Method for one-step purification and separation of ephedrine by cation exchange resin and expanded bed integrated technology

The technology of a cation exchange and purification method is applied in the field of one-step purification and separation of ephedrine and alkaloids by cation exchange resin and expanded bed integration technology, which can solve the problems of high toxicity, complicated purification steps and low product yield, and achieves simple steps, Ease of promotion, the effect of reducing operational steps

Inactive Publication Date: 2005-12-07
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The object of the present invention is to overcome the shortcomings of existing ephedrine purification methods, such as high toxicity, complicated purification steps and low product yield

Method used

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  • Method for one-step purification and separation of ephedrine by cation exchange resin and expanded bed integrated technology
  • Method for one-step purification and separation of ephedrine by cation exchange resin and expanded bed integrated technology
  • Method for one-step purification and separation of ephedrine by cation exchange resin and expanded bed integrated technology

Examples

Experimental program
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Effect test

Embodiment 1

[0022] Embodiment 1, the preparation of ephedrine stock solution

[0023] my country is the main country producing natural ephedrine, in view of the fact that most of the manufacturers in my country use plant extraction to produce ephedrine. Therefore, the stock solution of the ephedrine used in the present invention adopts conventional plant extraction method to obtain, and concrete process is as follows:

[0024] Break the ephedra grass, weigh 150 grams of ephedra grass fine powder, add 5 times the volume of 0.05M dilute hydrochloric acid and decoct for 40 minutes (time after boiling), pour out the upper layer of liquid medicine, then add 2 times the volume of acid water and decoct for 30 minutes, twice The liquid medicines are combined, and the buffer A (0.01M disodium hydrogen phosphate-sodium dihydrogen phosphate, pH 7.2) is diluted 2 to 3 times to obtain a raw material solution of crude ephedrine hydrochloride. Reverse phase chromatography records that ephedrine hydroch...

Embodiment 2

[0025] Embodiment 2, the linear gradient elution purification of ephedrine hydrochloride (determining optimized elution conditions)

[0026] Self-made 90cm×16mm I.D. expanded bed chromatography column, the material is glass, the medium used is styrene series cation exchange resin 001×7Styrene DVB, the filling height is 11±0.2cm, buffer A (0.01M disodium hydrogen phosphate- Sodium dihydrogen phosphate, pH 7.2) equilibrates the chromatographic medium, loads the sample through the peristaltic pump, and keeps the expansion ratio at 1.3. After the bed expands and stabilizes for 30 minutes, the sample solution is quickly switched from the buffer solution to the conventional plant solution in Example 1. The suspension of crude ephedrine hydrochloride raw material liquid obtained by extraction method (using a stirrer to obtain the suspension containing plant fragments). When the breakthrough point reaches 87%, stop the injection of feed liquid, and immediately wash 8 column volumes wi...

Embodiment 3

[0028] Embodiment 3, the step elution purification of ephedrine hydrochloride (optimized elution conditions)

[0029] Self-made 90cm×16mm I.D. expanded bed chromatography column, the material is glass, the medium used is styrene series cation exchange resin 001×7Styrene DVB, the filling height is 11±0.2cm, buffer A (0.01M disodium hydrogen phosphate- Sodium dihydrogen phosphate, pH 7.2) equilibrates the chromatographic medium, loads the sample through the peristaltic pump, and keeps the expansion ratio at 1.3. After the bed expands and stabilizes for 30 minutes, the sample solution is quickly switched from the buffer solution to the conventional plant solution in Example 1. The suspension of crude ephedrine hydrochloride raw material liquid obtained by extraction method (using a stirrer to obtain the suspension containing plant fragments). When the breakthrough point reaches 17%, stop the injection of feed liquid, and immediately wash 4 column volumes with buffer solution unti...

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Abstract

The invention provides a process for one-step purification and separation of ephedrine which comprises the following steps, using 2-3 times of cushioning liquid A to dilute raw feed liquid containing ephedrine hydrochloride pretreated by 0.05M diluted hydrochloric acid and obtained through the conventional Chinese ephedra plant extraction, synthesis, biofermentation method or cell culture method, adsorbing hydrochloric ephedra sinica stapf in one step by employing a liquid distributor filled by phenylethene group cationic resin 001X7 Styrene DVB, carrying out two phase step elution by employing 0.01M phosphates cushioning liquid containing 0.1M NaCl and 1.0M NaCl, finally collecting the eluent of the second elution peak.

Description

technical field [0001] The invention relates to the field of biotechnology, and relates to a preparation process of ephedrine, an alkaloid with important medical value, that is, a method for one-step purification and separation of ephedrine by using cation exchange resin and expanded bed integration technology. Background technique [0002] Ephedrine (Ephedrine, C 10 h 15 The scientific name of NO) is 2-methylamino-1-phenyl-1-propanol, which belongs to aromatic amino alcohol derivatives and has important medicinal value. It is mostly made into hydrochloride for practical use, and the market demand is huge. Because its molecular structure is very similar to that of adrenaline, it has the functions of exciting the central nervous system, shrinking capillaries, enhancing myocardial contractility, etc. Clinically, it is mainly used to prevent asthma attack and treat habitual bronchial asthma and other diseases. At present, due to the suspension of use of PPA-containing drugs ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C215/30
Inventor 陈卫东苏志国
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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