气相色谱法同时测定水果中毒死蜱、苯醚甲环唑和哒螨灵的残留

Simultaneous determination for residues of chlorpyrifos, difenoconazole and pyridaben in fruits by gas chromatography with electron capture detector

摘要: 建立了同时测定水果中毒死蜱、苯醚甲环唑和哒螨灵残留的气相色谱（GC/ECD）分析方法。样品经乙腈提取，氨基固相萃取小柱净化，GC/ECD检测，外标法定量。结果表明：在0.02 ~1 mg/L 范围内，3种供试农药的线性相关系数均大于0.99，检出限（LOD）为0.006 ~ 0.007 mg/kg，定量限（LOQ）为0.02 mg/kg；在0.02、0.05 和0.1 mg/kg 3 个添加水平下，平均回收率在78% ~108%之间，相对标准偏差（RSD）为2.9% ~16%。该方法适用于水果中毒死蜱、苯醚甲环唑和哒螨灵的检测。

Abstract: An analytical method for simultaneous determination of chlorpyrifos, difenoconazole and pyridaben residues in fruits using gas chromatography with electron capture detector (GC-ECD) was developed. The samples were extracted with acetonitrile, and further clean-up on NH2-SPE. It showed that good linearity was obtained from range 0.02 to 1.0 mg/L with correlation coefficients above 0.99. The limits of detection were 0.006-0.007 mg/kg and the limits of quantification were 0.02 mg/kg. Fortified recoveries at 0.02, 0.05 and 0.1 mg/kg were from range 78% to 108% with relative standard deviations (RSDs) from range 2.9% to 16%, respectively.The results showed the method was suitable for the determination of chlorpyrifos, difenoconazole and pyridaben in fruits.