气相色谱法测定水产品中7种拟除虫菊酯的残留量

Determination of 7 pyrethroids residues in aquatic product by gas chromatography

  • 摘要: 建立了水产品中联苯菊酯、甲氰菊酯、三氟氯氰菊酯、氯氰菊酯、氰戊菊酯、溴氰菊酯、氯菊酯7种拟除虫菊酯残留量同时测定的气相色谱(GC-ECD)法。样品中的菊酯用环己烷和乙酸乙酯提取,乙腈饱和的石油醚去脂肪,过LC-Florisil柱净化,正己烷定容,用带电子俘获器的气相色谱仪检测。该方法在1~100 μg/L浓度范围内线性关系良好,相关系数r>0.992;在5、10、20 μg/kg 3个添加浓度水平下的回收率在70.0%~114.8%之间,日内精密度为1.2%~9.8%(n=5),日间精密度为3.8%~11.2%(n=3);根据2倍信噪比计算,联苯菊酯、甲氰菊酯、三氟氯氰菊酯、氯氰菊酯的最低检测限为1 μg/kg,氯菊酯、氰戊菊酯、溴氰菊酯的最低检测限为2 μg/kg。

     

    Abstract: Gas chromatography with electron capture detection method was developed for the determination of 7 pyrethroids residues in aquatic products. Pyrethroids were extracted with cyclohexane and ethylacetate(1:1,V/V)and lipids were removed with petroleum ether. Cleanup was performed on a LC-Florisil column. The working curves for the pyrethroids were linear (r>0.992) in the range of 1 to 100 μg/L. When spiked with 5, 10 and 20 μg/kg of pyrethroids, the average recoveries were 70.0%~114.8% and the intra-day RSD(n=5) were 1.2%~9.8% and the inter-day RSD(n=3) were 3.8%~11.2%. The detection limit as estimated by 2 times signal to noise method for bifenthrin, fenpropathrin, lambdacyhalothrin, permethrin was 1 μg/kg and for permethrin, fenvalerate, deltamethrin was 2 μg/kg respectively.

     

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