【目的】建立哒螨灵在柑桔及土壤中残留的气相色谱分析方法,为评价哒螨灵在柑桔上使用的安全性提供科学依据。【方法】样品以甲醇提取,经石油醚液—液萃取和弗罗里硅土柱净化后,用带μ-ECD的气相色谱仪进行测定。【结果】桔皮、桔肉、全果及土壤样品中哒螨灵的最低检出浓度均为0.001mg/kg,平均回收率为84.78%~101.18%,变异系数为2.31%~8.68%。【结论】建立的方法操作简便,分离效果好,准确度和精密度均满足农药残留分析的技术要求,可用于柑桔及土壤中哒螨灵残留量的检测。
[Objective]The present experiment was conducted to establish a method to determine pyridaben residues in citrus fruits and soil using gas chromatography and provide a reference of evaluating safety of pyridaben in citrus. [Method]The samples were extracted with methyl alcohol, purified with petroleum ether, cleaned up using florisil column, and finally tested by gas chromatography using ECD-detector. [Result]The results indicated that lowest detectable concentration in citrus peel, pulp, whole fruit and soil was 0.001 mg/kg. Sample recovery ranged from 84.78 to 101.18%, and coefficient of variation from 2.31 to 8.68%. [Conclusion]The present method was easy to operate and gave good isolating and accurate results efficiently, and it is suitable for detecting very low concentration of pyridaben residues in citrus fruits and soils.