UPLC-MS/MS法检测肉类组织中的11种全氟化合物

Determination of Eleven Perfluorinated Compounds in Meat by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

建立了肉类组织中11种常见全氟化合物(全氟丁烷磺酸、全氟己烷磺酸、全氟庚酸、全氟辛酸、全氟辛烷磺酸、全氟壬酸、全氟癸酸、全氟十一酸、全氟癸烷磺酸、全氟十二酸、全氟十四酸)的Waters OasisHLB固相萃取净化/超高效液相色谱-串联质谱(UPLC-MS/MS)分析方法。肉类组织中加入内标,经乙腈均质、提取后,用玻璃纤维真空抽滤,再用乙腈饱和的正己烷除脂净化,经Waters Oasis HLB固相萃取小柱富集净化,氮吹浓缩,超高效液相色谱(UPLC)分离,以2 mmol/L醋酸铵-2 mmol/L醋酸铵甲醇溶液为流动相,使用串联四极杆电喷雾离子源负离子扫描,多反应监测(MRM)模式检测,内标法定量。11种全氟化合物在0.50～20.0μg/L范围内线性关系良好,方法的检出限为0.014～0.060μg/kg,定量下限为0.047～0.199μg/kg,回收率为70.9%～107.1%,相对标准偏差(RSD,n=6)为0.4%～11.4%。该方法具有净化效果好、定量准确、灵敏度高的特点,适用于肉类组织中11种常见全氟化合物的快速确认和准确定量。

A method was developed for the determination of 11 perfluorinated compounds（PFCs）（e.g.perfluorobutanesulfonate,perfluorohexane sulfonate,perfluoroheptanoic acid,perfluorooctanoate,perfluorooctane sulfonate,perfluorononanoic acid,perluorodecanoic acid,perfluoroundecanoic acid,perfluorodecanesulfonate,perfluorododecanoic acid and perfluorotetradecanoic acid）in meat by ultra performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS） with solid phase extraction column.After added with the isotopic labeled sodium perfluoro-1-[1,2,3,4,-13C4]octanesulfonat（MPFOA） and perfluoro-n-[1,2,3,4,-13C4]octanoic acid（MPFOS）,the samples were extracted and homogenized with acetonitrile,and then suction filted through glass fiber and defatted with n-hexane by liquid-liquid extraction method.The extract was purified with Waters Oasis HLB solid phase extraction column,and concentrated with N2.The perfluorinated compounds were separated with UPLC using a mixture of 2 mmol/L ammonium acetate-2 mmol/L ammonium acetate methanol solution as mobile phase,and analysed by UPLC-MS/MS ESI（-） under MRM mode with the internal standard method.The calibration curves were linear in the range of 0.50-20.0 μg/L for 11 PFCs.The limits of detection for the method（LODs） were between 0.014 μg/kg and 0.060 μg/kg,and the limits of quantitation were between 0.047 μg/kg and 0.199 μg/kg.The mean recoveries were in the range of 70.9%-107.1%,with relative standard deviations（RSDs,n=6） of 0.4%-11.4%.This method was suitable for the identification and quantification of 11 perfluorinated compounds in meat due to its simplicity,accuracy and high sensitivity.