title: Validated method for the determination of perfluorinated compounds in placental tissue samples based on a simple extraction procedure followed by ultra-high performance liquid chromatography-tandem mass spectrometry analysis.
abstract: Xenobiotic exposure during pregnancy is inevitable. Determination of perfluorinated compounds (PFCs), chemicals described as environmental contaminants by Public Health Authorities due to their persistence, bioaccumulation and toxicity, is a challenge. In the present work, a method based on a simplified sample treatment involving freeze-drying, solvent extraction and dispersive clean-up of the extracts using C18 sorbents followed by an ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) analysis was developed and validated for the determination of five perfluorinated carboxylic acids (C4-C8) and perfluorooctane sulfonate (PFOS) in placental tissue samples. The most influential parameters affecting the extraction method and clean-up were optimized using Design of Experiments (DOE). The method was validated using matrix-matched calibration. Found limits of detection (LODs) ranged from 0.03 to 2 ng g(-1) and limits of quantification (LOQs) from 0.08 to 6 ng g(-1), while inter- and intra-day variability was under 14% in all cases. Recovery rates for spiked samples ranged from 94% to 113%. The method was satisfactorily applied for the determination of compounds in human placental tissue samples collected at delivery from 25 randomly selected women.
authors.affiliation: Department of Analytical Chemistry, Superior Polytechnic School, University of Seville, C/Virgen de África 7, E-41011 Seville, Spain.
authors.forename: J
authors.initials: J
authors.lastname: Martín
authors.affiliation: Research Group of Analytical Chemistry and Life Sciences, Department of Analytical Chemistry, University of Granada, Campus of Fuentenueva, E-18071 Granada, Spain.
authors.forename: R
authors.initials: R
authors.lastname: Rodríguez-Gómez
authors.affiliation: Research Group of Analytical Chemistry and Life Sciences, Department of Analytical Chemistry, University of Granada, Campus of Fuentenueva, E-18071 Granada, Spain. Electronic address: azafra@ugr.es.
authors.forename: A
authors.initials: A
authors.lastname: Zafra-Gómez
authors.affiliation: Department of Analytical Chemistry, Superior Polytechnic School, University of Seville, C/Virgen de África 7, E-41011 Seville, Spain.
authors.forename: E
authors.initials: E
authors.lastname: Alonso
authors.affiliation: Research Group of Analytical Chemistry and Life Sciences, Department of Analytical Chemistry, University of Granada, Campus of Fuentenueva, E-18071 Granada, Spain.
authors.forename: J L
authors.initials: JL
authors.lastname: Vílchez
authors.affiliation: Research Group of Analytical Chemistry and Life Sciences, Department of Analytical Chemistry, University of Granada, Campus of Fuentenueva, E-18071 Granada, Spain.
authors.forename: A
authors.initials: A
authors.lastname: Navalón
mesh_terms: D005591:Chemical Fractionation / Q000379:methods*; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D004785:Environmental Pollutants / Q000032:analysis / Q000737:chemistry / Q000302:isolation & purification; D005260:Female; D005466:Fluorocarbons / Q000032:analysis* / Q000737:chemistry / Q000302:isolation & purification*; D005612:Freeze Drying; D006801:Humans; D057230:Limit of Detection; D016014:Linear Models; D010920:Placenta / Q000737:chemistry*; D011247:Pregnancy; D011786:Quality Control; D012997:Solvents / Q000737:chemistry; D053719:Tandem Mass Spectrometry / Q000379:methods*; D013696:Temperature; D013997:Time Factors
chemical_list: D004785:Environmental Pollutants; D005466:Fluorocarbons; D012997:Solvents
keywords: Dispersive solid phase extraction; Perfluorinated compounds; Placental tissue; UHPLC–MS/MS