Determination of perfluorosulfonate and perfluorocarboxylate precursors in eggs by ultra-highperformance liquid chromatography-mass spectrometry

Abstract

To develop a method for the determination of 11 perfluorosulfonate and perfluorocarboxylate precursors in eggs using ultra-high performance liquid chromatography-tandem quadruple mass spectrometry (UPLC-MS/MS). The target compounds of egg were extracted with 100 mmol/L NaOH-acetonitrile /water(90∶10, V/V) by ultrasonic. Then the extract was purified by solid phase extraction (Waters Oasis(@) WAX 6cc) and then eluted with 9% NH4OH in methanol. The target compounds were separated on a Waters ACQUITY(TM) BEH (18)C column (50 mm × 2.1 mm, 1.7 μm) and detected by negative electrospray ionization (ESI(-)) mass spectrometry in multiple reaction monitoring mode (MRM). All compounds were quantified with internal standards. The accuracy, precision and the limits of detection and quantification of the method were evaluated. Then we detected 7 different egg samples from the market. The average recoveries for the eleven precursors at 3 levels were 74.09%-116.82% and the relative standard deviations were 2.37%-13.62%. The limits of detection (LOD) of the method were in the range of 0.06-1.50 pg/g (wet weight) and the limits of quantification (LOQ) were in the range of 0.15-3.00 pg/g (wet weight). And 5 target compounds were detected in the 7 market samples. 6:2 fluorotelomer sulfonate (6:2 FTS) was detected in all of samples with the concentrations of 1.67-3.11 pg/g. 6:2 fluorotelomer unsaturated acid (FHUEA) and 6:2 disubstituted polyfluoroalkyl phosphate ester (6:2 diPAP) were detected in 6 samples and the concentrations were<LOD-5.11 pg/g and 3.78-9.16 pg/g, respectively. And the concentrations of 8:2 fluorotelomer sulfonate (8:2 FTS) and N-methyl perfluorooctane sulfonamidoacetic acid (N-Me FOSAA) founded in the same sample were 105.78, and 4.95 pg/g, respectively. This method was simple, rapid, and suitable for determination of perfluorosulfonate and perfluorocarboxylate precursors in eggs with high accuracy and sensitivity. It could also be applied to human burden studies of these precursors.