罗非鱼中拟除虫菊酯类农药检测净化条件的优化

The optimization of purification method for detection of pyrethroid pesticide residual in tilapia

目的研究罗非鱼中9种拟除虫菊酯类农药残留前处理的最佳净化方法。方法优化样品的净化条件,包括净化柱的选择、洗脱剂的选择和洗脱液体积等。最后用气相色谱-电子捕获法（GC-ECD）验证。结果最佳填充料为无水硫酸钠-Florisil吸附剂-无水硫酸钠（2∶3∶2,v/v/v）,洗脱剂为乙酸乙酯-正己烷（1∶9,v/v）,洗脱剂体积15mL。净化后的9种拟除虫菊酯在气相色谱图中分离良好,在1-100ng/mL范围内线性关系良好（r≥0.991）;平均回收率76.3%-117.6%,精密度3.1%-14.6%,最低检出限0.4-3.2μg/kg。结论在实验室建立的最优分析条件下,拟除虫菊酯类药物的回收率和样品的测定效果均能满足农药残留检测标准的要求。

Objective To study the best purification method of pre-treatment of nine pyrethroids pesticides residuals detection in tilapia.Methods Optimizing the purification condition,including the selection of purification column,the selection of elution,and the elution volume,etc.The verification method was by GC-ECD analysis.Results The best filling material was Na2SO4-Florisil-Na2SO4（2∶3∶2）,the elution was ethyl acetate-n-hexane（1∶9,v/v）,the dosage of elution was15 mL.The separation of nine kinds of pyrethroids in the gas chromatogram was better.linear correlation in 1-100ng/mL showed better（r≥0.991）,and mean recovery rates were 76.3%-117.6%.The precision ranges were 3.12-14.60%and the minimum detection limits were 0.4-3.2μg/kg.Conclusion With the establishing of the optimum analysis conditions in the lab,both of the recovery rate of pyrethroids pesticides and the detection result of samples can reach to the standard of pesticide residual detection.