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目的:建立一种高灵敏度测定水中11种对鱼高毒有机磷农药残留的气相色谱分析方法。方法:向10.0 ml水样中加入100μl二硫化碳(萃取剂)和200μl丙酮(分散剂),混匀后室温静置2 min,以4000 r/min离心5 min,吸取70μl~90μl沉淀相供上机测定。结果:在1.0μg/L~500μg/L(辛硫磷在5.0μg/L~1000μg/L)范围内,11种农药具有良好的线性关系,相关系数在0.996~0.9997之间,检出限为0.3μg/L~1.0μg/L(S/N=3)。方法加标回收率在80.0%~107%之间,相对标准偏差在1.9%~6.5%之间。结论:本方法已成功应用于养殖水域实际水样的有机磷农药残留分析,操作简单、快速、环保,灵敏度高,令人满意。
OBJECTIVE: To establish a high sensitivity gas chromatographic method for the determination of eleven highly toxic organophosphorus pesticide residues in fish. Methods: Add 100 μl of carbon disulfide (extractant) and 200 μl of acetone (dispersant) to 10.0 ml of water sample, mix well and let stand at room temperature for 2 min, centrifuge at 4000 r / min for 5 min, and draw 70 μl ~ Determination. Results: Among the range of 1.0μg / L to 500μg / L (phoxim in the range of 5.0μg / L to 1000μg / L), 11 kinds of pesticides had a good linear relationship and the correlation coefficient was between 0.996 and 0.9997. The detection limits were 0.3 μg / L to 1.0 μg / L (S / N = 3). The recoveries of the methods were between 80.0% and 107% with relative standard deviations between 1.9% and 6.5%. Conclusion: The method has been successfully applied to the analysis of residual organophosphorus pesticides in aquaculture water samples. The method is simple, rapid, environmental friendly, high sensitivity and satisfactory.