气相色谱-质谱法检测血液中15种农药残留

目的建立血液中15种农药的气相色谱-质谱检测方法(GC-MS)。方法取2ml全血,用二氯甲烷萃取浓缩,以古洛糖酸内酯甲醇溶液定容,供装有DB-35MS(30m×0.25mm×0.25μm)毛细管柱的GC-MS定性定量测定。结果二嗪农、阿特拉津、扑草净、丁草胺、联苯菊酯在4～80μg/L浓度范围内,甲拌磷、2,4-D丁酯、甲基对硫磷、马拉硫磷、氯丹、甲氰菊酯在10～200μg/L浓度范围内,α-硫丹、β-硫丹、三氟氯氰菊酯在20～400μg/L浓度范围内,乐果在40～800μg/L浓度范围内,具有良好的线性响应,相关系数(r2)在0.998～1.000之间,各待测物的方法加标回收率为51.3%～113.1%,方法的检出限为0.05～1.00μg/L,方法的定量限为0.20～3.00μg/L,批内精密度在3.17%～22.79%,批间精密度在5.58%～26.13%。结论该方法适用于血液样品中15种农药的含量检测。

Determination of 15 kinds of pesticides in blood by gas chromatography-mass spectrometry

Objective To develop the method of gas chromatography-mass spectrometry(GC-MS) for simultaneous determination of 15 herbicides in blood.Methods 2ml of blood in vitro were sampled,concentrated and extracted with dichloromethane,reconstant with methanol agents of Gulonic acid lactone solution,and detected by GC-MS.Results Experimental results show that diazinon,atrazine,prometryn,methyl parathion,butachlor,bifenthrin at 4-80μg/L,phorate,malathion,2,4-D butyl ester,chlordane,fenpropathrin at 10-200μg/L,α-endosulfan,β-endosulfan,cyhalothrin at 20-400μg/L,dimethoate at 40-800μg/L,with good linear response.The correlation coefficient(r2) were between 0.998-1.000,respectively.The recovery of all analysts averaged between 56%-128% in blood samples.The detection limits of all compounds between 0.05 and 1.00μg/L.The lower limit of quantification between 0.20 and 3.00μg/L.Conclusion The methods is apply to detect the content of analysts in blood samples.