超高效液相色谱-串联质谱法同时测定血液中115种农药

建立了超高效液相色谱-串联质谱法(UPLC-MS/MS)一针进样同时测定血液中115种农药的方法。血液样品与提取剂甲醇按1∶5体积比进行蛋白沉淀,涡旋振荡2 min,以12000 r/min离心10 min,取上清液进行UPLC-MS/MS分析。质谱分析采用电喷雾离子源(ESI),正离子模式和负离子模式同时切换采集。结果表明,115种目标农药在1~200 ng/mL质量浓度范围内线性关系良好(r>0.99),13%的目标农药检出限(S/N≥3)为0.2 ng/mL,其余目标物均为0.1 ng/mL,所有目标农药的定量下限(S/N≥10)均为1 ng/mL。在10、50、100 ng/mL加标水平下,方法的基质效应为81.8%~115%,目标农药的回收率为80.4%~109%,日内精密度(Intra-RSD)为1.6%~11%,日间精密度(Inter-RSD)为1.9%~13%。该方法简便快速、灵敏度高、稳定性好,适用于血液样品中多农药的定性定量分析。

Simultaneous Determination of 115 Pesticides in Blood by Ultra high Performance Liquid Chromatography-Tandem Mass Spectrometry

A method of ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was established for the simultaneous determination of 115 pesticides in blood.The blood sample and the extractant methanol were mixed at a volume ratio of 1∶5,vortexed for 2 min,centrifuged at 12000 r/min for 10 min,and the supernatant was taken for UPLC-MS/MS analysis.Scheduled multiple reaction monitoring in both electrospray ionization positive ion mode(ESI^+)and negative ion mode(ESI^-)were adopted in MS analysis.Results showed that there were good linear relationships for 115 target pesticides in the concentration range of 1-200 ng/mL with their correlation coefficients(r)larger than 0.99.The limits of detection(S/N≥3)were 0.2 ng/mL for 13%of the target pesticides and 0.1 ng/mL for the rest of pesticides.The limits of quantitation(S/N≥10)for all the target pesticides were 1 ng/mL.At the spiked levels of 10,50 and 100 ng/mL,the matrix effects of the method were between 81.8%and 115%.The recoveries for the target pesticides ranged from 80.4%to 109%,with intra-RSDs and inter-RSDs of 1.6%-11%and 1.9%-13%,respectively.The method was simple,rapid,sensitive and stable,and was suitable for the qualitative and quantitative analysis of multi-pesticide in blood samples.