尿液中杀它仗的高效液相色谱-串联质谱测定研究  

Determination of flocoumafen in urine by high-performance liquid chromatography with tandem mass spectrometry

作　　者：陈晓红[1] 姚浔平[1] 金米聪[1] 

机构地区：[1]浙江省宁波市疾病预防控制中心,浙江宁波315010

出　　处：《中国卫生检验杂志》2007年第8期1423-1424,共2页Chinese Journal of Health Laboratory Technology

基　　金：宁波市医学科技计划项目(2004056)

摘　　要：目的：建立尿液中测定杀它仗的高效液相色谱-串联质谱联用检测方法.方法：尿液酸化后经固相萃取浓缩、净化,采用XDB C18柱（150 mm×2.1 mm i.d.,5 μm）;流速：0.5 ml/min;柱温：30℃;流动相：甲醇＋0.2%乙酸（88＋12）;通过电喷雾电离离子化在多离子反应监测技术（MRM）模式下测定.结果：在0.002～0.5 mg/L范围内呈良好的线性关系,平均回收率为98.5%,其批内精密度小于6.0%,批间精密度小于6.5%,定量检出限为0.087 ng.结论：本方法简便、灵敏、重现性好、专属性强,能满足杀它仗中毒病人的诊断要求.Objective ：To establish a HPLC/MS/MS method for determination of flocoumafen in urine. Methods：After flocoumafen in urine acided with phosphoric acid, it was concentrated and cleaned with solid- phase extraction （SPE） using LC -18 cartridges. Then the sample was separated on ZORBAX Eclipse XDB C18 （150 mm× 2. 1 mm i. d. , 5 μm） at a constant temperature of 30℃ by using a mobile phase consisting of CH3OH （88%） and 0. 2% CH3COOH （ 12% ）. The flow rate was 0. 5 ml/ min. Detection was performed on negative electrospray ionization in the multi - reaction monitoring （MRM） mode. Results： Calibration curve was linear within the range of 0. 002 ～ 0. 5 mg/L and the limit of quantification was found to be 0. 087 ng. The average recovery was 98. 5% and the within and between - batch RSD were less than 6.0% and 6. 5%, respectively. Conclusion： This method is simple, sensitive and accurate for the determination of fiocoumafen in poisoned patients.

关 键 词：尿液 杀它仗 高效液相色谱-串联质谱 

分 类 号：O657.63[理学—分析化学]