Method for preparing sinomenine hydrochloride slow release injection
A technology of sinomenine hydrochloride and sustained-release 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 and processing. , the effect of high yield
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experiment example 1
[0064] Experimental example 1: Study on the extraction process of Tengteng chinensis
[0065] 1. Purpose of the test
[0066] 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.
[0067] 2. Test materials
[0068] 2.1 Raw materials: Qingfengteng provided by Baoji, Shaanxi
[0069] 2.2 Instruments:
[0070] Percolation cylinder;
[0071] PHS-2F PH meter: Shanghai Jingke Electronic Instrument Factory
[0072] ZF-2 three-purpose UV instrument: Shanghai Anting Electronic Instrument Factory
[0073] RE-52A rotary evaporator: Shanghai Yarong Biochemical Instrument Factory
[0074] SHB-3 circulating water multi-purpose vacuum pump: Zhengzhou Dufu Instrument Factory
[0075] 2.3 Reagent: hydrochloric acid Zhuzhou Quartz Chemical Co., Ltd.
[0076] Ammonia Changsha Antai Fine Chemical Industry Co., Ltd.
[0077] Chloroform Sinopha...
experiment example 2
[0123] Experimental Example 2: Comparative Experiment
[0124] Percolation extraction process 1 in Table 6: Prepared according to the method of Example 1
[0125] Percolation extraction process 2 in Table 6: prepared according to the method of Example 2
[0126] Percolation extraction process 3 in Table 6: Prepared according to the method of Example 3
[0127] The chloroform reflux extraction process in Table 6: according to the Chinese Pharmacopoeia 2010 edition one 622 pages attached sinomenine hydrochloride standard.
[0128] 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. ...
Embodiment 1
[0135] 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;
[0136] 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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