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One step solvent bar microextraction and derivatization followed by gas chromatography–mass spectrometry for the determination of pharmaceutically active compounds in drain water samples

Guo, Liang, Lee, Hian Kee
Journal of chromatography 2012 v.1235 pp. 26-33
agitation, derivatization, detection limit, drainage water, gas chromatography-mass spectrometry, ibuprofen, ionic strength, ketoprofen, liquid-phase microextraction, pH, propranolol, solid phase microextraction, solvents, temperature
For the first time, a simple and novel one-step combined solvent bar microextraction with derivatization with GC–MS analysis, was developed for the determination of pharmaceutically active compounds (PhACs) in water samples. In the procedure, the derivatization reagent was added in the extraction solvent (solvent bar), so that the analytes could be extracted from the aqueous sample and simultaneously derivatized in the solvent bar to enhance their volatility and improve chromatographic performance. After extraction, the derivatized analytes in the extract were directly injected into a GC–MS system for analysis. Six PhACs including naproxen, ibuprofen, ketoprofen, propranolol, diclofenac, and alprenolol were used here to develop and evaluate the method. The parameters affecting the derivatization and extraction efficiency including derivatization time and temperature, the proportion of derivatization reagent, the type of organic solvent, extraction time, extraction temperature, pH of sample solution, effect of ionic strength, and sample agitation speed, were investigated in detail. Under the most favorable conditions, the method provided good limits of detection ranging from 0.006 to 0.022μg/L, linearity (from 0.1–50 to 0.2–50μg/L, depending on analytes) and repeatability of extractions (RSDs below 9.5%, n=5). The proposed method was compared to hollow fiber protected liquid-phase microextraction and solid-phase microextraction, and showed higher extraction efficiency and/or shorter extraction time. The proposed method was applied to the determination of six PhACs in drain water, and was demonstrated to be simple, fast and efficient.