在线固相萃取/液相色谱-串联质谱法快速检测全血及尿液中15种杀鼠药  

Analysis of Fifteen Rodenticides in Whole Blood and Urine Samples by Liquid Chromatography-Tandem Mass Spectrometry with On-line Solid Phase Extraction

作　　者：黄克建[1] 莫静[2] 刘晓锋[1] 杨宁[1] 罗轩[2] 朱定姬[3] 李璐[1] 乔文涛[1] 黄晓青[1] 梁平[1] 易叶平 刘慧 侯笑然 HUANG Ke-jian;MO Jing;LlUXiao-feng;LUO Xuan;ZHU Dingji;LI Lu;QIAO Wen-tao;HUANG Xiao-qing;LIANG Ping;YI Ye-ping;LIU Hui;HOU Xiao-ran;YANG Ning(Evidence Identification Center,Guangxi Zhuang Autonomous Region Public Security Department,Nanning 530012;School of Chemistry and Chemical Engineering,Guangxi University,Nanning 530004,China;Guangxi Zhuang Autonomous Region Institute for the Prevention and Treatment of Occupational Diseases,Nanning 530021,China)

机构地区：[1]广西壮族自治区公安厅物证鉴定中心,广西南宁530012 [2]广西大学化学化工学院,广西南宁530004 [3]广西壮族自治区职业病防治研究院,广西南宁530021

出　　处：《分析测试学报》2018年第1期1-9,共9页Journal of Instrumental Analysis

基　　金：广西公安科学研究与技术开发计划立项项目(GAT2016-14)

摘　　要：建立了同时测定血液和尿液样品中15种杀鼠药的在线固相萃取/液相色谱-三重四极杆串联质谱(On-line SPE/LC-MS/MS)分析方法。用乙腈沉淀样品中的蛋白质,经稀释、离心、过滤后直接进样。通过在线固相萃取柱HLB富集纯化,以ZORBAX Eclipse Plus C18柱为分析柱,乙腈-0.01 mol/L乙酸铵水溶液为流动相进行梯度洗脱。采用电喷雾电离(ESI+/ESI-)快速正负切换模式,动态多反应监测模式(DMRM)扫描,外标法定量。结果表明,15种杀鼠药采用二次方程拟合时线性关系良好,血液中r^2≥0.997 8,尿液r^2≥0.996 5,方法的检出限和定量下限分别为0.10~5.00μg/L和0.50~10.0μg/L,3个添加水平下的回收率为81.8%~109.6%,日内相对标准偏差(RSD)为0.3%~3.6%,日间RSD为0.3%~3.8%(n=6)。该方法简单方便,灵敏度高,能够用以血液和尿液样品中15种杀鼠药的快速筛查和准确定量。A analytical method was developed for the simultaneous determination of fifteen in whole blood and urine samples by liquid chromato/raphy-tandem mass spectrometry(LC-MS/MS)with on-line solid phase extraction(on-line SPE).The samples were treated with acetonitrile,followed by dilution,centrifugation and filtration.The solution obtained was purified with polymer column for hydrophilic-lipophilic balance(HLB),then eluted on a ZORBAX Eclipse C1 column with acetonitrile and 0.01 mol/Lammonium acetate aqueous solution as mobile phase.The analytes were detected in dynamic multiple reaction monitorin/(DMRM)mode under alternate positive/negative electrospray ionization(E S I/ESI")mode,and quantified by external standard method.The results showed that there existed/ood linear relationships by quadratic equation fittin/for the fifteen rodenticides in whole blood and urine in the investigated mass concentration ran/es with the correlation coefficients not less than 0.997 8 for whole blood and not less than 0.996 5 for urine,respectively.The LODs and the LOQs varied from 0.10(xg/L to 5.00(xg/L and 0.50(xg/L to 10.0[xg/L,respectively.The recoveries at three spiked levels in whole blood and urine ran/ed from 81.8%to 109.6%with their RSDs of 0.3%-3.8%(zi=6).The developed method is simple and reliable,and is sensitive for the rapid detection and accurate quantification of fifteen rodenticides whole blood and urine samples.

关 键 词：在线固相萃取 液相色谱-串联质谱 杀鼠药 血液 尿液 二次方程 

分 类 号：O657.7[理学—分析化学] O657.63[理学—化学]