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Method for preparing sinomenine hydrochloride injection

A technology of sinomenine hydrochloride and injection, applied in anti-inflammatory agents, pharmaceutical formulations, non-central analgesics and other directions, can solve the problems of complicated benzene recovery, difficult discharge and environmental protection requirements, etc., and achieves simple operation, low pollution, and high yield. high rate effect

Active Publication Date: 2012-07-11
HUNAN ZHENGQING PHARM GRP CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Moreover, the recovery of benzene is relatively complicated, and the emission is difficult to meet the environmental protection requirements.

Method used

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  • Method for preparing sinomenine hydrochloride injection
  • Method for preparing sinomenine hydrochloride injection
  • Method for preparing sinomenine hydrochloride injection

Examples

Experimental program
Comparison scheme
Effect test

experiment example 1

[0068] Experimental example 1: Research on the extraction process of Qingfengteng

[0069] 1. Test purpose

[0070] Through this test, determine the process parameters of the extraction process, such as immersion time, percolation time, extraction times, pH adjustment range, etc., and optimize the process.

[0071] 2. Test materials

[0072] 2.1 Raw material: Qingfeng vine provided by Baoji, Shaanxi

[0073] 2.2 Instrument:

[0074] Percolation tube

[0075] PHS-2F PH meter: Shanghai Jingke Electronic Instrument Factory

[0076] ZF-2 three-purpose ultraviolet instrument: Shanghai Anting Electronic Instrument Factory

[0077] RE-52A Rotary Evaporator: Shanghai Yarong Biochemical Instrument Factory

[0078] SHB-3 circulating water multi-purpose vacuum pump: Zhengzhou Dufu Instrument Factory

[0079] 2.3 Reagent: Hydrochloric acid Zhuzhou Quartz Chemical Co., Ltd.

[0080] Ammonia Changsha Antai Fine Chemical Industry Co., Ltd.

[0081] Chloroform Sinopharm Chemical Reagent Co., Ltd.

[0082] Silic...

experiment example 2

[0128] Experimental example 2: Comparative experiment

[0129] Percolation extraction process 1 in Table 6: Prepared according to the method in Example 1

[0130] Percolation extraction process 2 in Table 6: prepared according to the method of Example 2

[0131] Percolation extraction process 3 in Table 6: Prepared according to the method in Example 3

[0132] The chloroform reflux extraction process in Table 6: According to the Chinese Pharmacopoeia 2010 edition, a 622 page with sinomenine hydrochloride standard.

[0133] The benzene reflux extraction process in Table 6: raw materials are crushed, dried, mixed with slaked lime to be evenly alkalized, placed in an extraction tank, and benzene is added in a fully sealed reflux extraction, concentration, filtration, cooling, and separation to obtain free sinomenine. The HCl was added to the sinomenine to transform into a solution of sinomenine hydrochloride, which was recrystallized with water to obtain the product sinomenine hydrochlori...

Embodiment 1

[0139] 200g Caulis serrata was dried and crushed for 20 meshes. Add 0.3mol / L HCl 160ml and stir evenly in a beaker. After wetting for 6 hours, place it in a percolation cylinder and add 0.3mol / L hydrochloric acid to cover the liquid surface. 10cm, after immersing for 24 hours, start percolating at a rate of 2 to 3 ml / min. After 24 hours, collect the percolate, add lime milk to adjust the pH to 11.3, filter, and then use HCl to adjust the pH to 8.8. Extracted with chloroform 4 times, the lower chloroform solution was dehydrated and concentrated under reduced pressure, the solvent was recovered, and the concentrated solution was adjusted to pH 2 with 6 mol / L hydrochloric acid, stirred, cooled and filtered to obtain crude sinomenine hydrochloride;

[0140] Take 5.8g crude sinomenine hydrochloride, heat it with 95% ethanol 90ml to reflux, stir to dissolve, add 0.24g activated carbon, keep refluxing for 30 minutes, filter while hot, concentrate the filtrate to 1 / 5, cool, crystallize, f...

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Abstract

The invention provides a preparation method of a sinomenine hydrochloride injection, which adopts the step of preparing sinomenine hydrochloride with a percolation method. The preparation method has the advantages that the method is simple in operation, cold treatment is employed and heating is obviated in an extraction process, the yield is high, mother liquor treatment is simple, and the methodhas good safety and reliability, low pollution and positive effect on environmental protection.

Description

Technical field [0001] The invention relates to a preparation method of sinomenine hydrochloride injection, in particular to a method for extracting the active ingredient sinomenine hydrochloride from Sinomenium sinomenine by percolation method to prepare sinomenine hydrochloride injection. Background technique [0002] Qingfengteng is a commonly used traditional Chinese medicine. It is the dry cane of the Chinese fangchi family plant Qingteng and Mao Qingteng. It has been recorded as early as in the Compendium of Materia Medica. It is now included in the 2010 edition of the Pharmacopoeia of the People’s Republic of China. Meridians and urination are used to treat rheumatic arthralgia, joint swelling, numbness and itching, as well as anti-arrhythmic and lowering blood pressure. [0003] The main component of sinomenine is alkaloids. The components that have been discovered are Sinomenine, Igoginomenine, SinoAcutine, Acutumidine, and Acutumidine. Sinaetine and Diginomenine, ethylsi...

Claims

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Application Information

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IPC IPC(8): A61K9/08A61K31/485A61K31/473A61P29/00A61P19/02A61P19/08A61P9/06C07D221/28C07D221/18
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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