title: Determination of perfluorinated compounds in mollusks by matrix solid-phase dispersion and liquid chromatography-tandem mass spectrometry.
abstract: Perfluorinated compounds (PFCs) have been used for over 40 years in different commercial and industrial applications mainly as surfactants and surface protectors and have become an important class of marine emerging pollutants. This study presents the development and validation of a new analytical method to determine the simultaneous presence of eight PFCs in different kinds of mollusks using matrix solid-phase dispersion (MSPD) followed by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Simplicity of the analytical procedure, low volume of solvent and quantity of sample required, low global price, and integration of extraction and clean-up into a single step, are the most important advantages of the developed methodology. Solvent, solid support (dispersing agent), clean-up sorbent, and their amounts were optimized by means of an experimental design. In the final method, 0.5 g of sample are dispersed with 0.2 g of diatomaceous earth and transferred into a polypropylene syringe containing 4 g of silica as clean-up sorbent. Then, analytes are eluted with 20 mL of acetonitrile. The extract is finally concentrated to a final volume of 0.5 mL in methanol, avoiding extract dryness in order to prevent evaporation losses and injected in the LC-MS/MS. The combination of this MSPD protocol with LC-MS/MS afforded detection limits from 0.05 to 0.3 ng g(-1). Also, a good linearity was established for the eight PFCs in the range from limit of quantification (LOQ) to 500 ng mL(-1) with R(2) > 0.9917. The recovery of the method was studied with three types of spiked mollusk and was in the 64-126% range. Moreover, a mussel sample was spiked and aged for more than 1 month and analyzed by the developed method and a reference method, ion-pair extraction, for comparison, producing both methods statistically equal concentration values. The method was finally applied to the determination of PFCs in different kinds of mollusks revealing concentrations up to 8.3 ng g(-1) for perfluoroundecanoic acid.
authors.affiliation: Department of Analytical Chemistry, Nutrition and Food Science, IIAA-Institute for Food Analysis and Research, University of Santiago de Compostela, Santiago de Compostela, Spain.
authors.forename: Eugenia
authors.initials: E
authors.lastname: Villaverde-de-Sáa
authors.forename: José Benito
authors.initials: JB
authors.lastname: Quintana
authors.forename: Rosario
authors.initials: R
authors.lastname: Rodil
authors.forename: Raúl
authors.initials: R
authors.lastname: Ferrero-Refojos
authors.forename: Elisa
authors.initials: E
authors.lastname: Rubí
authors.forename: Rafael
authors.initials: R
authors.lastname: Cela
mesh_terms: D000818:Animals; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D005466:Fluorocarbons / Q000032:analysis / Q000302:isolation & purification*; D008974:Mollusca / Q000737:chemistry*; D052616:Solid Phase Extraction / Q000379:methods*; D053719:Tandem Mass Spectrometry / Q000379:methods*; D014874:Water Pollutants, Chemical / Q000032:analysis* / Q000302:isolation & purification*
chemical_list: D005466:Fluorocarbons; D014874:Water Pollutants, Chemical