High performance liquid chromatography tandem mass spectrometry determination of perfluorinated acids in cow milk

Abstract

A new and sensitive liquid chromatography/electrospray-tandem mass spectrometric (LC/ESI-MS/MS) method for the determination of 12 perfluorinated compounds (PFCs) in cow milk is described. Milk samples were extracted with acetone and cleaned-up by a graphitized carbon black solid-phase extraction cartridge, optimizing the entire procedure by using a screening experimental design. LC/ESI-MS/MS was performed in negative ion mode using multiple reaction monitoring mode. The performance of the method was evaluated under the optimized conditions in terms of matrix effects, range of linearity, accuracy, and repeatability. For all compounds, linearity in matrix was observed in the range LOQ-10μgL(-1), and coefficients of determination R(2) ranged from 0.9982 to 0.9999. The analytical recoveries, relative to the isotopic internal standard, measured at 10 and 50ngL(-1) were in the range of 91-105%, with relative standard deviations below 6% and method detection limit, based on the blank value +3 times the standard deviation of the blank, ranged from 0.5 to 3ngL(-1). The final method developed was used to determine the concentration of PFCs in 15 retail milk samples. None of these compounds were detected in cow milk analyzed samples.

Keywords: Experimental design; Graphitized carbon black; LC–MS; Milk; Perfluoro acids; Solid phase extraction (SPE).