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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 nine pyrethroid pesticide residues in tilapia. Methods To optimize the purification conditions of the sample, including the choice of purification column, the choice of eluent and the volume of eluent. Finally, gas chromatography - electron capture (GC-ECD) verification. Results The best filler was anhydrous sodium sulfate-Florisil adsorbent-sodium sulfate anhydrous (2: 3: 2, v / v / v) and the eluent was ethyl acetate- v), eluent volume 15mL. The purified pyrethroids were well separated in the gas chromatogram with good linearity in the range of 1 ~ 100 ng / mL (r ≥ 0.991). The average recoveries ranged from 76.3% to 117.6% with the precision of 3.1% to 14.6% The lowest detection limit of 0.4 ~ 3.2μg / kg. Conclusion Under the optimal analytical conditions established in the laboratory, the recovery of pyrethroid drugs and the determination results of the samples can meet the requirements of pesticide residue detection standards.