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目的建立了液相色谱串联质谱(LC-MS/MS)法测定尿中二乙基磷酸酯、二硫代磷酸二甲酯、二硫代磷酸二乙酯、4-硝基酚、3-氯-4-甲基-7-羟基香豆素和TCPY 6种有机磷农药代谢物含量的方法。方法尿样中加入酶解液,37℃水浴4h后经oasis HLB柱固相萃取,用甲醇洗脱后离心浓缩,乙腈定容;以乙酸铵做缓冲溶液,乙腈和水为流动相等梯度洗脱,经Waters Symmetry C185μm(2.1mm×150mmcolumn)分离,经在线电喷雾离子源(ESI)负离子化后,采用多反应离子监测方式(MRM)选择离子对测定。结果目标化合物的线性范围为0～1000ng/ml,6种化合物的相关系数有5种大于0.990,加标回收率在79%～130%之间,RSD<8.2%;日内、日间相对标准偏差小于15%(n=6)。结论该方法样品采集简单,特异性强,能准确、高效地检测尿样中有机磷农药代谢物。
OBJECTIVE To establish a liquid chromatography tandem mass spectrometry (LC-MS / MS) method for the determination of diethyl phosphate, dimethyl dithiophosphate, diethyl dithiophosphate, 4-nitrophenol, Methyl-7-hydroxycoumarin and TCPY six kinds of organophosphorus pesticide metabolites content method. Methods The urine sample was hydrolyzed by the oasis HLB column after 4h at 37 ℃. The sample was eluted with methanol and concentrated by centrifugation. The sample was eluted with acetonitrile. The buffer was eluted with ammonium acetate and the mobile phase consisted of acetonitrile and water. , Separated by a Waters Symmetry C18 5 μm (2.1 mm × 150 mm column) and ionized using a multi-reactive ion monitoring mode (MRM) after negative ionization by an electrospray ionization source (ESI). Results The linear range of the target compound ranged from 0 to 1000ng / ml. The correlation coefficients of the six compounds were more than 0.990. The recoveries were between 79% and 130% with a RSD <8.2%. The relative standard deviations Less than 15% (n = 6). Conclusion The method of sample collection is simple and specific, and can accurately and efficiently detect organophosphorus pesticide metabolites in urine samples.