the following steps: crushing the stems and leaves of dried pueraria puerariae, adding 0.5-1% hydrochloric acid or sulfuric acid aqueous solution to extract, adjusting the pH of the extract to 7.5-8.5, adding an ultrafiltration membrane for ultrafiltration, Then add nanofiltration membrane and nanofiltration, adjust the pH of the concentrated solution to 9.5-11, extract with chloroform, concentrate the extract, and then use preparative liquid chromatography to separate, ultraviolet on-line detection, collect the target components, and dry at low temperature to obtain the sinomenine product . The invention has low energy consumption, less pollution and high product content, which can reach more than 98%, and is not only suitable for small-scale experiments, but also can be used for industrial production.

Description

technical field [0001] The invention belongs to the technical field of extraction and separation of traditional Chinese medicines, in particular to a preparation method of sinomenine. Background technique [0002] Bat kudzu ( Menis permum dauricum ) is a traditional Chinese medicine plant, and its dried rhizome can be used for medicinal purposes, called "Northern bean root". Bat kudzu has anti-arrhythmia, antihypertensive, antispasmodic and anti-cancer effects, and some active ingredients such as dauricine, bat daurinine, and bat kudzu have been isolated from the plant, but about bat kudzu There are few reports on the chemical constituents of stems and leaves. Liu Rui et al. (Journal of Northwest Forestry University, 2010, 25(5): 176-178) conducted research on the stems and leaves of Pueraria puerariae and found that it contains some active ingredients such as tetrandrine and sinomenine. [0003] Sinomenine, alias (9alpha, 13alpha, 14alpha)-7,8-didehydro-4-hydroxy-3,7-dim...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D221/28
Inventor 刘东锋万冬梅
Owner NANJING ZELANG MEDICAL TECH
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