摘要
目的建立长春西汀原料药细菌内毒素的检查方法。方法依据2020年版《中国药典(四部)》附录1143建立长春西汀原料药细菌内毒素的检测限;分别以盐酸和酒石酸作溶解剂,并优化稀释步骤,防止稀释过程中样品析出,采用光度测定法干扰试验对溶解剂和稀释步骤进行方法学验证,并用试验确定的条件,采用凝胶法对不同批号的样品进行干扰试验和细菌内毒素检查。结果用细菌内毒素检查用水溶解长春西汀和酒石酸,并稀释120倍,再用Tris缓冲液将样品溶液稀释至480倍,凝胶法和光度测定法干扰试验均符合规定,可排除干扰,且3批供试品内毒素含量均小于1.67 EU/mg。结论所建立的方法可用于长春西汀原料药细菌内毒素检查。
Objective To establish a method for bacterial endotoxin test of vinpocetine active pharmaceutical ingredients(API).Methods According to appendix 1143 of the Chinese Pharmacopoeia(2020 Edition),the limit of detection(LOD)of bacterial endotoxin in vinpocetine API was established.Hydrochloric acid and tartaric acid were selected as the dissolving agent respectively,and the dilution steps were optimized to prevent the precipitation of the samples during dilution.The photometric interference test was used to verify the dissolving agent and dilution steps.The interference test and bacterial endotoxin test of different batches of samples were carried out by gel method through the conditions determined in this test.Results The vinpocetine and tartaric acid were dissolved with bacterial endotoxin test water,and diluted by 120 times,and then the sample solution was diluted to 480 times by Tris buffer solution,in which the gel method and photometric interference test both met the requirements,which could eliminate the interference.The content of endotoxin in the three batches of test products was less than 1.67 EU/mg.Conclusion The established method can be used for bacterial endotoxin test of vinpocetine API.
作者
陈晨
裴宇盛
杜颖
蔡彤
高华
CHEN Chen;PEI Yusheng;DU Ying;CAI Tong;GAO Hua(National Institutes for Food and Drug Control,Beijing,China 102629)
出处
《中国药业》
CAS
2021年第22期78-81,共4页
China Pharmaceuticals
基金
国家科技重大专项(民口)课题[2018ZX09101-001]。
关键词
长春西汀
难溶性药物
细菌内毒素
检查方法
vinpocetine
poorly water-soluble drug
bacterial endotoxin
test method
