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目的:建立基于分散液相微萃取(DLLME)的水中7种菊酯类农药和8种有机磷农药残留检测方法。方法:5.0 ml水样用1.0 ml含30.0μl萃取剂的丙酮溶液萃取离心后取出氮吹吹干,用含0.10μg/ml环氧七氯B的20μl环己烷溶解置换后分别进电子捕获检测器(ECD)和火焰光度检测器(FPD)检测分析15种农药。结果:水中15种农药残留检测方法的线性范围为0.40μg/L～8.00μg/L,7种菊酯类农药方法检出限为0.05μg/L～0.11μg/L,8种有机磷农药的检出限为0.03μg/L～0.05μg/L,两者相关系数为0.9953～0.9996,加标回收率为82.5%～111.3%,相对标准偏差为7.5%～14.4%。结论:该方法检测水中农药残留操作简单、快捷,能作为日常水样中痕量农药残留检测的快速分析。
OBJECTIVE: To establish a method for the determination of 7 pyrethroid pesticides and 8 organophosphorus pesticide residues in water based on the liquid-phase microextraction (DLLME). Methods: 5.0 ml water sample was extracted with 1.0 ml acetone solution containing 30.0 μl extractant, centrifuged, then nitrogen was removed and air-dried. After 20 μl cyclohexane containing 0.10 μg / ml epoxy heptachlor B was dissolved and replaced, (ECD) and flame photometric detector (FPD) detection and analysis of 15 kinds of pesticides. Results: The linear range of 15 pesticide residue detection methods in water was 0.40μg / L ~ 8.00μg / L, and the detection limits of the seven pyrethroid pesticides were 0.05μg / L ~ 0.11μg / L. Eight kinds of organophosphorus pesticides The detection limit was 0.03μg / L ~ 0.05μg / L, the correlation coefficient was 0.9953 ~ 0.9996, the recoveries were 82.5% ~ 111.3% and the relative standard deviations were 7.5% ~ 14.4%. Conclusion: The method is simple, rapid and can be used as a rapid analysis of trace pesticide residues in water samples.