Preparation process for separating and purifying strychnine from total alkali of nux vomica

A technology of strychnine total alkaloids and strychnine, which is applied in the direction of organic chemistry, can solve the problems of small output and difficult separation, and achieve good environmental protection and cost-effective preparation

Inactive Publication Date: 2013-12-04
安徽宏信药业发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Due to the difficulty of separation, the relevant literature research is also less, of which only literature (Li etc., Separation and Purification of Strychnine and Strychnine in Strychnium Fructus by pH Zone Countercurrent Chromatography, Analytical Chemistry, 2010, 38(12): 17033-1707) reported that 50mg of strychnine was isolated from 308mg of Strychnium chinensis total alkaloids Strychnine and 120mg strychnine, the yields are respectively 72.8% and 85.1%; the purity is respectively 96.8% and 98.3%, this method has the deficiency of small yield, the market needs a kind of preparation of large-scale production of strychnine badly craft

Method used

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  • Preparation process for separating and purifying strychnine from total alkali of nux vomica
  • Preparation process for separating and purifying strychnine from total alkali of nux vomica
  • Preparation process for separating and purifying strychnine from total alkali of nux vomica

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Effect test

Embodiment 1

[0029] (1) Weigh 10 g of total alkaloids of Strychnis chinensis, dissolve with an appropriate amount of chloroform, mix evenly with 8 g of silica gel (200-300 mesh), evaporate the organic solvent to dryness, and use it as a sample separated by silica gel column chromatography.

[0030] (2) Weigh 180 g of silica gel (200-300 mesh), plug a glass column with a diameter of 5 cm at the bottom, and wet-pack the column with 95% ethanol, knock it down, and the height of the column bed is about 15 cm, which is a silica gel column for separation.

[0031] (3) Load the sample obtained in step (1) on the silica gel column prepared in step (2);

[0032] (4) eluting with 95% ethanol, collecting the eluent in sections, each section of the eluent is 2 times of column volume, and is identified as containing a single strychnine component by thin-layer chromatography of Strychnis in the Chinese Pharmacopoeia, Combine the eluents of each section of the single strychnine component and concentrate ...

Embodiment 2

[0035] (1) Weigh 10 g of total alkaloids of Strychnis chinensis, dissolve with an appropriate amount of chloroform, mix evenly with 10 g of silica gel (200-300 mesh), evaporate the organic solvent to dryness, and use it as a sample separated by silica gel column chromatography.

[0036] (2) Weigh 400 g of silica gel (200-300 mesh), plug a glass column with a diameter of 5 cm at the bottom, and wet-pack the column with 95% ethanol, knock it down, and the height of the column bed is about 25 cm, which is a silica gel column for separation.

[0037] (3) Load the sample obtained in step (1) on the silica gel column prepared in step (2);

[0038] (4) Elution with 95% ethanol first, collect the eluate of 1 times of column volume, then elute with ethanol solution containing 1% ammonium acetate, collect the eluate in sections, each section is 2 times of column volume, with In the Chinese Pharmacopoeia, the thin-layer chromatography of Strychnium is identified as containing a single st...

Embodiment 3

[0041] (1) Weigh 10 g of total alkaloids of strychnium, dissolve with an appropriate amount of chloroform, mix well with 20 g of silica gel (80-100 mesh), evaporate the organic solvent to dryness, and use it as a sample separated by silica gel column chromatography.

[0042] (2) Weigh 900g of silica gel (200-300 mesh), plug it into a glass column with a diameter of 5cm at the bottom, fill the column with anhydrous ethanol wet method, tap it, and the column bed height is about 30cm, which is a silica gel column for separation.

[0043](3) Load the sample obtained in step (1) on the silica gel column prepared in step (2);

[0044] (4) Elution with 95% ethanol first, collect the eluate of 1 times of column volume, then elute with ethanol solution containing 2% ammonium acetate, collect the eluate in sections, each section is 2 times of column volume, with In the Chinese Pharmacopoeia, the thin-layer chromatography of Strychnium is identified as containing a single strychnine comp...

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Abstract

The invention discloses a preparation process for separating and purifying strychnine from total alkali of nux vomica. Pure strychnine with the content exceeding 94% is prepared by taking total alkali of nux vomica as the raw material through a column chromatography and organic solvent extraction purification and separation method. The pure strychnine can be used as a chemical standard substance and a reference substance of nux vomica or an extract of the nux vomica or used as a raw material of a preparation. The preparation process is not only low in cost, simple and easy in process, but also applicable to the preparation of a larger amount of pure strychnine, and has wide social and economic effects.

Description

technical field [0001] The invention relates to the field of preparation of traditional Chinese medicine components, in particular to a preparation process for separating and purifying strychnine from total strychnine. Background technique [0002] Strychnos nux-vomica L., a traditional Chinese medicine, is the dry mature seed of Strychnos nux-vomica L., which has the effects of dredging collaterals, relieving pain, dispelling stagnation and reducing swelling. Modern studies have shown that its main active ingredients are alkaloids, with a content of about 1.5% to 5% of crude drugs, mainly strychnine, brucine and nitrogen oxides, among which strychnine Strychnine content tops the list, accounting for 1.2% to 2.2%; strychnine accounts for about 0.8%, which is a weakly alkaline indole alkaloid with a molecular formula of C 23 h 26 N 2 o 4 , relative molecular weight 394, white crystalline powder, extremely bitter taste; slightly soluble in water, soluble in organic solvent...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D491/22
Inventor 蔡宝昌顾锡镇何媛媛李兴尚李鹏秦昆明汪斌
Owner 安徽宏信药业发展有限公司
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