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New method for picking-up alkakoid of Chinese ephedra in large scale

An ephedrine alkaloid, large-scale technology, applied in the directions of alkaloids, alkaloids, chemical instruments and methods, etc., to achieve the effects of increasing extraction rate, short extraction time and good adsorption effect

Inactive Publication Date: 2005-03-30
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

It can be seen that this method also has certain shortcomings.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] After pulverizing 25 grams of Ephedra herbae, add 100 ml of water, extract with a frequency of 20KHz and a power of 50W for 30 minutes, filter to remove the medicinal residues; use 0.5N NaOH to adjust the pH of the leachate to 9, and pass the filtrate through the chemical plant of Nankai University to produce D151 weakly acidic cation exchange resin. After the exchange, elute with 0.01N hydrochloric acid, and concentrate the eluent under reduced pressure to obtain ephedrine hydrochloride crystals; the resin column can be used repeatedly after being washed with 10% ethanol, and the ethanol can be recovered under reduced pressure. By adopting the technology, the content of ephedrine before sample loading is increased from 4.9% to more than 90%, the purity is increased by 18.5 times, and the recovery rate is 96%.

Embodiment 2

[0031] After crushing 25 grams of Ephedra herbaceae, add 100 milliliters of 0.001N hydrochloric acid solution, use a frequency of 20KHz and a power of 50W for ultrasonic extraction for 30 minutes, filter and remove the medicinal residues; use 0.5N NaOH to adjust the pH of the leachate to 14, pass the filtrate through Rohm&Haas company Amberlite XAD-7 macroporous resin column. After the adsorption is complete, elute with a 2:1 mixed solution of 0.01N hydrochloric acid and ethanol. Concentrate the eluent under reduced pressure to obtain crystals of ephedrine hydrochloride; the resin column can be used repeatedly after being washed with 10% ethanol, and the ethanol can be recovered under reduced pressure. By adopting the technology, the content of ephedrine before sample loading is increased from 5.5% to more than 85%, the purity is increased by 14.8 times, and the recovery rate is 97%.

Embodiment 3

[0033] After crushing 25 grams of Ephedra herbae, add 100 milliliters of 0.005N sodium hydroxide solution, use a frequency of 20KHz and a power of 50W for ultrasonic extraction for 30 minutes, filter and remove the medicinal residues; use 0.5N NaOH to adjust the pH of the leachate to 10, pass the filtrate through Amberlite XAD-7 macroporous resin column from Rohm&Haas Company. After the exchange is completed, elute with a 3:1 mixture of 0.002N hydrochloric acid and acetone, and concentrate the eluate under reduced pressure to obtain ephedrine hydrochloride crystals; the resin column can be used repeatedly after being washed with 10% ethanol, and ethanol can be used under reduced pressure. Recycle. By adopting the technology, the content of ephedrine before sample loading is increased from 4.1% to more than 78%, the purity is increased by 18.9 times, and the recovery rate is 95%.

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Abstract

A process for extracting ephedra alkaloid including ephedrine, pseudoephedrine, methyl ephedrnie, demethyl ephedrine incldues such steps as pulverization fresh and drying ephedrine, soaking in solvent, releasing ephedrine alkaloid by outside field including microwave, ultrasonic wave, electromagnetic field etc, extracting, separating by solid mediator adsorbent, precipitation, crystallization and purifying.

Description

technical field [0001] The invention relates to a production method for large-scale extraction of ephedra alkaloids including ephedrine, pseudoephedrine, methylephedrine, demethylpseudoephedrine and the like. Background technique [0002] As a traditional Chinese medicine, ephedra has a history of more than 4,000 years of application. The medicinal species are mainly grass ephedra, horsetail ephedra and middle ephedra. It mainly has the effects of sweating, relieving asthma, diuresis, and removing wind. It can cure wind-cold cold, fever and chills, no sweat, whooping cough, bronchitis, bronchial asthma and other diseases. Its main active ingredients are (-) ephedrine and (+) pseudoephedrine, two nitrogen-containing methyl alkaloids, whose structure is similar to that of epinephrine. Since the use of PPA-containing drugs has been suspended at home and abroad, ephedrine, as the best substitute for PPA, has a net increase of more than 200 tons in the domestic market alone, a...

Claims

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Application Information

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IPC IPC(8): C07C213/10C07C215/30C07G5/00
Inventor 查丽杭苏志国廖小雪
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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