提出了快速检测出口泥鳅中硫丹及其代谢物硫丹硫酸盐的气相色谱-负化学电离离子化-质谱法。考察了快速溶剂萃取法、均质提取法和振荡提取法对试验效果的影响。通过固相萃取辅以冷冻离心的净化方法有效解决了油脂对硫丹及其代谢物测定的干扰问题。通过优化仪器条件,有效缩短了检测时间。硫丹及其代谢物的线性范围为0.005~0.400 mg·L-1,检出限在0.04~0.05 μg·kg-1之间,测定下限在0.12~0.18 μg·kg-1之间。对空白泥鳅样品进行加标回收试验,回收率在89.1%~100%之间,测定值的相对标准偏差(n=6)在2.9%~8.3%之间。本方法适用于出口泥鳅快速批量检测。

A method of GC-MS with negative ion chemical ionization was proposed for determination of endosulfan and its metabolite (endosulfan sulfate). The effects of rapid solvent extraction, homogeneous extraction and oscillation extraction were examined. The interference of oils in the samples was eliminated effectively by solid-phase extraction purification combined with centrifugation method. The detection time was effectively shortened by optimizing the instrument conditions. The linearity range of the mass concentration of endosulfan and its metabolites was 0.005-0.400 mg·L-1 with detection limits in the range of 0.04-0.05 μg·kg-1 and lower limits of determination in the range of 0.12-0.18 μg·kg-1. Recovery rates measured by standard addition method were in the range of 89.1%-100%, and RSD (n=6) was in the range of 2.9%-8.3%. The method was suitable for rapid batch detection of export loach.