超高效液相色谱-串联四极杆复合线性离子阱质谱法同时识别和测定尿液中毒死蜱代谢物  

Identification and Quantification of Chlorpyrifos Metabolites in Urine Samples by Ultra Performance Liquid Chromatography-Triple Quadrupole-Linear Ion Trap Mass Spectrometry

作　　者：宋宁慧[1] 徐怀洲 吉贵祥[1] 张圣虎[1] 张芹[1] 郭敏[1] 石利利[1] SONG Ning-Hui;XU Huai-Zhou;JI Gui-Xiang;ZHANG Sheng-Hu;ZHANG Qin;GUO Min;SHI Li-Li(Nanjing Institute of Environmental Sciences,Nanjing 210042,China)

机构地区：[1]环境保护部南京环境科学研究所,南京210042

出　　处：《分析化学》2018年第5期796-802,共7页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金项目(No.41101307);中央级公益性科研院所基本科研业务费专项资金项目(20160210)资助~~

摘　　要：建立了超高效液相色谱-串联四极杆复合线性离子阱质谱(Ultra performance liquid chromatographytriple quadrupole-linear ion trap mass spectrometry,UPLC-QTRAP)技术结合QuEChERS(Quiek,Easy,Cheap,Effective,Rugged,and Safe)法检测尿样中毒死蜱代谢产物残留的分析方法。采用乙腈提取,PSA和BCB净化,ZORBAX Eclipse Plus C18色谱柱分离,以乙腈-0.2%氨水为流动相梯度洗脱,在电喷雾电离(ESI负离子模式下),使用触发增强子离子扫描方式(MRM-IDA-EPI)对尿样中毒死蜱的代谢产物进行定性和定量分析。方法线性范围为1.0~100.0μg/L,检出限0.10~0.73μg/L。尿样中3种毒死蜱代谢物的平均加标回收率在80.3%~90.1%之间,RSD均小于5%。本方法操作简单、灵敏度高、准确性好、重现性强,利用QTRAP的质谱优势可有效的对色谱峰进行鉴定,有效预防样品的假阳性。本方法已成功应用于人体尿液实际样品中,检出的浓度范围为ND^54.6μg/L。本方法可为复杂基质中化学品的识别和定量提供技术参考。A method was established for the determination of chlorpyrifos metabolites employing QuEChERS method and ultra performance liquid chromatography-triple quadrupole-linear ion trap mass spectrometry(UPLC-QTRAP).The urine samples were extracted by acetonitrile and then cleaned up with PSA and GCB.The samples were separated with the gradient elution of acetonitrile-0.2%ammonia water on ZORBAX Eclipse Plus C 18 column.The analytes were detected by tandem mass spectrometry under negative ion mode with electrospray ionization(ESI)source and MRM-IDA-EPI mode.Under the optimized conditions,the calibration curve was linear in range of 1.0-100.0μg/L,and the limits of detection were 0.10-0.73μg/L.The average recoveries were 80.3%-90.1%,and RSDs were all within 10%.The developed method was simple,sensitive,accurate,and repeatable,and could avoid false positive result of samples effectively.The established method was successfully applied to determine the exposure level of chlorpyrifos metabolites in real samples of human health risk analysis.The results showed that the maximum concentration of chlorpyrifos metabolites was 54.6μg/L.This method provided technic support for simultaneous identification and quantification of chemicals in complex matrix.

关 键 词：毒死蜱 代谢产物 超高效液相色谱-串联四极杆离子阱质谱 尿样 

分 类 号：O657.63[理学—分析化学] R12[理学—化学]