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建立了QuEChERS法提取净化、气相色谱质谱联用仪测定水产品中的硫丹(α-硫丹和β-硫丹)及其代谢物硫丹硫酸盐的方法。样品用10 mL乙腈提取,取1 mL加入PSA和C18粉末振荡后离心,上清液过滤膜后用气相色谱质谱联用仪测定。3种物质在0.5~100μg/L范围内线性良好,在1,5,10μg/kg3个浓度水平下3种目标物平均添加回收率在72.3%~101.6%之间,RSD小于10%,定量限为0.5μg/kg,满足进出口检测要求,已应用于水产品中硫丹残留的测定。
A method for the determination of endosulfan (α-endosulfan and β-endosulfan) and its metabolite endosulfan sulfate in aquatic products by QuEChERS extraction and purification and gas chromatography-mass spectrometry was established. The sample was extracted with 10 mL of acetonitrile, centrifuged by adding 1 mL of PSA and C18 powder, and the supernatant was filtered and determined by gas chromatography-mass spectrometry. The linearity of the three substances in the range of 0.5 ~ 100μg / L was good. Under the concentrations of 1, 5 and 10μg / kg, the average recoveries of the three target compounds ranged from 72.3% to 101.6% with RSD less than 10% 0.5μg / kg, to meet the import and export testing requirements, has been applied to the determination of endosulfan residues in aquatic products.