Validation of a GC-MS/MS method for simultaneous determination of 86 persistent organic pollutants in marine sediments by pressurized liquid extraction followed by stir bar sorptive extraction |
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Authors: | Camino-Sánchez F J Zafra-Gómez Alberto Pérez-Trujillo J P Conde-González J E Marques J C Vílchez José Luis |
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Institution: | a Laboratories Cavendish S.L.U.™, Research Department, E-18220 Granada, Spain b Research Group of Analytical Chemistry and Life Sciences, Department of Analytical Chemistry, Faculty of Sciences, University of Granada, Avda. Fuentenueva s/n, E-18071 Granada, Spain c Analytical Chemistry Department, University of La Laguna, E-38204 Tenerife, Spain d Exact Sciences and Engineering Center, University of Madeira, Penteada 9000-390, Portugal |
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Abstract: | A multiresidue method for the analysis of 86 persistent pollutants in marine sediments at ultra-trace level has been developed and validated using pressurized liquid extraction (PLE) and stir-bar sorptive extraction (SBSE) coupled with thermal desorption and gas chromatography-triple quadrupole mass spectrometry (TD-GC-MS/MS QqQ). The compounds analyzed belong to various families such as polychlorinated biphenyls, polycyclic aromatic hydrocarbons, polybrominated diphenylethers, organophosphorus and organochlorine pesticides and other pesticides such as urons, and triazines. The analytes have very different polarities and log Kow values, which is an important parameter in the optimization of a SBSE method. Due to PLE high efficiency and throughput rates, along with the proven ability for multiresidue analysis and excellent sensitivity of SBSE, we present an efficient method. The limits of quantification obtained ranged from 0.014 to 1.0 ng g−1, with detection limits below pg g−1 levels. In order to validate the proposed methodology, quality parameters such as recovery, linearity and reproducibility were studied. Recoveries ranged from 63% to 119%, reproducibility (in terms of Relative Standard Deviation for ten determinations) was lower than 35% in all cases, and determination coefficients higher than 0.990 for all analytes. The main factors that affect PLE, SBSE and GC-MS/MS procedures were optimized. The method was applied to the analysis of nine marine sediments obtained from the nine main submarine wastewater discharge points (emissaries) presents along the coast of Tenerife Island (Canary Islands, Spain). |
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Keywords: | Pressurized liquid extraction Stir bar sorptive extraction GC-MS/MS Marine sediments Persistent pollutants |
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