PMID- 22673809 OWN - NLM STAT- MEDLINE DCOM- 20120904 LR - 20120626 IS - 1873-3778 (Electronic) IS - 0021-9673 (Linking) VI - 1247 DP - 2012 Jul 20 TI - Solid-phase extraction combined with large volume injection-programmable temperature vaporization-gas chromatography-mass spectrometry for the multiresidue determination of priority and emerging organic pollutants in wastewater. PG - 104-17 LID - 10.1016/j.chroma.2012.05.022 [doi] AB - In the present work the simultaneous extraction for the multiresidue determination in wastewater samples of organic compounds such as polychlorinated biphenyls (PCBs), polybrominated biphenyls (PBBs), pesticides, polycyclic aromatic hydrocarbons (PAHs), phthalate esters (PEs), alkylphenols (APs), bisphenol A (BPA) or hormones included in different lists of priority and emerging pollutants because of their action as endocrine disrupting compounds (EDCs) was developed. Different solid phase extraction (SPE) variables such as the nature of the solid phase (Oasis-HLC, C18 and Lichrolut), the sample volume, the addition of MeOH and NaCl, the pH of the water phase and the volume of the eluent solvent were optimized in order to analyze simultaneously the priority and emerging families of pollutants mentioned above. Good recoveries were obtained for Milli-Q water (80-120%), however, since the use of deuterated analogues and dilution of the sample did not correct the matrix effect, additional SPE clean-up step using Florisil(R) cartridges was necessary to obtain good results for wastewater samples (80-125%). In order to improve the limits of detection (LODs), large volume injection (LVI) using programmable temperature vaporizer (PTV) coupled to gas chromatography-mass spectrometry (GC-MS) was also optimized. Since analytes losses in the case of the most volatile congeners occurred during the derivatization step and no separation of the derivatized and the non-derivatized analytes was possible during SPE elution, two different injections were optimized for each analyte group. LODs were in good agreement with those found in the literature and relative standard deviations (RSDs) were in the 10-25% range for Milli-Q and 12-30% for wastewater samples. The method was finally applied to the determination of target analytes in three different wastewater treatment plants (WWTPs, Bakio, Gernika and Galindo (Spain)) and in one water purification plant (WPP) in Zornotza (Spain). CI - Copyright (c) 2012 Elsevier B.V. All rights reserved. FAU - Bizkarguenaga, E AU - Bizkarguenaga E AD - Department of Analytical Chemistry, Faculty of Science and Technology, University of the Basque Country-UPV/EHU, PK 644, 48080 Bilbao, Spain. FAU - Ros, O AU - Ros O FAU - Iparraguirre, A AU - Iparraguirre A FAU - Navarro, P AU - Navarro P FAU - Vallejo, A AU - Vallejo A FAU - Usobiaga, A AU - Usobiaga A FAU - Zuloaga, O AU - Zuloaga O LA - eng PT - Journal Article PT - Research Support, Non-U.S. Gov't DEP - 20120514 PL - Netherlands TA - J Chromatogr A JT - Journal of chromatography. A JID - 9318488 RN - 0 (Organic Chemicals) RN - 0 (Water Pollutants, Chemical) SB - IM MH - Gas Chromatography-Mass Spectrometry/*methods MH - Limit of Detection MH - Organic Chemicals/*analysis/chemistry/isolation & purification MH - Reproducibility of Results MH - Solid Phase Extraction/*methods MH - Temperature MH - Waste Disposal, Fluid/*methods MH - Water Pollutants, Chemical/*analysis/chemistry/isolation & purification MH - Water Purification EDAT- 2012/06/08 06:00 MHDA- 2012/09/05 06:00 CRDT- 2012/06/08 06:00 PHST- 2012/02/27 00:00 [received] PHST- 2012/04/16 00:00 [revised] PHST- 2012/05/06 00:00 [accepted] PHST- 2012/06/08 06:00 [entrez] PHST- 2012/06/08 06:00 [pubmed] PHST- 2012/09/05 06:00 [medline] AID - S0021-9673(12)00724-8 [pii] AID - 10.1016/j.chroma.2012.05.022 [doi] PST - ppublish SO - J Chromatogr A. 2012 Jul 20;1247:104-17. doi: 10.1016/j.chroma.2012.05.022. Epub 2012 May 14.