title: Analysis of antithyroid drugs in surface water by using liquid chromatography-tandem mass spectrometry.
abstract: This paper describes development and validation of a new method for the simultaneous determination of six antithyroid drugs (ATDs) in surface waters by using liquid chromatography-triple quadrupole mass spectrometry (LC-MS/MS). Target compounds include two ATD classes: thiouracil derivatives (thiouracil (TU), methyl-thiouracil (MTU), propyl-thiouracil (PTU), phenyl-thiouracil (PhTU)) and imidazole derivatives (tapazole (TAP), and mercaptobenzimidazole (MBI)). Sensitivity and selectivity of the LC-multiple reaction monitoring (MRM) analysis allowed applying a simple pre-concentration procedure and "shooting" the concentrated sample into the LC-MS/MS system without any other treatment. Recoveries were higher than 75% for all analytes. Intra-day precision and inter-day precision, calculated as relative standard deviation (RSD), were below 19 and 22%, respectively. Limits of detection (LODs) ranged from 0.05 to 0.25 μg/L; limits of quantitation (LOQs) varied between 0.15 and 0.75 μg/L. The validated method was successfully applied to the analysis of ATD residues in surface water samples collected from the Tiber River basin and three lakes of Lazio (central Italy). The analytes were quantified based on matrix-matched calibration curves with mercaptobenzimidazole-d4 (MBI-d4) as the internal standard (IS). The most widespread compound was TAP, one of the most common ATDs used in human medicine, but also TU and MBI were often detected in the analysed samples.
authors.affiliation: Department of Analytical Chemistry, Physical Chemistry and Chemical Engineering, Faculty of Chemistry, University of Alcalá, Ctra. Madrid-Barcelona, Km. 33.600, 28871 Alcalá de Henares (Madrid), Spain.
authors.forename: Virginia
authors.initials: V
authors.lastname: Pérez-Fernández
authors.affiliation: Dipartimento di Chimica, Facoltà di Scienze Matematiche Fisiche e Naturali, Università degli Studi di Roma "La Sapienza", P.le Aldo Moro 5, 00185 Roma, Italy.
authors.forename: Stefano
authors.initials: S
authors.lastname: Marchese
authors.affiliation: Dipartimento di Chimica, Facoltà di Scienze Matematiche Fisiche e Naturali, Università degli Studi di Roma "La Sapienza", P.le Aldo Moro 5, 00185 Roma, Italy. Electronic address: alessandra.gentili@uniroma1.it.
authors.forename: Alessandra
authors.initials: A
authors.lastname: Gentili
authors.affiliation: Department of Analytical Chemistry, Physical Chemistry and Chemical Engineering, Faculty of Chemistry, University of Alcalá, Ctra. Madrid-Barcelona, Km. 33.600, 28871 Alcalá de Henares (Madrid), Spain.
authors.forename: María Ángeles
authors.initials: MÁ
authors.lastname: García
authors.affiliation: Dipartimento di Chimica, Facoltà di Scienze Matematiche Fisiche e Naturali, Università degli Studi di Roma "La Sapienza", P.le Aldo Moro 5, 00185 Roma, Italy.
authors.forename: Roberta
authors.initials: R
authors.lastname: Curini
authors.affiliation: Dipartimento di Chimica, Facoltà di Scienze Matematiche Fisiche e Naturali, Università degli Studi di Roma "La Sapienza", P.le Aldo Moro 5, 00185 Roma, Italy.
authors.forename: Fulvia
authors.initials: F
authors.lastname: Caretti
authors.affiliation: Dipartimento di Chimica, Facoltà di Scienze Matematiche Fisiche e Naturali, Università degli Studi di Roma "La Sapienza", P.le Aldo Moro 5, 00185 Roma, Italy.
authors.forename: Daniela
authors.initials: D
authors.lastname: Perret
mesh_terms: D013956:Antithyroid Agents / Q000032:analysis*; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D060106:Lakes / Q000737:chemistry*; D057230:Limit of Detection; D045483:Rivers / Q000737:chemistry*; D053719:Tandem Mass Spectrometry / Q000379:methods*; D014874:Water Pollutants, Chemical / Q000032:analysis*
chemical_list: D013956:Antithyroid Agents; D014874:Water Pollutants, Chemical
keywords: Antithyroid drugs; Liquid chromatography–tandem mass spectrometry; Multi-residue analytical method; River water analysis; Surface water analysis; Thyreostatics