蔬菜中氨基甲酸酯类农药残留的HPL/CMS测定研究

Determination of the residues of carbamate pesticites in vegetables by liquid chromatography mass spectrometry

目的：建立简便、灵敏、准确的高效液相色谱电喷雾质谱测定蔬菜中氨基甲酸酯残留的检测方法。方法：样品经乙腈提取、甲醇：二氯甲烷（1：99v／v）溶解后，用固相萃取小柱进行净化、提纯。选用Pickering C8（250mm×4．0mm×5μm）作为分析柱，甲醇／酸化水（内含0．1％乙酸）梯度洗脱，通过选择性离子监测（SIM）及电喷雾电离离子化技术进行测定。结果：线性范围为50．0～1500．0μg/L，定量检测下限为4．8～8．6μg／kg，方法回收率为78．5％～108．4％，标准偏差为4．6％～7．9％，RSD均小于8％。结论：该法灵敏度高、操作简便、快速，适用于实际样品的测定。

Objective：To establish an analytical method for determination of carbamates in vegetables by liquid chromatography - mass spectrometry with an electrospray ionization （ESI） in the positive mode. Methods： The samples were extracted by CH3 CN and cleaned with solid - phase extraction. The separation was performed on a pickering Cs column （ 250 mm × 4. 0 mm i. d. , 5 μm）, the gradient mobile phase consisting of 0. 1% CH3 COOH and CH3 OH. The selected ion monitoring （SIM） mode was selected to quantify. Results： The linear range was 50. 0 - 1 500. 0 μg/L and the limits of quantification was 4. 8 - 8.6 μg/ kg. The recovery was between 78.5% - 108.4%. RSD was less than 8%. Conclusion：This method is found to be sensitive,fast and accurate. It can be used for determination of the residues of carbamate pesticides in vegetables.