两种前处理方法应用于气相色谱-质谱联用测定水产品中三氯杀螨醇残留量

Two Sample Pretreatment Methods and Their Applications in the Determination of Dicofol Residue in Aquatic Foods by Gas Chromatography-mass Spectrometry

建立了两种样品前处理方法应用于气相色谱串联质谱法测定水产品中三氯杀螨醇残留量。样品经氯化钠配合乙腈/水均质研磨,超声辅助提取,提取液经净化后,供气相色谱-质谱联用(GC/MS)分析。采用选择离子扫描方式(SIM),外标法定量。在优化前处理和上机条件下测试,三氯杀螨醇检出限(S/N≥10)为0.006mg/kg,在加标水平0.01～0.10mg/kg范围内,方法Ⅰ的回收率为76.8%～110.3%,RSD为3.06%～9.43%;方法Ⅱ的回收率为76.6%～100.4%,RSD为3.21%～8.35%。该方法的准确度和精密度符合农残分析要求,可为我国水产品出口提供技术支持。

Two sample pretreatment methods for the determination of dicofol residue in aquatic foods by gas chromatography-mass spectrometry（GC/MS）were established.The compounds were extracted using acetonitrile/water and NaCl assisted by ultrasonication,and the supernatants were purified by solid phase extractions prior to GC/MS analysis.The determinations were performed in selected ion monitoring（SIM）mode with external standard method for quantification.Under the optimal conditions of pretreatment and determination,the pesticide detection limit of the GC/MS method（S/N≥10）was 0.006mg/kg.With the addition of standard at the concentrations of 0.01～0.10mg/kg,the recoveries of the methodⅠ were 76.8%～110.3% with RSDs of 3.06%～9.43%,and the recoveries of the methodⅡ were 76.6%～100.4% with RSDs of 3.21%～8.35%.The method showed good recoveries and precisions,which could provide an effective technical support for China’s export of aquatic foods.