Abstract
An analytical procedure involving solid-phase extraction (SPE) and gas chromatography–mass spectrometry (GC–MS) has been developed for determination of pharmaceutical compounds (aspirin, caffeine, carbamazepine, diclofenac, ketoprofen, naproxen, ibuprofen, clofibrate, clofibric acid, and gemfibrozil) in a variety of aqueous samples (wastewater and surface water). After filtration, samples were extracted and concentrated using C18 or HLB cartridges, depending on the type of compound. Sample storage conditions were checked and optimized to ensure preservation of the pharmaceutical substance, taking into consideration environmental sampling conditions. For most of the pharmaceuticals monitored, recovery was in the range 53 to 99% and the variability was below 15% for the complete procedure, with limits of detection ranging from 0.4 to 2.5 ng L−1, depending on the compound. The methods were successfully applied to monitoring of pharmaceutical contamination of the Seine estuary. Concentrations varied from several dozens of nanograms per liter for surface waters to several hundreds of nanograms per liter for wastewaters.
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References
Halling-Sorensen B, Nielsen SN, Lanzky PF, Ingerslev F, Holten Lützhoft HC, Jorgensen SE (1998) Chemosphere 36:357–393
Sacher F, Lange FT, Brauch H-J, Blankenhorn I (2001) J Chromatogr A 938:199–210
Ternes TA, Hirsch R, Mueller J, Haberer K (1998) Fresenius J Anal Chem 362:329–340
Zuccato E, Castiglioni S, Fanelli R (2005) J Hard Mater 122:205–209
Koutsouba V, Heberer T, Fuhrmann B, Schmidt-Baumler K, Tsipi D, Hiskia A (2003) Chemosphere 51:69–75
Castiglioni S, Fanelli R, Calamari D, Bagnati R, Zuccato E (2004) Regul Toxicol Pharm 39:25–32
Farré M, Ferrer I, Ginebreda A, Figueras M, Olivella L, Tirapu L, Vilanova M, Damia B (2001) J Chromatogr A 938:187–197
Buser HR, Poiger T, Müller MD (1998) Environ Sci Technol 32:3449–3456
Golet EM, Alder AC, Giger W (2002) Environ Sci Technol 36:3645–3651
Tauxe-Wuersch A, De Alencastro LF, Grandjean D, Tarradellas J (2005) Water Res 39:1761–1772
Andreozzi R, Raffaele M, Nicklas P (2003) Chemosphere 50:1319–1330
Kolpin DW, Furlong ET, Meyer MT, Thurman EM, Zaugg SD, Barber LB, Buxton HT (2002) Environ Sci Technol 36:1202–1211
Kumazawa L, Sato T, Suzuki O (1997) J Chromatogr Sci 35:302–308
Sun Y, Takaba K, Kido H, Nakashima MN, Nakashima K (2003) J Pharm Biomed 30:1611–1619
Theodoridis G, Koster H, de Jong (2000) J Chromatogr B 745:49–82
Santos JL, Aparicio I, Alonso E, Callejon M (2005) Anal Chim Acta 550:116–122
Ulrich S (2000) J Chromatogr A 902:167–194
Fagerquist CK, Lightfield AR (2003) Rapid Commun Mass Spectrom 17:660–671
Löffler D, Ternes TA (2003) J Chromatogr A 1021:133–144
Hilton MJ, Thomas KV (2003) J Chromatogr A 1015:129–141
Ternes TA, Stüber J, Haerrmann N, McDowell D, Ried A, Kampmann M, Teiser B (2003) Water Res 37:1976–1982
Metcalfe CD, Miao XS, Koenig BG, Struger J (2003) Environ Toxicol Chem 22:2881–2889
Moeder M, Schrader S, Winkler M, Popp P (2000) J Chromatogr A 873:95–106
Deng A, Himmelsbach M, Zhu QZ, Frey S, Sengl M, Buchberger W, Niessner R, Knopp D (2003) Environ Sci Technol 37:3422–3429
El Haj BM, Al Ainri AM, Hassan MH, Bin Khadem RK, Marzouq MS (1999) Forensic Sci Int 105:141–153
Budzinski H, Devier MH, Labadie P, Togola A (2006) Anal Bioanal Chem 386:1429–1439
Ternes TA (1998) Water Res 32:3245–3260
Ternes TA, Meisenheimer M, McDowell D, Sacher F, Brauch HJ, Haist-Gulde B, Preuss G, Wilme U, Zulei-Seibert N (2002) Environ Sci Technol 36:3855–3863
Ternes TA, Hirsch R (2000) Environ Sci Technol 34:2741–2748
Tixier C, Singer HP, Ollers S, Muller SR (2003) Environ Sci Technol 37(6):1061–1068
Ternes TA (2001) Trends Anal Chem 20:419–434
Desbrow C, Routledge E, Brighty G, Sumpter JP, Waldock MJ (1998) Environ Sci Technol 32:1549–1558
Verenitch SS, Lowe CJ, Mazumder A (2006) J Chromatogr A 1116:193–203
Lam MW, Young CJ, Brain RA, Johnson DJ, Hanson MA, Wilson CJ, Richards SM, Solomon KR, Mabury SA (2004) Environ Toxicol Chem 23:1431–1440
Joss A, Keller E, Alder AC, Gobel A, McArdell CS, Ternes T, Siegrist H (2005) Water Res 39:3139–3152
Buser HR, Müller M, Theobald N (1998) Environ Sci Technol 32:188–192
Metcalfe CD, Koenig BG, Bennie DT, Servos M, Ternes TA, Hirsch R (2003) Environ Toxicol Chem 22:2872–2880
Acknowledgment
The authors wish to thank the “Région Aquitaine”, the Seine Aval and the “GIS ECOBAG” programs for research funding. They want also to acknowledge the ORQUE (Environmental Quality Research Observatory) program and the NFS (National Funding for Science) for providing the PhD grant of A. Togola.
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Togola, A., Budzinski, H. Analytical development for analysis of pharmaceuticals in water samples by SPE and GC–MS. Anal Bioanal Chem 388, 627–635 (2007). https://doi.org/10.1007/s00216-007-1251-x
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DOI: https://doi.org/10.1007/s00216-007-1251-x