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[目的]建立一种简便易行,适用于检测蔬菜中4大类农药残留的气相色谱分析样品前处理方法。[方法]以甲胺磷、对硫磷作为有机磷农药代表,灭多威为氨基甲酸酯类农药代表,氯菊酯为菊酯类农药代表,采用液-液萃取、索氏提取、国标固相萃取法、本法的固相萃取法4种前处理方法处理样品,按GB/T 5009.145-2003和GB/T 5009.146-2003法测定并对不同的前处理方法的测定结果进行比较。[结果]该方法所检测的农药的最低检出限为0.002~0.05 0;加标回收率为86.3%~104.9%;相对标准偏差为3.92%~11.08%;校正曲线相关系数为0.997 9~0.999 8。[结论]与国标前处理方法比较,它在保证国标方法要求的精密度和准确性的同时,具有检验时间减少、前处理试剂消耗少、空白的背景干扰小等特点。
[Objective] The research aimed to establish a simple and easy-to-use gas chromatographic sample preparation method for detecting four kinds of pesticide residues in vegetables. [Method] With methamidophos and parathion as organophosphorus pesticides, methomyl as carbamate pesticide and permethrin as pyrethroid pesticide. Liquid - liquid extraction, Soxhlet extraction, GB Phase extraction method, the method of solid phase extraction four pretreatment methods to deal with samples, according to GB / T 5009.145-2003 and GB / T 5009.146-2003 method to determine and compare the results of different pretreatment methods were compared. [Result] The minimum detectable limit of pesticides detected by this method was 0.002 ~ 0.05 0; the recoveries were 86.3% -104.9%; the relative standard deviations were 3.92% ~ 11.08%; the correlation coefficients of calibration curves were 0.997 9 ~ 0.999 8. [Conclusion] Compared with the national standard pretreatment method, it has the features of reduced test time, less pretreatment reagent consumption and less background interference in the blanket while ensuring the precision and accuracy required by the national standard method.