title: Fluorocarbon-bonded magnetic mesoporous microspheres for the analysis of perfluorinated compounds in human serum by high-performance liquid chromatography coupled to tandem mass spectrometry.
abstract: 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.
authors.affiliation: Department of Pharmaceutical Analysis, School of Pharmacy, Fudan University, No. 826 Zhangheng Road, Shanghai 201203, PR China.
authors.forename: Xiaodan
authors.initials: X
authors.lastname: Liu
authors.affiliation: Department of Pharmaceutical Analysis, School of Pharmacy, Fudan University, No. 826 Zhangheng Road, Shanghai 201203, PR China.
authors.forename: Yingjia
authors.initials: Y
authors.lastname: Yu
authors.affiliation: Department of Pharmaceutical Analysis, School of Pharmacy, Fudan University, No. 826 Zhangheng Road, Shanghai 201203, PR China. Electronic address: yanli@fudan.edu.cn.
authors.forename: Yan
authors.initials: Y
authors.lastname: Li
authors.affiliation: Department of Biology, Dezhou University, Shandong 253023, PR China.
authors.forename: Haiying
authors.initials: H
authors.lastname: Zhang
authors.affiliation: Department of Pharmaceutical Analysis, School of Pharmacy, Fudan University, No. 826 Zhangheng Road, Shanghai 201203, PR China.
authors.forename: Jin
authors.initials: J
authors.lastname: Ling
authors.affiliation: Department of Pharmaceutical Analysis, School of Pharmacy, Fudan University, No. 826 Zhangheng Road, Shanghai 201203, PR China.
authors.forename: Xueni
authors.initials: X
authors.lastname: Sun
authors.affiliation: Department of Pharmaceutical Analysis, School of Pharmacy, Fudan University, No. 826 Zhangheng Road, Shanghai 201203, PR China.
authors.forename: Jianan
authors.initials: J
authors.lastname: Feng
authors.affiliation: Department of Pharmaceutical Analysis, School of Pharmacy, Fudan University, No. 826 Zhangheng Road, Shanghai 201203, PR China.
authors.forename: Gengli
authors.initials: G
authors.lastname: Duan
mesh_terms: D017738:Alkanesulfonic Acids / Q000097:blood*; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D005466:Fluorocarbons / Q000097:blood / Q000737:chemistry*; D006801:Humans; D008280:Magnetics; D046529:Microscopy, Electron, Transmission; D008863:Microspheres; D012015:Reference Standards; D017550:Spectroscopy, Fourier Transform Infrared; D053719:Tandem Mass Spectrometry / Q000379:methods*
chemical_list: D017738:Alkanesulfonic Acids; D005466:Fluorocarbons; C076994:perfluorooctane sulfonic acid
keywords: Fluorous solid phase extraction (F-SPE); High-performance liquid chromatography coupled to tandem mass spectrometry (LC–MS/MS); Human serum; Magnetic mesoporous microspheres; Perfluorinated compounds (PFCs)