血液中13种有机磷农药代谢产物的QuEChERS-超高效液相色谱-四极杆/静电场轨道离子阱高分辨质谱法检测

Determination of 13 metabolites of organophosphorus pesticides in blood by ultra performance liquid chromatography-quadrupole/electrostatic field orbitrap mass spectrometry

建立了QuEChERS结合超高效液相色谱-四极杆静电场轨道离子阱高分辨质谱(UPLC-Q Exactive Orbitrap HRM S)同时检测血液中13种有机磷农药代谢产物的方法。血液样品经甲醇-乙腈溶液(3:2,V/V)提取,优化的QuEChERS方法净化后,进行UPLC-Q Exactive Orbitrap HRM S检测。实验结果显示:13种有机磷农药代谢产物在一定浓度范围内线性关系良好,相关系数(R^(2))均大于0.9969,检出限(LOD)和定量限(LOQ)分别在0.2~10 ng/mL和0.5~10 ng/mL之间;在20,50,100 ng/mL 3个添加水平下,13种有机磷农药代谢产物的回收率为60.6%~119.0%,基质效应为54.4%~122.1%,日内和日间精密度RSD均小于11%。该方法适用于公安机关在办理有机磷农药中毒案(事)件中对血液里多种有机磷农药代谢产物的检测鉴定。

A method was established for simultaneous determination of thirteen kinds of organophosphorus pesticide metabolites in blood by QuEChERS combined with ultra performance liquid chromatography quadrupole/electrostatic field orbital mass spectrometry( UPLC-Q Exactive Orbitrap HRMS). The blood samples were extracted with methanol/acetonitrile( 3 ∶ 2,V/V) and purified by optimized QuEChERS method.The samples were detected by UPLC-Q Exactive Orbitrap HRMS. The results showed that there was a good linear relationship between the concentration of metabolites of thirteen kinds of organophosphorus pesticides and MS signals. The correlation coefficients( R^(2)) were greater than 0. 9969. The limits of detection( LODs) and limits of quantitation( LOQs) were 0. 2-10 ng/m L and 0. 5-10 ng/m L,respectively. The recoveries of 13 metabolites of organophosphorus pesticides were 60. 6%-119. 0% and the matrix effect was 54. 4%-122. 1%. The RSDs of intra day and inter day precision were less than 11%. The method is suitable for the detection and identification of various metabolites of organophosphorus pesticides in the blood samples obtained in organophosphorus pesticide poisoning cases handled by public security organs.