Journal
JOURNAL OF CHROMATOGRAPHY A
Volume 1218, Issue 37, Pages 6240-6247Publisher
ELSEVIER
DOI: 10.1016/j.chroma.2011.06.112
Keywords
In situ derivatization; NSAIDs; SALLE
Funding
- DGI [CTQ2010-17514/BQU]
- Consejeria de Educacion y Cultura of the Junta de Castilla y Leon [GR87]
- Xunta de Galicia for the concession [09MDS038103PR]
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A new analytical method for the determination of trace levels of five non-steroidal anti-inflammatory drugs (NSAIDs: clofibric acid, ibuprofen, naproxen, diclofenac and ketoprofen) in water samples is described. The analytical procedure involves in situ aqueous derivatization with N-(3-dimethylaminopropyl)-N'-ethylcarbodiimide hydrochloride (EDC) and 2,2,2-trifluoroethylamine hydrochloride (TFEA) and salting-out liquid-liquid extraction (SALLE), followed by gas chromatography-programmed temperature vaporizer-mass spectrometry (GC-PTV-MS). The influence of several parameters on the efficiency of the derivatization (stirring time, reaction time, reagent concentration and pH), and the extraction (solvent, volume, salts and stirring time) and injection steps (liner, injection volume, liner temperature, injection time, venting time and venting flow) was investigated. The detection limits of the method in water varied from 0.042 mu g/L for ibuprofen to 1.2 mu g/L for ketoprofen. The relative standard deviations (RSD) values were found to be relatively low (<10% for all compounds). The methodology developed was applied to the determination of NSAIDs in several environmental matrices including tap, river, sea and influent and effluent waste water samples. The results obtained show the presence of ibuprofen and naproxen in the influent waste water sample. (C) 2011 Elsevier B.V. All rights reserved.
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