| Title: | One step solvent bar microextraction and derivatization followed by gas chromatography-mass spectrometry for the determination of pharmaceutically active compounds in drain water samples |
| Address: | "Department of Chemistry, National University of Singapore, 3 Science Drive 3, Singapore 117543, Singapore" |
| DOI: | 10.1016/j.chroma.2012.02.068 |
| ISSN/ISBN: | 1873-3778 (Electronic) 0021-9673 (Linking) |
| Abstract: | "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 0.022 mug/L, linearity (from 0.1-50 to 0.2-50 mug/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" |
| Keywords: | "Chemical Fractionation/*methods Gas Chromatography-Mass Spectrometry/*methods Osmolar Concentration Pharmaceutical Preparations/analysis/*isolation & purification Reproducibility of Results Solvents/chemistry Temperature Water/*analysis Water Pollutants, ;" |
| Notes: | "MedlineGuo, Liang Lee, Hian Kee eng Research Support, Non-U.S. Gov't Validation Study Netherlands 2012/03/23 J Chromatogr A. 2012 Apr 27; 1235:26-33. doi: 10.1016/j.chroma.2012.02.068. Epub 2012 Mar 5" |
