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Technology for extraction and separation of scopolamine from low content datura metel

A technology of scopolamine and galanthus, applied in the field of raw material medicine preparation, can solve the problems of difficulty in improving the pure product, poor enrichment, low recovery rate, etc., and achieve the effects of less impurities in extraction, high extraction rate and small dosage

Inactive Publication Date: 2018-10-02
ANHUI DEXINJIA BIOPHARM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

And the preparation method of scopolamine that has been reported at present is that Inner Mongolia produces high-content datura as raw material, and it extracts with chloroform-saturated acid aqueous solution, then carries out strong acidic cation exchange resin purification to the extract, and then after multi-step chloroform extraction Crystallization obtains high-purity scopolamine hydrobromide. If this method is carried out with low-content raw materials, problems such as poor enrichment, low recovery rate, and difficulty in improving product purity will occur in the resin purification stage, and a large amount of chloroform solution is used in the whole process. Expensive, highly toxic and costly

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] The present embodiment extracts and separates the technology of scopolamine from low-content Dajinhua as follows:

[0034] 1. Preparation of scopolamine crude extract

[0035] Take the dried datura flower and pulverize it with a pulverizer, and pass through a 40-mesh sieve to obtain datura powder; add the obtained datura powder to a mixture of ammonia and dichloromethane for ultrasonic extraction, and the datura powder and dichloromethane The mass volume ratio of datura powder and ammonia water (mass concentration is 23-25%) is 1g:2mL, filtered, and the filter residue is repeatedly extracted twice, and the combined extracts are dried to obtain scopolamine crude extract;

[0036] 2. The first step of liquid-liquid extraction

[0037] The scopolamine crude extract obtained in step 1 was redissolved in chloroform, then extracted twice with hydrobromic acid aqueous solution (pH=6), and the acidic aqueous phase was combined;

[0038] 3. The second step of liquid-liquid ex...

Embodiment 2

[0054] Others are the same as in Example 1, except that 732 type strongly acidic cation exchange resin is used for purification in the macroporous resin purification stage. According to the method described in Example 1, the adsorption and desorption capacity of 732 type strong acidic cation exchange resins to scopolamine is tested, and the results show that: the adsorption capacity of 732 type strong acidic cation exchange resins to scopolamine is 9.1mg / g, and the adsorption rate is 94.8%, and the desorption rate is 27.6%.

Embodiment 3

[0056] Others are the same as in Example 1, except that X-5 resin is used for purification in the macroporous resin purification stage. According to the method described in Example 1, the adsorption and desorption capacity of X-5 resin to scopolamine is tested, and the results show that: the adsorption capacity of X-5 resin to scopolamine is 6.93mg / g, the adsorption rate is 72.57%, and the desorption rate is 72.57%. 28.3%.

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Abstract

The invention discloses a technology for extraction and separation of scopolamine from low content datura metel. The technology includes: adopting ultrasonic-assisted dichloromethane process for extraction, then using acid water and carbon tetrachloride for extraction to realize preliminary enrichment of scopolamine, and then combining macroporous resin with crystallization technology for purification to obtain high purity scopolamine hydrobromide. The technology has the advantages of low dosage of high toxic organic solvent, high purity and recovery product, strong enrichment and purificationeffect, large sample handling capacity, simple and feasible process, suitability for low content raw materials and the like.

Description

technical field [0001] The invention relates to the field of preparation of crude drugs, in particular to a process for extracting and separating scopolamine from low-content datura flowers. Background technique [0002] Scopolamine is an alkaloid widely present in Solanaceae plants. It has various functions such as antispasmodic, mydriatic, anticholinergic, analgesic, and sedative. It has been widely used in clinical pharmacy. The demand for the product is very high. Currently, scopolamine is generally extracted from the Solanaceae plant Dajina. Yangjinhua, also known as big morning glory, mountain eggplant, phoenix flower, mandala flower, etc., is widely distributed and is produced in Jiangsu, Zhejiang, Fujian, Anhui, Inner Mongolia, Xinjiang and other places in China. However, because Yangjinhua The content of scopolamine in it will vary greatly depending on the place of origin and the season. The 2015 edition of "Chinese Pharmacopoeia" stipulates that the content of sc...

Claims

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Application Information

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IPC IPC(8): C07D451/10
CPCC07D451/10
Inventor 许坤张文成付传香惠爱玲
Owner ANHUI DEXINJIA BIOPHARM
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