Fluorocarbon-bonded magnetic mesoporous microspheres for the analysis of perfluorinated compounds in human serum by high-performance liquid chromatography coupled to tandem mass spectrometry.

We report herein an extraction method for the analysis of perfluorinated compounds in human serum based on magnetic core-mesoporous shell microspheres with decyl-perfluorinated interior pore-walls (Fe3O4@mSiO2-F17). Thanks to the unique properties of the Fe3O4@mSiO2-F17 microspheres, macromolecules like proteins could be easily excluded from the mesoporous channels due to size exclusion effect, and perfluorinated compounds (PFCs) in protein-rich biosamples such as serum could thus be directly extracted with the fluorocarbon modified on the channel wall without any other pretreatment procedure. The PFCs adsorbed Fe3O4@mSiO2-F17 microspheres could then be simply and rapidly isolated by using a magnet, followed by being identified and quantified by LC-MS/MS (high-performance liquid chromatography coupled to tandem mass spectrometry). Five perfluorinatedcarboxylic acids (C6, C8-C11) and perfluorooctane sulfonate (PFOS) were selected as model analytes. In order to achieve the best extraction efficiency, some important factors including the amount of Fe3O4@mSiO2-F17 microspheres added, adsorption time, type of elution solvent, eluting solvent volume and elution time were investigated. The ranges of the LOD were 0.02-0.05 ng mL(-1) for the six PFCs. The recovery of the optimized method varies from 83.13% to 92.42% for human serum samples.