复方乙酰水杨酸片质量标准研究  

Study on the quality standard of compound acetylsalicylic acid tablets

作　　者：陈承贵 刘敏 李美芳 庞发根 李玉兰 王铁杰 CHEN Cheng-gui;LIU Min;LI Mei-fang;PANG Fa-gen;LI Yu-lan;WANG Tie-jie(Shenzhen Institute for Drug Control,Shenzhen Key Laboratory of Drug Quality Standard Research,Shenzhen 518057,China)

机构地区：[1]深圳市药品检验研究院,深圳市药品质量标准研究重点实验室,深圳518057

出　　处：《药物分析杂志》2021年第3期515-524,共10页Chinese Journal of Pharmaceutical Analysis

基　　金：2016年国家药典委员会药品标准提高课题(309)。

摘　　要：目的:完善复方乙酰水杨酸片的质量标准,提高其质量控制水平。方法:采用《中华人民共和国药典》2015年版四部相关方法和拟定标准方法,对复方乙酰水杨酸片拟定的质控项目进行检验,建立复方乙酰水杨酸片的薄层色谱鉴别方法,建立HPLC同时测定HPLC鉴别(1)、游离水杨酸、溶出度、含量均匀度和含量测定的方法,同时以3个主成分为目标,建立了该片剂的溶出度方法。结果:HPLC鉴别和薄层色谱鉴别专属性强,简便快速;建立了HPLC测定游离水杨酸、溶出度、含量均匀度和含量测定,其线性关系均较好,重复性良好,回收率均符合要求。9批次复方乙酰水杨酸片的游离水杨酸含量为0.1%~0.3%,含量均匀度(咖啡因)结果为98.0%~102.9%,含量测定(乙酰水杨酸)结果为97.9%~101.7%,含量测定(非那西丁)结果为98.1%~103.9%,含量测定(咖啡因)结果为96.8%~103.1%,溶出度结果大多在79%~101%之间,部分企业溶出度检测不合格;建议游离水杨酸限度修订为0.3%,溶出度限度均为75%。结论:本研究完善和提高了复方乙酰水杨酸片的质量控制方法。Objective:To improve the quality standard of compound acetylsalicylic acid tablets and improve its quality control level.Methods:The proposed quality control items of compound acetylsalicylic acid tablets were determined according to the ChP(2015 edition,volume 4).The TLC identification method were established.The HPLC method for HPLC identification(1),free salicylic acid,dissolution,content uniformity and content determination were established at the same time.The tablets dissolution method were established with three principal components in compound acetylsalicylic acid tablets.Results:The methods of HPLC identification(1)and TLC identification(2)were specific,simple and rapid.The HPLC methods for determination of free salicylic acid,dissolution,content uniformity and content determination were established,their linearity and repeatability were good.The recovery results were conformed to the requirements.The ranges for the free salicylic acid contents and content uniformity(caffeine)of 9 batches were 0.1%-0.3% and 98.0%-102.9%.The ranges for the content determination of acetyl salicylic acid,phenacetin and caffeine were 97.9%-101.7%,98.1%-103.9% and 96.8%-103.1% respectively.The dissolution of aspirin phenacetin and caffeine(APC)were mostly between 79%-101%.Dissolution results from some companies were failed.The limit of each test items for compound acetylsalicylic acid tablets were proposed as follows:limit of free salicylic acid was 0.3%,the dissolution limit of APC was 75%.Conclusion:The established method improves the quality control of compound acetylsalicylic acid tablets.

关 键 词：复方乙酰水杨酸片 质量标准 高效液相色谱 薄层色谱鉴别 溶出度 含量测定 

分 类 号：R917[医药卫生—药物分析学]