Multi-residue analysis of pharmaceutical compounds in wastewaters by dual solid-phase microextraction coupled to liquid chromatography electrospray ionization ion trap mass spectrometry

Unceta, N. and Sampedro, M.C. and Bakar, N.K.A. and Gómez-Caballero, A. and Goicolea, M.A. and Barrio, R.J. (2010) Multi-residue analysis of pharmaceutical compounds in wastewaters by dual solid-phase microextraction coupled to liquid chromatography electrospray ionization ion trap mass spectrometry. Journal of Chromatography A, 1217 (20). pp. 3392-3399. ISSN 00219673 , DOI https://doi.org/10.1016/j.chroma.2010.03.008.

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Abstract

The aim of this article is to present a new procedure based on dual solid-phase microextraction (dSPME) for the simultaneous extraction of 16 pharmaceutical compounds with acidic and basic characteristics in urban wastewaters. Water samples are divided into two aliquots of 2mL each extracted by two CW-TPR fibers at different pH values (pH 3 and 11) and with a NaCl concentration of 300gL-1 at 75°C for 30min. The analytes in both fibers are desorbed one after the other in the desorption chamber in static mode with mobile phase for 10min. The extracts are injected into an LC system coupled to an ion trap mass spectrometer, leading to the accurate quantification of 16 pharmaceutical compounds in wastewaters, in MS2 mode. All the target compounds found in wastewaters provide good signals corresponding to the protonated precursor ion M+H+. The parameters influencing adsorption and desorption of the analytes on fiber were optimized. The assessment of the analytical method was performed by studying the linearity (LOQ to 10ngmL-1) and the intra- and interday accuracy (89.2-109.7%) and precision (RSD <13.6%). The quantification limits obtained ranged between 0.005 and 0.05μgL-1. The application of the method to real samples proves its effectiveness in identifying and detecting naproxen, valsartan, bezafibrate, torasemide, diclofenac, carbamazepine, citalopram, lorazepan, fluoxetine, imipramine and amitriptyline in influent and effluent wastewater treatment plant samples.

Item Type: Article
Funders: UNSPECIFIED
Uncontrolled Keywords: Dual-SPME Emerging pollutant Ion trap analyser LC-ESI-ITMS Pharmaceutical Wastewater Amitriptyline Analytes Analytical method Bezafibrate Carbamazepine Citalopram Diclofenac Emerging pollutants Fluoxetine Ion trap mass spectrometer Ion traps Liquid chromatography electrospray Mobile phase Multi-residue analysis NaCl concentration Naproxens pH value Pharmaceutical compounds Pharmaceutical wastewater Protonated Quantification limit Real samples Solid-phase microextraction Target compound Torasemide Urban wastewater Valsartan Wastewater treatment plants Water samples Adsorption Amides Desorption Effluent treatment Effluents Electrospray ionization Ions Liquid chromatography Mass spectrometers Mass spectrometry Sodium chloride Solvent extraction Wastewater reclamation Water treatment plants Wastewater treatment imipramine lorazepam naproxen accuracy article controlled study drug isolation electrospray mass spectrometry pH priority journal process optimization quantitative analysis solid phase microextraction urban area waste water water sampling Chromatography, Liquid Pharmaceutical Preparations Spectrometry, Mass, Electrospray Ionization Water Pollutants, Chemical
Subjects: Q Science > QD Chemistry
Divisions: Faculty of Science > Department of Chemistry
Depositing User: miss munirah saadom
Date Deposited: 02 Jul 2013 01:38
Last Modified: 02 Jul 2013 01:38
URI: http://eprints.um.edu.my/id/eprint/6258

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