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建立了乙醚小体积液液萃取结合PSA分散固相萃取,在线GPC净化-气质联用分析鱼塘水中农药的方法。加入内标磷酸三丁酯的鱼塘水样,经乙醚提取后取分层上清液,加入0.1g PSA,涡旋,离心过滤后,经在线凝胶色谱净化-气质联用仪进行21种农药的净化富集和检测。鱼塘水样中农药的检出限在0.31~26.70ng/m L之间,定量下限在0.87~80.1ng/m L之间,氯氟氰菊酯、氯氰菊酯、氰戊菊酯在0.1~3.2μg/m L浓度范围内,其余18种农药在5~320ng/m L浓度范围内的线性关系良好。方法可用于鱼塘水样中农药残留的快速检验分析。
A method for the analysis of pesticides in fish ponds with small-volume liquid-liquid extraction of diethyl ether combined with PSA dispersive solid-phase extraction and on-line GPC-GC / MS was established. Add the internal standard of tributyl phosphate fish pond water samples, the ether extract was layered supernatant, add 0.1g PSA, vortex, centrifugal filtration, on-line gel chromatography - GC-MS for 21 species Pesticide purification enrichment and testing. The detection limit of pesticides in fish ponds ranged from 0.31 to 26.70 ng / m L with the lower limit of quantification being between 0.87 and 80.1 ng / m L. Cyhalothrin, cypermethrin and fenvalerate ranged from 0.1 to 3.2 The linear range of the other 18 pesticides in the concentration range of 5 ~ 320ng / m L was good within the range of μg / mL. The method can be used for rapid test and analysis of pesticide residues in fish pond water samples.