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Organic solvent-free preparation method of sinomenine hydrochloride cataplasm

A technology of sinomenine hydrochloride and cataplasm, which is applied in the field of preparation of sinomenine hydrochloride cataplasm, which can solve the problems of high cancer-controlling rate, achieve high purity, reduce investment, and reduce potential harm

Active Publication Date: 2013-06-26
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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  • Organic solvent-free preparation method of sinomenine hydrochloride cataplasm
  • Organic solvent-free preparation method of sinomenine hydrochloride cataplasm
  • Organic solvent-free preparation method of sinomenine hydrochloride cataplasm

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Experimental program
Comparison scheme
Effect test

experiment example 1

[0027] Experimental example 1: Study on the extraction process of Qingfengteng non-organic solvent

[0028] 1. Experimental method

[0029] 1.1 Materials and Instruments

[0030] Qingfengteng crude powder, macroporous adsorption resin, sinomenine hydrochloride reference substance, hydrochloric acid, ammonia water, sodium hydroxide, ethanol, sodium chloride, etc.

[0031] Glass column (diameter 3cm, height 30-40cm), HPLC high-performance liquid phase detector, rotary evaporator.

[0032] 1.2 Methods and results

[0033] 1.2.1 Judgment method

[0034] (1) Selection of alkaloid indicator

[0035] 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

[0092] Embodiment 1: a kind of preparation method of the sinomenine hydrochloride cataplasm of non-organic solvent, the method comprises the steps:

[0093] 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;

[0094] 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 ...

Embodiment 2

[0099] Embodiment 2: a kind of preparation method of the sinomenine hydrochloride cataplasm of non-organic solvent, the method comprises the steps:

[0100] 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;

[0101] 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, soa...

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Abstract

The invention provides a preparation method of sinomenine hydrochloride cataplasm. The preparation method of sinomenine hydrochloride cataplasm adopts cation exchange resin or macroporous adsorption resin to replace conventional benzene extraction and chloroform extraction processes with large toxicity. The method is high in extraction yield and simple in operation, avoids harm and pollution of large amount of toxic organic solvent to operator health and environment, reduces treatment process of organic solvent, benefits environment protection and environment-friendly production, and reduces input of factory environment-protection facilities. The sinomenine hydrochloride extracted and separated by the inventive method, as a pharmaceutical material, has higher purity, no solvent residue, and reduced potential harm to human body.

Description

technical field [0001] The invention relates to a preparation method of a sinomenine hydrochloride cataplasm, in particular to a method for extracting the active ingredient sinomenine hydrochloride cataplasm in Caulis chinensis by a 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 t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): A61K9/70A61K31/473A61K47/44A61P29/00A61P19/02A61P19/08A61P9/06
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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