基质固相分散-气相色谱法测定苹果中的多种农药残留

 【目的】研究适合苹果中35种有机磷、有机氯及拟除虫菊酯类农药的多残留快速检测方法。【方法】通过对35种农药的色谱条件试验、基质固相分散（MSPD）材料的选择及其与样品的比例试验、洗脱条件试验以及加标回收率试验，建立和优化35种农药的MSPD-GC多残留分析方法。【结果】MSPD-GC-FPD法对苹果样品中16种有机磷农药回收率为79.67%～104.68%，变异系数≤4.15%，方法的最低检出限为0.0032～0.010 mg?kg-1；MSPD-GC-ECD法对苹果中19种有机氯和菊酯类农药的回收率为78.6%～103.4%，变异系数≤4.06%，方法的最低检出限为0.000098～0.007 mg?kg-1。对苹果中上述35种农药的最低检出限均低于国内及国际上对苹果中农药残留的MRL值。【结论】基质固相分散-气相色谱方法简便、快速、准确、灵敏、节省样品和有机溶剂，可满足苹果中多种常见农药残留同时检测的实际需要。

Matrix Solid-Phase Dispersion and Gas Chromatography determination of Multi-Residue Pesticides in Apples

Abstract: 【Objective】To study the multi-residue analytical methods of organophsphorous, organochlorine and pyrethroid pesticides in apples by matrix solid-phase dispersion and gas chromatography(MSPD-GC). 【Method】The MSPD-GC methods for the simultaneous determination of 35 pesticides in apples was established through the experimentation of chromatographic instrumentation working condition, choice test of materials for MSPD extraction, the ratio of solid-phase material to sample, the elution tests, and the recovery trials at different fortification levels. 【Result】The MSPD-GC method for simultaneously analysis of 35 pesticide residues in apples was optimized and established in this study, The method has shown good recovery (78.6%-104.68%) for various levels of spiked samples, the coefficient variations(CV) were ≤4.15% for all pesticides studied. The limit of detection(LOD) of all pesticide residues were lower than their maximal residues limit(MRL). 【Conclusion】 The proposed method is easier to perform, faster, higher recoveries and sensitivity, consumes less sample and organic solvents. It can meet the demands of practical use for the simultaneous determination of multi-residue pesticides in apples.