Journal of Chromatography A, 1216 (2009) 4071–4082 Contents lists available at ScienceDirect Journal of Chromatography A journal homepage: www.elsevier.com/locate/chroma A new gas chromatography/mass spectrometry method for the simultaneous analysis of target and non-target organic contaminants in waters M.J. Gómez a,b,∗ , M.M. Gómez-Ramos a , A. Agüera a , M. Mezcua a , S. Herrera a , A.R. Fernández-Alba b a Pesticide Residue Research Group, University of Almería, 04120 Almería, Spain b IMDEA-Agua, Madrid, Spain article info Article history: Received 29 December 2008 Received in revised form 20 February 2009 Accepted 27 February 2009 Available online 6 March 2009 Keywords: Gas chromatography/mass spectrometry (GC/MS) Multi-residue method Personal care product ingredients (PCPIs) Emergent contaminants SIM Full-scan Wastewaters River waters abstract In this study we developed a GC–MS method for the analysis of priority pollutants, personal care prod- ucts (PCPs) and other emerging contaminants in waters using large volume injection with backflushing. Analyses are performed in the SIM/scan mode, so that in addition to the targeted organic contaminants, this method allows the simultaneous screening of non-target compounds. The scan data are analysed using Deconvolution Reporting Software (DRS) which screens the results for 934 organic contaminants. Deconvolution helps identify contaminants that are buried in the chromatogram by co-extracted materi- als and significantly reduces chromatographic resolution requirements, allowing shorter analysis times. All compounds have locked retention times and we can continually update and extend the mass spectral library including new compounds. Linearity and limits of detection in SIM and full-scan mode were stud- ied. Method detection limits (MDLs) in effluent wastewater ranged in most of the cases from 1 to 36 ng/L in SIM mode and from 4 to 66ng/L in full-scan mode; while in river water from 0.4 to 14 and 2–29ng/L in SIM and full-scan mode, respectively. We obtained a linearity of the calibration curves over two orders of magnitude. The method has been applied to the screening of a large number of organic contaminants – not only to a subset of targets – in urban wastewaters from different wastewater treatment plants and also in river waters. Most of the target compounds were detected at concentration levels ranging from 11 to 8697ng/L and from 7 to 1861ng/L in effluent wastewater and river waters, respectively. Additionally, a group of 12 new compounds were automatically identified using the AMDIS and NIST libraries. Other compounds, such as the 4-amino musk xylene, a synthetic fragrance metabolite, which was not included in the databases, but has been manually searched in the full-scan chromatograms. © 2009 Elsevier B.V. All rights reserved. 1. Introduction Water pollution is perhaps the most prominent environmen- tal concern for European citizens, and therefore a priority for environmental authorities [1]. Although anti-pollution measures taken over the past half-century have dramatically reduced the presence of many known contaminants in water, the number of potentially hazardous chemicals that can reach the environment is very large and new substances are constantly being developed and released. The focus for water pollution research has recently been extended from the conventional “priority” pollutants to the so-called “emerging contaminants” or “new environmental con- taminants”: many of which have been unknown until recently. Of these, personal care product ingredients (PCPIs) represent a group of increasing interest [2–5] since the endocrine-disrupting ∗ Corresponding author at: Pesticide Residue Research Group, University of Almería, 04120 Almería, Spain. E-mail address: mjramos@ual.es (M.J. Gómez). effects of certain compounds have been emphasized [2–6] in addition, most of these compounds are very lipophilic and tend to accumulate in the environment [7,8]. This group of emerging contaminants constitutes a broad class of chemicals widely used in daily life, such as synthetic fragrances, U.V-filters, antiseptics, antioxidants, insect repellents, etc. The large amount of PCPIs, and other emerging contaminants consumed in modern society, contribute to a wide range of contamination in the aquatic envi- ronment: introduced through municipal sewage treatment plants (STPs) or, directly via release from the skin during swimming or bathing [5,9]. Because of the potentially dangerous consequences of the pres- ence of these contaminants in the environment, data concerning the concentration, fate and behaviour of these pollutants in the environment is urgently needed. With this purpose in mind, ana- lytical methods for a rapid, sensitive and selective determination of a broad range of compounds in complex environmental matrices are required. Multi-residue analytical methodologies are becom- ing the required tools, as they provide greater knowledge about the contamination of the waters [10–12] and they reduce the overall 0021-9673/$ – see front matter © 2009 Elsevier B.V. All rights reserved. doi:10.1016/j.chroma.2009.02.085