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.
作者
黄克建
莫静
刘晓锋
杨宁
罗轩
朱定姬
李璐
乔文涛
黄晓青
梁平
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)
出处
《分析测试学报》
CAS
CSCD
北大核心
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)
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
on-line solid phase extraction(on-line SPE)
liquid chromato/raphy-tandem mass spectrometry(LC-MS/MS)
rodenticides
whole blood
urine
quadratic equation