同位素稀释-超高效液相色谱-串联质谱法测定鱼肉中8 种全氟化合物

建立鱼肉中8 种全氟化合物的同位素稀释-超高效液相色谱-串联质谱快速分析方法。鱼肉加入同位素内标 后使用乙腈超声萃取，经WAX固相萃取小柱净化后，采用C18反相色谱柱进行分离，用配有电喷雾离子源的三重四 极杆质谱进行多反应离子监测，同位素稀释内标法定量。8 种全氟化合物在0.1～50.0 μg/L范围内线性关系良好， 相关系数不低于0.998，方法检出限在0.03～0.15 μg/kg之间，平均加标回收率为87.7%～104.4%，相对标准偏差为 4.1%～10.7%。该法灵敏度高、快速准确，适用鱼肉中全氟化合物的定性和定量检测。

Determination of Eight Perfluorinated Compounds in Fish Muscles by Isotope Dilution Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

A method for the rapid determination of eight perfluorinated compounds (PFCs) in fish muscles was developed
by isotope dilution ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS-MS). Samples were
extracted with acetonitrile after addition of eight isotopically labeled internal standards. The extracts were cleaned up on a
WAX solid phase extraction column. The target compounds were separated on a ZORBAX Eclipse plus C18 (100 mm ×
3.0 mm, 3.5 μm) and analyzed by a triple quadruple tandem mass spectrometer with electrospray ionization source (EIS)
in multiple reaction monitoring (MRM) mode. The analytes were quantified by the internal standards labeled with stable
isotopes. The standard curves were linear in the ranges of 0.1–50.0 μg/L for 8 PFCs with correlation coefficients greater than
0.998. The limits of detection were 0.03–0.15 μg/kg. The average recoveries of PFCs in fish muscles were in the range of
87.7%–104.4%. The relative standard deviations (RSD) for PFCs were in the range of 4.1%–10.7%. These results show that
the method is sensitive and accurate, and suitable for the qualitative and quantitative determination of PFCs residues in fish
muscle samples.