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建立了测定尿中有机磷农药代谢产物-二烷基磷酸酯(DAPs)类化合物的气相色谱-质谱(GC-MS)分析方法。样品经乙腈-乙醚(1:1,V/V)萃取,五氟溴苄苯衍生,再由正己烷提取衍生物,固相萃取净化,气相色谱-质谱(GCM S)结合选择离子监测模式(SIM)定性,内标法定量。各种二烷基磷酸酯的衍生物在0.05~10 mg/L范围内线性关系良好,相关系数r≥0.993;平均回收率为51.6%~90.8%,相对标准偏差(n=6)小于29%;方法检出限为0.001~0.002 mg/L。
A gas chromatography-mass spectrometry (GC-MS) method for the determination of dialkyl phosphate (DAPs), a metabolite of organophosphorus pesticides in urine, was established. Samples were extracted with acetonitrile-diethyl ether (1: 1, V / V), pentafluorobenzylbenzene, and then derivatized with n-hexane, followed by solid-phase extraction and gas chromatography-mass spectrometry (GCM S) SIM) qualitative, internal standard method. The derivatives of various dialkylphosphates showed a good linearity in the range of 0.05-10 mg / L with a correlation coefficient of r ≥ 0.993. The average recoveries ranged from 51.6% to 90.8% with relative standard deviations (n = 6) less than 29% The detection limit was 0.001 ~ 0.002 mg / L.