水产品中十氯酮农药残留的气相色谱测定和气相色谱-质谱联用确证方法的建立

Determination of Residual Chlordecone in Aquatic products by Gas Chromatography and Gas Chromatography-Mass Spectrometry

建立固相萃取-气相色谱法检测和气相色谱-质谱法确证水产品中十氯酮残留的分析方法。先使用正己烷配合乙腈、水对样品进行均质提取，再加入氯化钠继续均质，离心分层。取部分乙腈浓缩后过Florisil柱净化，用乙酸乙酯-正己烷（体积比1：9）溶剂淋洗去除油脂和其他杂质，再使用丙酮-正己烷（体积比1：9）溶剂洗脱分析物供气相色谱仪（GC）和气相色谱-质谱仪（GC—MS）分析。气相色谱检测采用电子捕获检测器（ECD），气相色谱-质谱联用确证采用选择离子监测方式（SIM）．外标法定量。在优化的样品前处理条件和仪器测试条件下，方法的定量限（RSN≥10）为0．01mg／kg，在加标水平为0．01-0．10mg／kg时，回收率为73％-110％，相对标准偏差为3．5％-10.4％。该方法准确、快速、灵敏，可满足水产品中十氯酮农药残留的检测要求。

A method for the determination of chlordecone residue in aquatic products was developed by gas chro-matography （GC） and gas chromatography-mass spectrometry （GC-MS）. For the method, the residue was extracted from homogenized tissue with aeetonitrile-water assisted by n-hexane, separated with liquid-liquid partition. The supernatant was purified using solid phase extraction（Florisil column） prior to the GC and GC-MS analysis. Determinations were per-formed by using electron capture detector （ECD） in GC method and selected ion monitoring （SIM） mode in GC-MS method,then external standard method was used in the quantification.The method was convenient and rapid after investi-gating the conditions of pretreatment and determination.Under the optimal conditions; the detection limit of the method （RSN≥ 10） was 0.01 mg/kg. Tests for recovery were carried by addition of standard at concentration of 0.01 mg/kg, 0.04 mg/kg and 0.10 mg/kg, the results were 73%-110%, and the relative standard deviations were in the range of 3.5%-10.4%. The method owns the advantages of easy, fast, and more sensitive, which can meet the requirement of the de- termination of chlordecone residue in aquatic products.