固相支撑液液萃取/气相色谱-串联质谱法同时测定血液中双甲脒、杀虫脒及其代谢产物

建立了气相色谱-串联质谱法同时测定血液中双甲脒、杀虫脒及其代谢产物的分析方法。优化了样品前处理方法及气相色谱-串联质谱的分析条件,样品经固相支撑液液萃取柱(SLE)净化,乙腈-二氯甲烷(体积比1∶1)洗脱后,在多反应监测模式(MRM)下检测。结果表明,2,4-二甲基苯胺、4-氯邻甲苯胺和双甲脒在1.0~1 000 ng/m L范围内,其余目标物在2.0~1 000 ng/m L范围内线性关系良好,相关系数均大于0.99;定量下限为1.0~2.0 ng/m L,加标回收率为88.6%~113%。该方法简便、快捷、样品用量小,结果准确可靠,灵敏度高,适用于血液中6种目标物的同时检测。

Determination of Amitraz,Chlordimeform and Their Metabolites in Blood by Solid Supported Liquid Extraction and Gas Chromatography-Tandem Mass Spectrometry

A method was developed for the determination of amitraz,chlordimeform and their metabolites in blood by gas chromatography-tandem mass spectrometry (GC-MS/MS).The conditions for sample pretreatment and GC-MS/MS parameters were optimized.The samples were pretreated by solid supported liquid extraction (SLE),and eluted with acetonitrile-dichloromethane (1 ∶ 1).The detection was carried out by GC-MS/MS in multiple reaction monitoring (MRM) mode.Good linear relationships for 2,4-dimethylaniline (DMA),4-chloro-2-methylaniline and amitraz were obtained in the range of 1.0-1 000 ng/mL,and those for other three compounds were obtained in the range of 2.0-1 000 ng/mL,with correlation coefficients more than 0.99.The limits of quantitation were in the range of 1.0-2.0 ng/mL,and the recoveries ranged from 88.6％ to 113％.With the advantages of simplicity,rapidness,low sample consumption,accuracy and reliability,this methed is suitable for the determination of six compounds in blood.