人血浆中红霉胺的LC-MS/MS法测定  

Determination of Erythromycylamine in Human Plasma by LC-MS/MS

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作  者:郭立志[1] 赵曦 杨汉煜 殷立新[1] 任进民[1] 

机构地区:[1]河北医科大学第二医院,河北石家庄050000 [2]中奇制药技术有限公司,河北石家庄050051

出  处:《中国医药工业杂志》2008年第5期362-365,共4页Chinese Journal of Pharmaceuticals

摘  要:建立了LC-MS/MS法测定人血浆中红霉胺的含量。样品用固相萃取提取,采用C18柱,流动相为甲醇-0.5%甲酸水溶液(50∶50),以酚妥拉明为内标,电喷雾离子化,选择正离子多离子反应监测(MRM),检测离子分别为m/z735.7→577.5(红霉胺)和m/z282.2→212.2(内标)。红霉胺在5~1000ng/ml浓度范围内线性关系良好,方法回收率大于93%,提取回收率大于90%,日内和日间RSD小于4.8%。A LC-MS/MS method was established for the determination of erythromycylamine in human plasma. The samples were treated by solid phase extraction with average extraction recovery was above 90%. A C18 column was used with the mobile phase of methanol-0.5 % formic acid (50 : 50), Phentolamine was used as intemal standard. ESI was applied and operated in positive mode, The detected ions were m/z 735,7→577.5 (erythromycylamine) and m/z 282.2→212,2 (phentolamine). The calibration curve was linear in the range of 5 - 1000ng/ml. The average recovery was more than 93 %. The RSDs of inter- and intra-day were less than 4,8 %.

关 键 词:红霉胺 液相色谱-串联质谱 固相萃取 测定 

分 类 号:TQ460.72[医药卫生—药物分析学] O657.63[化学工程—制药化工]

 

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