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Method for preparing sinomenine hydrochloride by using non-organic solvent

A non-organic technology of sinomenine hydrochloride, which is applied in the field of preparation of sinomenine hydrochloride, can solve the problem of high carcinogenesis rate, and achieve the effects of high purity, environmental protection, and no solvent residue

Active Publication Date: 2012-07-25
HUNAN ZHENGQING PHARM GRP CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

(Chen Yukun's "Chinese Medicine Extraction Technology", 1992), the existing methods all use very toxic benzene or chloroform as the extraction solvent, and benzene is a first-class toxic solvent with a high carcinogenesis rate, which has been banned in the pharmaceutical industry, and in The recovery and treatment of solvents requires a very complicated process to meet environmental protection requirements, and chloroform is a secondary toxic reagent, so benzene and chloroform solvents should be avoided as much as possible in the extraction of traditional Chinese medicine

Method used

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  • Method for preparing sinomenine hydrochloride by using non-organic solvent
  • Method for preparing sinomenine hydrochloride by using non-organic solvent
  • Method for preparing sinomenine hydrochloride by using non-organic solvent

Examples

Experimental program
Comparison scheme
Effect test

experiment example 1

[0018] Experimental example 1: Study on the extraction process of Qingfengteng non-organic solvent

[0019] 1. Experimental method

[0020] 1.1 Materials and Instruments

[0021] Qingfengteng crude powder, macroporous adsorption resin, sinomenine hydrochloride reference substance, hydrochloric acid, ammonia water, sodium hydroxide, ethanol, sodium chloride, etc.

[0022] Glass column (diameter 3cm, height 30-40cm), HPLC high-performance liquid phase detector, rotary evaporator.

[0023] 1.2 Methods and results

[0024] 1.2.1 Judgment method

[0025] (1) Selection of alkaloid indicator

[0026] Prepare three alkaloid indicators, bismuth potassium iodide dilute solution, alkaline potassium ferricyanide, and silicotungstic acid test solution, according to the method in Part One of the Chinese Pharmacopoeia 2010 edition, and take 1 to 2 drops respectively in the test solution for precipitation, The color reaction, compared with previous experiments, shows that the indication ...

Embodiment 1

[0084] Embodiment one: a kind of preparation method of the sinomenine hydrochloride of non-organic solvent, this method comprises the steps:

[0085] A. Extraction: 500kg of Qingfengteng coarse powder, wet with 500L of 0.5mol / L HCl for 3 hours, install the percolation cylinder, add 0.5mol / L HCl to make the liquid surface cover the powder by 2cm, soak for 12 hours, press Start percolation at a speed of 3ml / min, stop percolation after 12 hours, obtain percolation liquid, and set aside;

[0086] B. Column elution: Put the treated cation exchange resin or 152 type resin on the percolation liquid, the ratio of diameter to height is 1:10, and the sample loading speed is 3 times the column volume / hour, until the effluent is tested with silicotungstic acid If there is precipitation in the liquid inspection, stop loading the sample when there is no alkaloid spot detected by thin-layer chromatography, and stop when the eluent is eluted with purified water until the eluent has no color, ...

Embodiment 2

[0088] Embodiment two: a kind of preparation method of the sinomenine hydrochloride of non-organic solvent, this method comprises the steps:

[0089] A. Extraction: 800kg of Qingfengteng coarse powder, wet it with 1000L of 0.9mol / L HCl for 5 hours, install the percolation cylinder, add 0.9mol / L HCl to make the liquid surface cover the powder by 2cm, after soaking for 20 hours, press Start percolation at a speed of 5ml / min, stop percolation after 24 hours, obtain percolation liquid, and set aside;

[0090] B. Column elution: put the treated cation exchange resin 001*4 type or 152 type resin on the percolation liquid, the ratio of diameter to height is 1:10, and the loading speed is 5 times the column volume / hour, until the effluent is used If there is precipitation in the silicotungstic acid test solution, stop loading the sample when there is no alkaloid spot detected by thin-layer chromatography, and stop when the eluent is colorless by elution with purified water, soak the r...

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Abstract

The invention provides a preparation method of sinomenine hydrochloride. The method comprises the steps of: A) extraction: wetting caulis sinomenii coarse powder by using hydrochloric acid (HCl), installing a percolator, adding HCl for impregnation and percolation to obtain percolate; B) eluting treated cation exchange resin or 152 resin on the percolate by using ammonia water-ethanol solution or HCl with concentration being 3-10 percent, desalting, condensing and drying to obtain sinomenine hydrochloride crude products; and C) taking the sinomenine hydrochloride crude products, heating the crude products in ethanol or purified water for back flowing, condensing filtrate, cooling, crystallizing, filtering and using ethanol to wash a filter cake to obtain the sinomenine hydrochloride. Since the method adopts an absorbing process through the cation exchange resin or large-pore absorbing resin to replace the traditional extraction process through high-toxicity benzene and chloroform, the extraction rate is high, the method is simpler and convenient to operate, the harm and the pollution caused by high quantity of high-toxicity organic solvent to operator health and the environment can be avoided, the treatment process of the organic solvent is reduced, the environmental protection is further facilitated, the investment in environmental protection facilities of a factory is reduced and the environmental-friendly production is facilitated. The sinomenine hydrochloride prepared by adopting the method through extraction and separation can be used as a raw material for pharmaceutical preparations, the purity is higher, solvent residue does not exists and the potential harm to human bodies is reduced.

Description

technical field [0001] The invention relates to a preparation method of sinomenine hydrochloride, in particular to a method for extracting the active ingredient sinomenine hydrochloride in Caulis chinensis by non-organic solvent. Background technique [0002] Qingfengteng is a traditional Chinese medicine commonly used in traditional Chinese medicine. It is the dry cane of Fangjiaceae plants Qingteng and Ivy twig. Meridian, urination effect, used to treat rheumatic arthralgia, joint swelling, numb itching, anti-arrhythmia and antihypertensive effects. [0003] The main components in C. chinensis are alkaloids. The components that have been found so far are Sinomenine, Igoginomenine, SinoAcutine, Acutumidine, and Acutumine. Sinaetine and Diginomenine, Ethylsinomenine, Sinactine, Tetrahydroepiperberine, Bat Pueroline, Bat Ge Ning, Tetrahydropalmatine et al. [0004] Sinomenine (Sinomenine) is an alkaloid monomer extracted from Teng chinensis. It is the main active ingredien...

Claims

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Application Information

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IPC IPC(8): C07D221/28
Inventor 吴飞驰仇萍文迎艺滕健许李董绍象彭祖仁王小伟
Owner HUNAN ZHENGQING PHARM GRP CO LTD
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