水产品中拟除虫菊酯类农药残留检测方法的研究

Review on the Analyzing Method of Pyrethroids Pesticide Residue in Aquatic Products

建立了水产品中氯氰菊酯、甲氰菊酯、氰戊菊酯和溴氰菊酯等拟除虫菊酯类农药残留的提取、净化以及毛细管气相色谱的测定方法。选择40mL正己烷:丙酮(V/V,2:1)混合溶液作为提取液,经冷冻去脂,柱层析净化过程中选用3g中性氧化铝作为净化填料,30mL正己烷:丙酮(V/V,4:1)混合溶液进行洗脱,然后用气相色谱法测定,外标法定量。实验结果表明,在10～200ng/mL线性范围内线性良好,相关系数在0.9993～0.9998。标准品添加量在10～66μg/kg范围内,罗非鱼样品加标实验的回收率在76.9～90.3%,相对标准偏差在1.25～4.66%,样品中氯氰菊酯、甲氰菊酯、氰戊菊酯、溴氰菊酯残留量检测方法的检出限为10μg/kg。另外采用鳗鱼和对虾样品的标准添加回收实验进行方法的验证,实验结果表明,平均回收率达到70%以上,相对标准偏差小于10%,符合药残检测要求。本方法可用于进行水产品中多种菊酯类农药残留的检测分析。

The gas chromatographic method was described for measuring Cypermethrin, Fenpropathrin, Fenvalerate, Decamethrin residues in aquatic products. The four pyrethroid pesticide residues in samples were extracted by acetone -hexane （2： 1 ） mixture, the extraction was eliminated by freezing - lipid filtration, then cleaned up by column chromatography with the purification filler of 3g Al2O3 and the elution of acetone -hexane （4：1 ） mixture, and then analyzed by gas chromatograph equipped with an electron capture detector, quantified by the external standard method. The linear ranges of these pesticides were 10 - 200 ng/mL, and the correlation coefficients were 0. 9993 - 0. 9998. The average recovery of the added test from 10 to 66μg/kg was 76.9 -90. 3%, and the RSD% was 1.25 -4. 66%. The detection limit of Cypermethrin, Fenpropathrin, Fenvalerate, Decamethrin residues in aquatic products was 10μg/kg. In addition, the average recovery of the eel and penaeus added test was up to 70%, and the RSD% was low to 10%. The method was consistent with the pesticide residue -detecting request, which was used for detecting many pyrethroids pesticide residue in aquatic products.