凝胶渗透色谱-气相串联质谱同时测定海产品中34种多氯联苯和76种农药

The Simultaneous Determination of 34 Poly Chlorinated Biphenyls and 76 Residual Analysis of Pesticides in Marine Product by GPC-GC-MS/MS

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。

A gel permeation chromatography （GPC）-Gas Chromatography-tandem Mass Spectrometry （GC-MS/MS） method combined was developed for the simultaneous determination of 34 Poly Chlorinated Biphenyls （PCBS） and 76 residual analysis of pesticides in marine product. The samples were extracted with acetonitrile, dehydrated with salting out method and cleaned-up by gel permeation chromatography （GPC）. The GPC eluant collected from 26 min to 50 min was concentrated to 1 mL, then analyzed using GC-MS/MS. A DB-1701 column was used for the separation. The MS detec- tion was performed in multiple reaction monitoring mode （MRM）. Calibration curves showed good linearity in the range of 1.0 to 500 μg/kg for all compounds （R2 〉 0.99）, and the limit of detection（LOD） ranged from 0.05 to 108.43 μg/kg. Recoveries in spiked samples were 51.6% to120.5% with RSD of 0.84% to 24.5%. The number of compounds with the average spiked recoveries of which were between 60% and 110% was 106. The sensitivity and accuracy of the method met the requirements of the multiple residues. This method was selective, accurate and easy to operate, and could be used for the routine analysis of the multiple residues in marine product.