PSA分散固相萃取液相色谱柱后衍生荧光法测定蔬菜和水果中的13种氨基甲酸酯

Study on determination of thirteen carbamate pesticides in vegetables and fruits by HPLC with post-column derivatization and fluorescence detection after PSA dispersive solid-phase extraction cleanup

建立了PSA分散固相萃取净化,液相色谱柱后衍生荧光法测定蔬菜和水果中13种氨基甲酸酯农药的分析方法。在建立的测定条件下,13种氨基甲酸酯的含量与峰面积之间成线性关系,相关系数大于0.994,保留时间的相对标准偏差在0.03%-0.22%之间,检测下限在2.00-2.28μg/kg范围内。西瓜、杏、茄子及胡萝卜中13种氨基甲酸酯的平均回收率在71.7%-110%之间,相对标准偏差在0.68%-15%之间,分析结果优于氨基柱固相萃取法。

Determination of thirteen carbamate pesticides residues in vegetables and fruits by HPLC with PSA dispersive solid-phase extraction cleanup and post-column derivatization fluorescence detection is developed. Under the optimal determination conditions, the detection limits of thirteen carbamate pesticides are in the range of 2.00 - 2.28μg/kg. There is a good linear relationship in the content range of determination. The correlation coefficients of thirteen carbamate pesticides are more than 0.99. The relative standard deviations of retention time are in the range of 0.03% - 0.22%. It is simpler in sample handling by PSA dispersive solid-phase extraction than by NH2 column solid-phase extraction. There are little interference in matrix, and high quality results are obtained. The spiked average recoveries of thirteen carbamate pesticide residues ranged from 71.7% - 110% with RSDs of 0.68% - 15% for watermelon, apricot, eggplant and carrot. The results are very satisfactory.