生物样品中痕量敌鼠和氯鼠酮的高效液相色谱/质谱联用法同时测定研究  

Simultaneous detection of trace diphacinone and chlorophacinone in biological sample by high-performance liquid chromatography coupled with mass spectrometry

作　　者：陈晓红[1] 徐明敏[2] 范建中[1] 金米聪[1] 

机构地区：[1]浙江省宁波市疾病预防控制中心宁波市毒物研究与控制重点实验室,浙江宁波315010 [2]浙江省宁波市北仑区疾病预防控制中心,浙江宁波315080

出　　处：《中国卫生检验杂志》2009年第8期1716-1719,共4页Chinese Journal of Health Laboratory Technology

基　　金：浙江省医药卫生优秀青年科技人才专项基金(2007QN014);宁波市自然科学基金(2007A610072);宁波市农业与社会发展基金(2007C10084)

摘　　要：目的：建立生物样品中敌鼠和氯鼠酮的高效液相色谱/质谱联用同时测定方法。方法：全血样品经甲醇＋乙腈（50＋50,v/v）提取,尿液样品经Oasi sHLB固相萃取小柱净化富集后,采用Extend C18柱（150 mm×4.6 mm i.d.,5μm）,以乙酸铵-乙酸（0.02 mol/L,pH 5.5）＋甲醇（15＋85,v/v）为流动相,采用选择离子监测（SIM）技术在电喷雾电离（ESI）负离子模式下同时检测,敌鼠和氯鼠酮的定量检测离子分别为m/z 339.0[M-H]-和m/z 373.0[M-H]-,外标法定量。结果：针对全血样品,敌鼠在2.0-500.0μg/L,氯鼠酮在1.0-200.0μg/L范围内呈良好线性关系,敌鼠和氯鼠酮的回收率分别在92.1%-94.5%和93.0%-94.2%范围,RSD分别小于7.5%和6.5%,检出限分别为2.0μg/L和1.0μg/L。针对尿液样品,敌鼠在0.5-100.0μg/L,氯鼠酮在0.2-40.0μg/L范围内呈良好线性关系,敌鼠和氯鼠酮的回收率分别为95.2%-97.0%和92.0%-96.5%,RSD分别小于6.0%和7.5%,检出限分别为0.5μg/L和0．2μg／L。结论：本方法简便、灵敏、莺现性好，能满足敌鼠和氯鼠酮中毒病人的临床诊断检测要求。Objective： To establish a method for the simultaneous detection of diphacinone and chlorophacinone in biological sample by high-performance liquid chromatography coupled with mass spectrometry（LC-MS）.Methods：After the whole blood was extracted by methanol＋acetonitrile（50＋50,v/v） and urine was cleaned and enriched by Waters OasisHLB SPE cartridges,the samples were separated on an Extend C18 column（150 mm×4.6 mm i.d.,5 μm）by using the mobile phase consisting of ammonium acetate-acetate acid（0.02 mol/L,pH 5.5）＋methanol（15＋85,v/v）.Detection was carried out by LC-MS using a negative electrospray ionization interface in the selected ion monitoring（SIM） mode.Quantified ions were selected for their molecular ions,m/z 339.0-for diphacinone,m/z 373.0-for chlorophacinone.Results：Calibration curves of the whole blood were linear within the range of 2.0500.0 μg/L and 1.0200.0 μg/L,and the limits of quantification were 2.0 μg/L and 1.0 μg/L for diphacinone and chlorophacinone,respectively.The ext.raction recoveries of the whole blood were 92.1%94.5% and 93.0%94.2%,and the RSD were less than 7.5% and 6.5% for diphacinone and chlorophacinone,respectively.Calibration curves of urine were linear within the range of 0.5100.0 μg/L and 0.240.0 μg/L,and the limits of quantification were 0.5 μg/L and 0.2 μg/L for diphacinone and chlorophacinone,respectively.The extraction recoveries of urine were 95.2%97.0% and 92.0%96.5%,and the RSDs were less than 6.0% and 7.5% for diphacinone and chlorophacinone,respectively.Conclusion：This method is simple,sensitive,accurate and of good specificity for the satisfactory determination of trace diphacinone and chlorophacinone residues in poisoned patients.

关 键 词：全血 尿液 敌鼠 氯鼠酮 高效液相色谱/质谱法 

分 类 号：O657.63[理学—分析化学]