title: Multiresidue analysis of endocrine-disrupting compounds and perfluorinated sulfates and carboxylic acids in sediments by ultra-high-performance liquid chromatography-tandem mass spectrometry.
abstract: A multiresidue analytical method for the determination of 11 perfluorinated compounds and 22 endocrine-disrupting compounds (ECDs) including 13 natural and synthetic estrogens (free and conjugated forms), 2 alkylphenols, 1 plasticiser, 2 UV-filters, 1 antimicrobial, and 2 organophosphorus compounds in sediments has been developed. Ultrasound-assisted extraction followed by solid phase extraction (SPE) with graphitized carbon black (GCB) cartridge as clean-up step were used. The extraction process yield was optimized in terms of solvent composition. Then, a 3(2) experimental design was used to optimize solvent volume and sonication time by response surface methodology, which simplifies the optimization procedure. The final extract was analyzed by ultra-high performance liquid chromatography coupled with tandem mass spectrometry. The optimized sample preparation method is simple and robust, and allows recovery of ECDs belonging to different classes in a complex matrix such as sediment. The use of GCB for SPE allowed to obtain with a single clean-up procedure excellent recoveries ranging between 75 and 110% (relative standard deviation <16%). The developed methodology has been successfully applied to the analysis of ECDs in sediments from different rivers and lakes of the Lazio Region (Italy). These analyses have shown the ubiquitous presence of chloro-substituted organophosphorus flame retardants and bisphenol A, while other analyzed compounds were occasionally found at concentration between the limit of detection and quantification.
authors.affiliation: Dipartimento di Chimica, Università di Roma "La Sapienza", Rome, Italy.
authors.forename: Chiara
authors.initials: C
authors.lastname: Cavaliere
authors.affiliation: Dipartimento di Chimica, Università di Roma "La Sapienza", Rome, Italy. Electronic address: annalaura.capriotti@uniroma1.it.
authors.forename: Anna Laura
authors.initials: AL
authors.lastname: Capriotti
authors.affiliation: Dipartimento di Chimica, Università di Roma "La Sapienza", Rome, Italy.
authors.forename: Francesca
authors.initials: F
authors.lastname: Ferraris
authors.affiliation: Dipartimento di Chimica, Università di Roma "La Sapienza", Rome, Italy.
authors.forename: Patrizia
authors.initials: P
authors.lastname: Foglia
authors.affiliation: Dipartimento di Chimica, Università di Roma "La Sapienza", Rome, Italy.
authors.forename: Roberto
authors.initials: R
authors.lastname: Samperi
authors.affiliation: Dipartimento di Chimica, Università di Roma "La Sapienza", Rome, Italy.
authors.forename: Salvatore
authors.initials: S
authors.lastname: Ventura
authors.affiliation: Dipartimento di Chimica, Università di Roma "La Sapienza", Rome, Italy.
authors.forename: Aldo
authors.initials: A
authors.lastname: Laganà
mesh_terms: D002264:Carboxylic Acids / Q000032:analysis*; D002851:Chromatography, High Pressure Liquid; D002853:Chromatography, Liquid; D052244:Endocrine Disruptors / Q000032:analysis*; D004784:Environmental Monitoring / Q000295:instrumentation / Q000379:methods*; D004785:Environmental Pollutants / Q000032:analysis; D019015:Geologic Sediments / Q000737:chemistry*; D007558:Italy; D045483:Rivers; D052616:Solid Phase Extraction; D013431:Sulfates / Q000032:analysis*; D053719:Tandem Mass Spectrometry
chemical_list: D002264:Carboxylic Acids; D052244:Endocrine Disruptors; D004785:Environmental Pollutants; D013431:Sulfates
keywords: Endocrine-disrupting compounds; Experimental design; Graphitized carbon black; Liquid chromatography–mass spectrometry (LC–MS); Sediments; Solid phase extraction (SPE)