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建立海产品中34种多氯联苯和76种农药气相色谱-串联质谱分析方法。用乙腈为萃取溶剂,均质法均质提取样品,盐析法除水,凝胶渗透色谱净化,收集26~50 min流出液,在线浓缩。用气相色谱柱(DB-1701)分离后,在多离子反应监测模式(MRM)下进行质谱检测。在1.0~500μg/kg范围内线性关系良好(R2﹥0.99),方法检出限(LOD)0.05~108.43μg/kg。空白样品添加回收率51.6%~120.5%,相对标准偏差范围0.84%~24.5%,回收率60%~110%,目标化合物为106种。该方法通用性强,选择性好,灵敏度、准确度和精密度均符合多残留检测的技术要求,适用于动物源性海产品中多残留的日常检测。
The establishment of 34 kinds of PCBs in seafood and 76 kinds of pesticides by gas chromatography - tandem mass spectrometry method. Acetonitrile was used as the extraction solvent. Homogenization was used to extract samples homogeneously. The samples were removed by salting-out method and purified by gel permeation chromatography. The effluent was collected for 26-50 min and concentrated on-line. After separation with a gas chromatographic column (DB-1701), mass spectrometry was performed in a multi-ion reaction monitoring mode (MRM). The linear range was 1.0 ~ 500μg / kg (R2> 0.99), and the limit of detection (LOD) was 0.05 ~ 108.43μg / kg. The recoveries of blank samples ranged from 51.6% to 120.5%, with relative standard deviations ranging from 0.84% to 24.5%. The recoveries ranged from 60% to 110% with 106 target compounds. The method has strong versatility, good selectivity, sensitivity, accuracy and precision meet the technical requirements of multi-residue detection, and is suitable for the daily detection of multiple residues in animal-derived seafood.