NDLI: Solid-phase extraction followed by liquid chromatography–time-of-flight–mass spectrometry to evaluate pharmaceuticals in effluents. A pilot monitoring study

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Solid-phase extraction followed by liquid chromatography–time-of-flight–mass spectrometry to evaluate pharmaceuticals in effluents. A pilot monitoring study

Content Provider	Royal Society of Chemistry (RSC)
Author	Fernández-Alba, Amadeo R. Gómez, María José Ferrer, Imma Agüera, Ana Malato, Octavio
Copyright Year	2007
Abstract	The present work provides a multi-residue analytical method for determining a selection of 20 pharmaceuticals from diverse therapeutical classes in hospital effluent wastewater. The method is based on the simultaneous extraction of the target compounds by solid phase extraction (SPE), followed by liquid chromatography–time-of-flight–mass spectrometry (LC–TOF–MS) analysis. Using TOF–MS, accurate mass measurements within 2 ppm error were obtained for most of the pharmaceuticals studied. Empirical formula information can be obtained by this method, allowing the unequivocal identification of the target compounds in the samples. Validation studies showed that LC–TOF–MS analysis is a valuable new tool for identification and quantification of pharmaceuticals in wastewater. Recoveries, using Oasis HLB cartridges at pH 7, were higher than 75% for all pharmaceuticals, except for ranitidine, 4-methylaminoantipyrine (4-MAA), cefotaxime and omeprazole, which needed specific pH conditions for their extraction. Linearity of response over two orders of magnitude was demonstrated (r > 0.99). Matrix effects resulting in suppression of the response were observed. For most of the compounds ion suppression was less than 39%, except for metronidazole, carbamazepine 10,11-epoxide, naproxen and erythromycin, where the signal suppression was 42%, 59%, 46% and 95%, respectively. A simple and effective approach to minimize or avoid matrix interferences was the 1 : 4 dilution of the SPE extracts. Method detection limits (MDLs) and quantification limits (MQLs) ranged between 4–115 ng l−1 and 14–384 ng l−1, respectively. The precision of the method, calculated as relative standard deviation (RSD), ranged from 1.1–19.8% and 1.7–21.7% for intra- and inter-day, respectively. The developed analytical method was applied to the analysis of hospital effluent wastewater during a survey study. 18 of the 20 pharmaceuticals studied were detected at concentration levels of μg l−1, reaching in some cases concentrations over 100 μg l−1, and in the case of the analgesic and antipyretic dipyrone metabolite, higher than 1000 μg l−1.
Starting Page	718
Ending Page	729
Page Count	12
File Format	HTM / HTML PDF
ISSN	14640325
Volume Number	9
Issue Number	7
Journal	Journal of Environmental Monitoring
DOI	10.1039/b702844j
Language	English
Publisher	Royal Society of Chemistry
Access Restriction	Subscribed
Subject Keyword	Oasis HLB Wastewater Solid phase extraction Empirical formula Oasis PH Ranitidine Cefotaxime Omeprazole Ion Metronidazole Carbamazepine Epoxide Naproxen Erythromycin Positive-definite matrix Coefficient of variation Analgesic Antipyretic Metamizole Metabolite
Content Type	Text
Resource Type	Article
Subject	Public Health, Environmental and Occupational Health Management, Monitoring, Policy and Law

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