摘要
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。
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.
出处
《分析测试学报》
CAS
CSCD
北大核心
2017年第4期539-543,共5页
Journal of Instrumental Analysis
关键词
气相色谱-串联质谱法
固相支撑液液萃取
血液
杀虫脒
双甲脒
代谢产物
gas chromatography - tandem mass spectrometry ( GC - MS/MS )
solid supported liquid extraction
blood
chlordimeform
amitraz
metabolites