Preparation method of sinomenine

A technology of sinomenine hydrochloride and Qingfeng, which is applied in the field of preparation of sinomenine hydrochloride, can solve the problems of cumbersome recovery of benzene, difficult discharge and environmental protection requirements, and achieve the effect of simple operation, simple treatment and high yield

Active Publication Date: 2012-04-04
HUNAN ZHENGQING PHARM GRP CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Moreover, the recovery of benzene is relatively complicated, and the e

Method used

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  • Preparation method of sinomenine

Examples

Experimental program
Comparison scheme
Effect test

experiment example 1

[0059] Experimental example 1: Study on the extraction process of Tengteng chinensis

[0060] 1. Purpose of the test

[0061] Through this experiment, the process parameters of this extraction process are determined, such as soaking time, percolation time, extraction times, pH adjustment range, etc., to optimize the process.

[0062] 2. Test materials

[0063] 2.1 Raw materials: Qingfengteng provided by Baoji, Shaanxi

[0064] 2.2 Instruments:

[0065] Percolation cylinder;

[0066] PHS-2F PH meter: Shanghai Jingke Electronic Instrument Factory

[0067] ZF-2 three-purpose UV instrument: Shanghai Anting Electronic Instrument Factory

[0068] RE-52A rotary evaporator: Shanghai Yarong Biochemical Instrument Factory

[0069] SHB-3 circulating water multi-purpose vacuum pump: Zhengzhou Dufu Instrument Factory

[0070] 2.3 Reagent: hydrochloric acid Zhuzhou Quartz Chemical Co., Ltd.

[0071] Ammonia Changsha Antai Fine Chemical Industry Co., Ltd.

[0072] Chloroform Sinopha...

experiment example 2

[0118] Experimental Example 2: Comparative Experiment

[0119] Percolation extraction process 1 in Table 6: Prepared according to the method of Example 1

[0120] Percolation extraction process 2 in Table 6: prepared according to the method of Example 2

[0121] Percolation extraction process 3 in Table 6: Prepared according to the method of Example 3

[0122] The chloroform reflux extraction process in the table six: by Chinese Pharmacopoeia 2010 edition one 622 pages attached sinomenine hydrochloride standard.

[0123] The benzene reflux extraction process in Table 6: the raw materials are pulverized, dried and mixed with slaked lime for uniform alkalization, put into the extraction tank, add benzene, fully seal and reflux, extract and concentrate, filter, cool, and separate to obtain free sinomenine. HCl is added to the perine to convert it into a sinomenine hydrochloride solution, and then recrystallized with water to obtain the product sinomenine hydrochloride.

[0124...

Embodiment 1

[0129] 200g of Qingfengteng is dried and crushed through 20 meshes, add 160ml of 0.3mol / L HCl and stir evenly in a beaker, after wetting for 6 hours, put it in the percolation drum, add 0.3mol / L hydrochloric acid to cover the liquid surface After soaking for 24 hours, start to percolate at a speed of 2-3ml / min. After 24 hours, collect the percolation liquid, add lime milk to adjust the pH value to 11.3, filter, and then use HCl to adjust the pH value to 8.8. Extracted 4 times with chloroform, the chloroform solution in the lower layer was dehydrated, concentrated under reduced pressure, recovered the solvent, adjusted the pH value of the concentrated solution to 2 with 6mol / L hydrochloric acid, stirred, cooled and filtered to obtain the crude product of sinomenine hydrochloride;

[0130] Take 5.8g of the crude product of sinomenine hydrochloride, heat it to reflux with 90ml of 95% ethanol, add 0.24g of activated carbon after stirring and dissolving, keep it warm and reflux for ...

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Abstract

The invention provides a preparation method of sinomenine, comprising the process for preparing and refining a sinomenine crude product. The preparation method provided by the invention comprises the following steps of: wetting and percolating caulis sinomenii coarse powder with HCL (hydrochloric acid), and extracting and crystallizing the percolation liquid to obtain a sinomenine crude product; and adding ethanol or purified water in the sinomenine crude product and heating and refluxing till the sinomenine crude product is dissolved, adding active carbon for filtering, then cooling, crystallizing, filtering and cleaning a filter cake with ethanol till the filtrate is colorless, and thus obtaining the sinomenine. The preparation method is simple to operate, belongs to cold treatment completely without the need of needs heating in the extraction process; the yield is high, and mother liquid is treated simply; moreover, the preparation method is safe and reliable, causes low pollution and plays a positive effect on environmental protection because only inorganic acid and alkali and a mall amount of level-two toxicity solvent are used.

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 percolation. Background technique [0002] Qingfengteng is a traditional Chinese medicine commonly used in traditional Chinese medicine. It is the dry cane of the anti-healing plants Qingteng and Ivy, which has been recorded in "Compendium of Materia Medica" and is now included in the 2010 edition of "Pharmacopoeia of the People's Republic of China". It has the functions of expelling wind, The effect of clearing the meridians and urinating is used to treat rheumatic arthralgia, joint swelling, numbness and itching, as well as 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...

Claims

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Application Information

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IPC IPC(8): C07D221/28
Inventor 仇萍文迎艺滕健彭祖仁唐顺之
Owner HUNAN ZHENGQING PHARM GRP CO LTD
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