液相色谱柱后衍生法测定蔬菜、水果中氨基甲酸酯类农药

目的 建立液相色谱柱后衍生法测定蔬菜、水果中氨基甲酸酯类农药的残留量。方法 用乙腈提取氨基甲酸酯类农药, 提取液经固相吸附剂净化, 氮气吹干后用甲醇复溶, 液相色谱仪荧光检测器柱后衍生法测定。结果 经多次摸索采用Kromasil 100-5-C18的色谱柱, 流动相使用乙腈/水得到稳定的基线和完全分离的色谱峰, 10种氨基甲酸酯类农药浓度在0.025~0.500 ?g/mL范围内线性关系良好; 方法检出限分别为0.002~0.008 mg/kg之间; 方法加标回收率在75.8%~92.8%之间; 精密度和重复性RSD均在10.0%以内。 结论 该方法简便、快速、准确, 完全满足实验要求。

Determination of carbamate pesticides in vegetables and fruits by post-column derivatization of high performance liquid chromatography

Objective To establish a method for the determination of carbamate pesticide residues in vegetables and fruits by liquid chromatography with post-column derivatization was established. Methods Carbamate pesticides were extracted by acetonitrile. The extract was purified by solid-phase adsorbent, dried by nitrogen and dissolved by methanol. The method was determined by post-column derivatization with fluorescence detector of liquid chromatography. Results After many explorations, the Kromasil 100-5-C18 column was used. The mobile phase was acetonitrile/water to obtain stable baseline and completely separated peaks. The linear relationship of 10 carbamate pesticides was good in the range of 0.025?0.500 g/mL. The detection limits were 0.002?0.008 mg/kg, respectively. The recovery rate of the method was 75.8%?92.8%. The precision and repeatability of RSD were within 10.0%. Conclusion The method is simple, rapid and accurate, and can completely meet the experimental requirements.