HPLC-MS/MS法对双氯芬酸钠多种杂质的定量检测  

Quantitative detection of various impurities in diclofenac sodium by HPLC-MS/MS

作　　者：刘雨阳 范志熊 王兰 谷俊尧 蔡强 彭缨[4] LIU Yuyang;FAN Zhixiong;WANG Lan;GU Junyao;CAI Qiang;PENG Ying(School of Traditional Chinese Materia Medica,Shenyang Pharmaceutical University,Benxi 117004,China;Zhuhai Rundu Pharmaceutical Co.,Ltd,Zhuhai 519040,China;Shenyang Pharmaceutical LeiYunshang Pharmaceutical Co.,Ltd,Benxi 117004,China;Wuya College of Innovation,Shenyang Pharmaceutical University,Shenyang 110016,China)

机构地区：[1]沈阳药科大学中药学院,辽宁本溪117004 [2]珠海润都制药股份有限公司,深圳珠海519040 [3]沈阳药大雷允上药业有限责任公司,辽宁本溪117004 [4]沈阳药科大学无涯创新学院,辽宁沈阳110016

出　　处：《沈阳药科大学学报》2025年第2期191-198,共8页Journal of Shenyang Pharmaceutical University

摘　　要：目的建立HPLC-MS/MS法,对双氯芬酸钠原料药的杂质进行定性和定量,为双氯芬酸钠原料药的质量控制提供参考依据。方法采用HPLC-Q TOF MS法对双氯芬酸钠原料药的杂质种类进行分析,进而建立HPLC-QQQ MS法对双氯芬酸钠原料药的多种杂质进行含量测定,并进行方法学验证,分别对珠海润都制药股份有限公司提供的三个批次的双氯芬酸钠原料药杂质进行检测,并对双氯芬酸钠原料药进行含量测定。结果三个批次双氯芬酸钠原料药的杂质A的含量分别为0.30‰,0.33‰,0.28‰;杂质B的含量分别为10.01、13.34、12.82 mg·kg^(-1);杂质C的含量分别为10.35、14.14、11.29 mg·kg^(-1)。三批原料药中双氯芬酸钠的百分含量分别为99.81%(RSD=0.90%)、98.88%(RSD=0.50%)、99.03%(RSD=0.71%)。结论双氯芬酸钠原料药的杂质分析方法的建立,可以有效对此类杂质进行针对性地控制,为双氯芬酸钠原料药的质量控制提供参考依据。Objective A HPLC-MS/MS method was established to determine and quantify a variety of impurities of diclofenac sodium API,providing reference for the quality control of diclofenac sodium API.Methods LC-Q TOF MS method was established to analyze the impurities of diclofenac sodium API.The LC-QQQ MS method was further established to determine the content of various impurities in diclofenac sodium API,and the methodology was verified.Three batches of diclofenac sodium APIs provided by Zhuhai Rundu Pharmaceutical Co.,Ltd.were tested for impurities,and the content of diclofenac sodium APIs were determined.Results The contents of impurity A in the three batches of diclofenac sodium APIs were 0.30‰,0.33‰ and 0.28‰ respectively;the contents of impurity B were 10.01,13.34 and 12.82 mg·kg^(-1);the contents of impurity C were 10.35,14.14 and 11.29 mg·kg^(-1).The percentages of diclofenac sodium in the three batches of APIs were 99.81%(RSD=0.90%),98.88%(RSD=0.50%)and 99.03%(RSD=0.71%).Conclusion The impurity analysis method of diclofenac sodium API has been established,which can effectively control such impurities and provide a reference for the quality control of diclofenac sodium API.

关 键 词：双氯芬酸钠 杂质 液相质谱联用法 

分 类 号：R917[医药卫生—药物分析学]