Continuous preparation method for extracting ephedrine from ephedra

A technology for ephedrine and ephedra, which is applied in the field of natural medicine extraction, can solve the problems of long production cycle, low recovery rate, high toxicity, etc., and achieves the effects of simple operation, large processing capacity and favorable industrial production.

Pending Publication Date: 2022-03-04
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
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Problems solved by technology

At present, the separation and purification methods of ephedrine mainly include cation exchange resin method, oxalic acid crystallization method, xylene extraction method, etc., which have problems such as low purity, low recovery rate, long production cycle, and high toxicity, so the development can be efficient and large-scale production The new process of high-purity ephedrine is of great significance

Method used

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  • Continuous preparation method for extracting ephedrine from ephedra
  • Continuous preparation method for extracting ephedrine from ephedra

Examples

Experimental program
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Effect test

Embodiment 1

[0017] 1) Preparation of Ephedra extract: take 50g of Ephedra root and pulverize it into coarse powder, pass through a 24-mesh sieve, take the coarse powder that has passed through the sieve, and extract with 500 mL of 0.1% formic acid water (V / V) at 100°C under reflux for 1 h for a total of 1 h. Extract 2 times (repeated 1 time), obtain ephedra extract after merging the filtrate, the mass content of ephedrine in the extract is about 2.2%, the mass content of pseudoephedrine, desmethylephedrine and desmethylpseudoephedrine are successively about 0.68%, 0.14 %, 0.20%;

[0018] 2) preparation of permeate: pass the ephedra extract through 750KD hollow fiber ultrafiltration membrane to obtain permeate;

[0019] 3) Preparation of enrichment solution: After equilibrating reversed-phase column 1 (filler is C18HCE, particle size is 7 μm, inner diameter 4.6 mm, column length 250 mm) with 3 column volumes of formic acid water (final volume concentration of formic acid is 0.1%), take Th...

Embodiment 2

[0022] 1) Preparation of Ephedra extract: take 200g of Ephedra root and pulverize it into coarse powder, pass through a 60-mesh sieve, take the coarse powder under the sieve, and extract with 4000mL of 0.5% hydrochloric acid water (V / V) ultrasonic (ultrasonic power 600W, frequency 50kHz) for 1h , extract 3 times, filter to obtain ephedra extract, the mass content of ephedrine in the extract is about 1.7%, and the mass content of pseudoephedrine, desmethylephedrine and desmethylpseudoephedrine are about 0.51%, 0.10%, 0.13% successively;

[0023] 2) Preparation of permeate: the ephedra extract was passed through a 500KD hollow fiber ultrafiltration membrane to obtain permeate;

[0024] 3) Preparation of enrichment solution: After equilibrating the reversed-phase column 1 (filler is C18HCE, particle size is 10 μm, inner diameter 20 mm, column length 250 mm) with 4 times the column volume of formic acid water (the final volume concentration of formic acid is 0.5%), take the step (...

Embodiment 3

[0027] 1) Preparation of Ephedra extract: take 1000g Ephedra root and pulverize it into coarse powder, pass through a 100-mesh sieve, take out the coarse powder, and extract with 15L of 1% acetic acid water (V / V) under reflux for 1.5h, extract twice, and combine the filtrates After obtaining ephedra extract, the mass content of ephedrine in the extract is about 2.4%, and the mass contents of pseudoephedrine, demethylephedrine and demethylpseudoephedrine are about 0.65%, 0.16%, and 0.18% successively;

[0028] 2) preparation of permeate: pass the ephedra extract through 750KD hollow fiber ultrafiltration membrane to obtain permeate;

[0029] 3) Preparation of enrichment solution: reversed-phase column 1 (filler is C18HCE, particle size is 40 μm, inner diameter 50 mm, column length 250 mm) is equilibrated with 5 times the column volume of formic acid water (the final volume concentration of formic acid is 1%), and the step ( 2) The obtained permeate was applied to the above-ment...

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Abstract

The invention provides a method for efficiently separating and purifying four alkaloids such as ephedrine from ephedra. Specifically, an ephedra medicinal material extracting solution passes through an ultrafiltration membrane to obtain a permeate, the permeate is enriched by a reversed-phase column 1 to obtain an enriched solution, and the enriched solution is purified by a reversed-phase column 2 to obtain four alkaloid compounds such as ephedrine and the like. The method is characterized in that a running water type continuous preparation technology for extracting ephedrine from ephedra is introduced, and four alkaloids such as high-purity ephedrine can be obtained only through one-time concentration; according to the method, the content of ephedrine is increased from about 2% to about 24% through enrichment of the reversed-phase column 1, the ephedrine with the purity of 99% is obtained through purification of the reversed-phase column 2, the recovery rate can reach 80%, meanwhile, three alkaloids including pseudoephedrine, demethylated ephedrine and demethylated pseudoephedrine are obtained, and the method is rapid, efficient, easy and convenient to operate and beneficial to industrial production.

Description

technical field [0001] The invention belongs to the field of natural medicine extraction, in particular to an efficient separation method of high-purity ephedrine. Background technique [0002] Ephedra is the dry herbaceous stem of Ephedra sinica Stapf., Ephedra intermedia Schrenk et C.A.Mey. or Ephedra equisetina Bge. Ephedra has a long history of clinical application in traditional Chinese medicine. The effect of reducing swelling is used for colds and colds, chest tightness and asthma, bronchial asthma and other symptoms. Studies have shown that alkaloid compounds are the main medicinal components in ephedra, such as ephedrine, pseudoephedrine, desmethylephedrine, desmethylpseudoephedrine, etc. Among them, ephedrine has the most important medicinal value. [0003] Ephedrine is mainly used to prevent asthma attacks and treat habitual bronchial asthma and other diseases, and the market demand is very large. At present, the separation and purification methods of ephedrine ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C213/10C07C215/30
CPCC07C213/10C07C215/30
Inventor 梁鑫淼刘艳芳姚禹民徐犇金红利
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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