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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。
Objective To establish a gas chromatography-mass spectrometry (GC-MS) method for the determination of 15 pesticides in blood. Methods Two ml of whole blood was extracted and concentrated by extraction with dichloromethane. The content of gulonolactone in methanol was determined by GC-MS with DB-35MS (30m × 0.25mm × 0.25μm) capillary column. Results Diazinon, atrazine, prometryn, butachlor, bifenthrin in the concentration range of 4 ~ 80μg / L, phorate, 2,4-D butyl, methyl parathion, Malathion, chlordane and fenpropathrin in the concentration range of 10 ~ 200μg / L, α-endosulfan, β-endosulfan and cyhalothrin in the concentration range of 20 ~ 400μg / 800μg / L, the correlation coefficients (r2) ranged from 0.998 to 1.000, and the spiked recoveries of all analytes ranged from 51.3% to 113.1%. The detection limits were 0.05 ~ 1.00μg / L, the limit of quantification was 0.20-3.00μg / L, the intra-assay precision was 3.17% -22.79%, and the inter-assay precision was 5.58% -26.13%. Conclusion This method is suitable for the determination of 15 pesticides in blood samples.