高效液相色谱-串联质谱法检测清肺止咳散中添加阿奇霉素含量  

Determination of Azithromycin in Qingfeizhikesan Powder by High-performance Liquid Chromatography-tandem Mass Spectrometry

作　　者：章安源 张传津 王洪涛 张琦 陈志强 李有志 魏秀丽 牛华星 杨修镇 薄永恒 刘霄飞 魏茂莲 田学磊 陈玲 ZHANG An-yuan;ZHANG Chuan-jin;WANG Hong-tao;ZHANG Qi;CHEN Zhi-qiang;LI You-zhi;WEI XiU-Li;Niu Hua-xing;YANG Xiu-Zhen;BO Yong-Hen;LIU Xiao-fei;WEI Mao-Lian;TIAN Xue-Lei;CHEN-Ling(Institute of Veterinary Drug Quality Inspection of Shandong Province,Shandong Provincial Key Laboratory of Quality Safety Monitoring and Risk Assessment for Animal Products,Jinan 250022,China;Weifang Customs,Weifang,Shandong 261041,China;Qingdao Xinnuobang Biotechnology Co.Ltd.,Qingdao,Shandong 266000,China)

机构地区：[1]山东省兽药质量检验所,山东省畜产品质量安全监测与风险评估重点实验室,济南250022 [2]潍坊海关,山东潍坊261041 [3]青岛信诺邦生物科技有限公司,山东青岛266000

出　　处：《中国兽药杂志》2021年第9期8-14,共7页Chinese Journal of Veterinary Drug

摘　　要：建立了清肺止咳散中非法添加阿奇霉素的HPLC-MS/MS含量检测方法。样品经乙腈提取稀释后,以Agilent ZORBAX Eclipse Plus C18色谱柱为分离柱,质谱正离子扫描分析测定。结果显示,在5~250 ng/mL范围内线性关系良好(R^(2)=0.9993);方法检出限为25 mg/kg,定量限为50 mg/kg。在50、100、200、500 mg/kg添加水平的回收率为89.1%~98.6%,批内变异系数小于1.6%,批间变异系数为4.1%。本方法灵敏、快速、重现性好,适用于清肺止咳散中非法添加阿奇霉素含量的测定。A HPLC-MS/MS method for the determination of azithromycin illegally added in Qingfei Zhike powder was established.The sample was extracted and diluted with acetonitrile,Agilent ZORBAX Eclipse Plus C18 was used as the separation column,scanned positive ion by mass spectrometry.The results showed that the good linear range was from 5 to 250 ng/mL(R^(2)=0.9993);The detection limit was 25 mg/kg,and the quantitation limit was 50 mg/kg.The analysis of additive concentration 50,100,200,500 mg/kg showed that the recoveries ranged from 89.1%to 98.6%and the coefficient of variation between and within batches were below 4.1%,1.6%.The experiment showed that the method was reliable,sensitive and suitable for the determination of azitromycin added in Qinfeizhikesan powder.

关 键 词：阿奇霉素 清肺止咳散 高效液相色谱-串联质谱法 

分 类 号：S859.796[农业科学—临床兽医学]