凝胶色谱净化-气相色谱串联质谱法测定海产品中得克隆残留量

Determination of the Dechlorane Plus in Seafoods by GPC and GC-MS/MS

建立了凝胶色谱(GPC)净化、气相色谱-串联质谱(GC-MS/MS)测定海产品中得克隆的方法。得克隆包括syn-DP和anti-DP两种异构体,样品中的得克隆经正己烷/丙酮(1:1,v/v)溶液提取、GPC净化后,GC-MS/MS采用多反应监测模式(MRM)采集数据后进行定性/定量分析。得克隆的加标回收率:syn-DP测定回收率为89.3%~102.5%;anti-DP测定回收率为85.4%~102.1%。syn-DP和anti-DP的检出限分别为0.2μg/kg和0.5μg/kg(S/N=3)。方法的相对标准偏差(RSD)均≤10.0%。采用本方法对采自温州的美国红鱼、中国毛虾,采自台州的鲈鱼,以及采自舟山的大黄鱼进行检测分析,结果上述样品均未检出。

A method of determination Dechlorane Plus （DP） in seafoods by gel permeation chromatography （GPC） purification and gas chromatography-tandem mass spectrometry （GC/MS-MS） detection.The Dechloran Plus were extracted using hexane and acetone （1： 1, v/v）. The fire retardants extracted from sample were separated and purified with matrices such as fat by GPC. The fire retardants were finally separated and detected by GC-MS/MS with multiple reaction monitoring （MRM） mode. The recoveries for syn-DP standards spiked were between 89.3% and 102.5%, and these for anti-DP were between 85.4% and 102.1%. The limits of detecion （LOD） were 0.2μg/kg of syn-DP and 0.5μg/kg of anti-DP（S/N=3）. Dechlorane Plus was not founded in American Red fish and Acetes chinensis from Wenzhou, Japanese sea bass from Taizhou, Large Yellow Croaker from Zhoushan.