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Method for preparing stephanine

A stephanine and stephenine technology, which is applied in the field of stephenine preparation, can solve the problems of unfavorable large-scale production operations, serious pollution, and low stephenine content

Inactive Publication Date: 2010-05-12
SUZHOU PAITENG BIOLOGICAL 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 methods of stephine mainly adopt organic solvent method, etc., but the content of stephine obtained by these extraction processes is low, the pollution is serious in the production process, and it is unfavorable for large-scale production operations

Method used

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  • Method for preparing stephanine

Examples

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Effect test

Embodiment 1

[0016] Take 10Kg of fresh Stephania vine roots and stems, add 10 times its weight in water and soak for 24 hours, separate the medicinal solution, filter, concentrate, adjust the pH value to 11 with concentrated ammonia water, add an equal volume of chloroform for extraction, take the chloroform layer, and recover the solvent And dry to get the total alkaloids, add chloroform to dissolve, inject high-efficiency countercurrent extractor, use chloroform-0.07mol / L sodium phosphate-0.04mol / L citric acid buffer solvent system, the upper phase is the stationary phase, and the lower phase is the mobile phase , collect steppaline segments, concentrate, collect crystals, wash and dry to obtain 5.4 g steppineine, which is detected by HPLC with a purity of 98.6%.

Embodiment 2

[0018] Take 10Kg of fresh Stephania vine roots and stems, add 12 times its weight in water and soak for 72 hours, separate the liquid medicine, filter, concentrate, adjust the pH value to 14 with concentrated ammonia water, add an equal volume of chloroform for extraction, take the chloroform layer, and recover the solvent And dry to get the total alkaloids, add chloroform to dissolve, inject high-efficiency countercurrent extractor, use chloroform-0.07mol / L sodium phosphate-0.04mol / L citric acid buffer solvent system, the upper phase is the stationary phase, and the lower phase is the mobile phase , collect steppaline segments, concentrate, collect crystals, wash and dry to obtain 8.4 g steppineine, which is detected by HPLC with a purity of 98.3%.

Embodiment 3

[0020] Take 10Kg of fresh Stephania vine roots and stems, add 15 times its weight in water and soak for 48 hours, separate the liquid medicine, filter, concentrate, adjust the pH value to 13 with concentrated ammonia water, add an equal volume of chloroform for extraction, take the chloroform layer, and recover the solvent And dry to get the total alkaloids, add chloroform to dissolve, inject high-efficiency countercurrent extractor, use chloroform-0.07mol / L sodium phosphate-0.04mol / L citric acid buffer solvent system, the upper phase is the stationary phase, and the lower phase is the mobile phase , collect the stephine segment, concentrate, collect the crystals, wash and dry to obtain 7.6 g stephine, which is detected by HPLC with a purity of 99.3%.

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Abstract

The invention relates to a method for preparing stephanine, which has the advantages of simple and convenient operation, light pollution and less equipment investment. The method comprises the following process steps: taking fresh roots and stems of stephania japonica, adding water of which the weight is 10 to 20 times that of the roots and stems of the stephania japonica, soaking for 24 to 72 hours, separating liquor, filtering, concentrating, adjusting pH value to between 11 and 14 with strong ammonia water, adding chloroform with equal volume for extraction, taking a chloroform layer, recovering a solvent and drying to obtain total alkaloids; and adding chloroform to dissolve the total alkaloids, injecting into a high-efficiency countercurrent extractor, collecting the stephanine section with a chloroform-0.07mol / L sodium phosphate-0.04mol / L citric acid buffer solution solvent system by taking a fixed phase as an upper phase and a mobile phase as a lower phase, concentrating, and collecting crystals. The stephanine prepared by the method has high purity, and industrial enlargement is easy to realize.

Description

technical field [0001] The invention relates to a method for preparing stephine, in particular to a method for extracting stephine from plants. Background technique [0002] Stephanine (Stephanine), molecular formula: C 19 h 19 NO 3 , molecular weight: 309.364, CAS accession number: 517-63-5, the structural formula is as follows: [0003] [0004] Stephanine is a natural compound with various physiological activities such as antibacterial and anti-inflammatory, and it is widely found in various plants of the genus Stephania Lour. [0005] Stephania japonica (Thunb.) Miers is the main source of traditional Chinese medicine Stephania japonica, which contains a large amount of stephanine. [0006] In the prior art, the extraction and separation of stephine mainly adopts organic solvent method, etc., but the content of stephine obtained by these extraction processes is low, the pollution is serious in the production process, and it is unfavorable for large-scale productio...

Claims

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Application Information

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IPC IPC(8): C07D491/06
Inventor 王琳范淦彬
Owner SUZHOU PAITENG BIOLOGICAL MEDICAL TECH
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