Abstract:
A method of ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-ESI-MS/MS)combined with improved QuEChERS was established for the determination of 13 perfluorinated compounds(PFCs)in animal-derived food. The samples were extracted with 0.2% hydrochloric acid acetonitrile and cleaned up with a sorbent mixture of N-propylethylenediamine(PSA),octadecyl bonded silica gel(C
18)and graphitized carbon black(GCB). The PFCs were separated by an Atlantis T3 reversed-phase column using gradient elution with a mixed solution of 2.5 mmol/L ammonium acetate methanol and 2.5 mmol/L ammonium acetate,and detected by electrospray ionization in negative mode using the multiple reaction monitoring(MRM)mode. The samples were quantified using isotope internal standard.The calibration curves of 13 PFCs were linear in the concentration range of 0.05~10 ng/mL. The limits of detection(LODs)were between 0.02 and 0.05 μg/kg,and the limits of quantitation(LOQs)were between 0.06 and 0.15 μg/kg. At the spiked levels of 0.2,1 and 2 μg/kg,the average recoveries were in the range of 62.3%~119.3%,with relative standard deviations(RSDs)of 3.5%~19.9%. With its simplicity,accuracy and high sensitivity,this method is suitable for the identification and quantification of 13 PFCs in animal-derived food.