气相色谱-串联质谱法测定稻田水产品中26种持久性有机污染物

Determination of 26 persistent organic pollutants in aquatic products cultured in paddy field by gas chromatography-tandem mass spectrometry

建立了固相萃取净化气相色谱-串联质谱(GC-MS/MS)测定稻田水产品中26种持久性有机污染物残留的检测方法。样品经二氯甲烷-正己烷(1∶1,V/V)混合溶剂超声提取,由氨基固相萃取柱净化,采用气相色谱分离,在选择反应监测模式(SRM)下测定。结果表明,26种目标物在1~500μg/L范围内线性关系良好,相关系数R2均大于0.997,方法的检测限(LOD)为0.20~1.00μg/kg,定量限(LQD)为0.60~3.00μg/kg。26种目标物在鲤(Cyprinus carpio)和克氏原螯虾(Procambarus clarkii)空白样品中不同添加水平的平均回收率为70.6%~115.0%,相对标准偏差(RSD)为3.29%~10.90%。该方法适用于稻田水产品中26种持久性有机污染物的测定。

A method was established for the simultaneous determination of twenty-six persistent organic pollutants(POPs)in aquatic products cultured in paddy field by gas chromatography-tandem mass spectrometry(GC-MS/MS).Samples were extracted with dichloromethane-hexane(1∶1,V/V)by ultrasonic wave and purified by amino solid phase extraction column.The target compounds were separated by gas chromatography,and mass spectrometric acquisition was carried out by selective reaction monitoring(SRM)mode.The results showed that good linearities of 26 POPs were obtained in the range of 1-500μg/L,and the correlation coefficients were all greater than 0.997.The limits of detection(LODs)and quantitation(LQDs)were 0.20-1.00μg/kg and 0.60-3.00μg/kg respectively.The average recoveries of 26 analytes at different levels in the blank samples of Cyprinus carpio and Procambarus clarkii were between 70.6%and 115.0%,with RSDs of 3.29%-10.90%.This method is applicable to the determination of 26 POPs in aquatic products cultured in paddy field.