Application of dynarnic liquid-phase microextraction and injection port derivatization combined with gas chromatography-mass spectrometry to the determination of acidic pharmaceutically active compounds in water samples

A method has been established for the determination of four pharmaceutically active compounds (ibuprofen, ketoprofen, naproxen and clofibric acid) in water samples using dynamic hollow fiber liquid microextraction (HF/LPME) followed by gas chromatography (GC) injection port derivatization and CC-mass spectrometric (MS) determination. Dynamic HF/LPME is a novel approach to microextiaction that involves the use of a programmable syringe pump to move the liquid phases participating in the extraction so as to facilitate the process Trimethylanilinium hydroxide (TMAH) Was Used as derivatization reagent for the analytes to increase their volatility and Improve chromatographic separation Parameters that affect extraction efficiency (selection of organic solvent, volume of organic solvent, agitation in the donor phase, plunger movement and extraction wine) were investigated Under optimal conditions, the proposed method provided good enrichment factors Up to 251, reproducibility hanging from 3 26% to 10 61%. and good linearity from 0 2 to 50 g mu/L. The limits of detection ranged between 0 01 and 0 05 mu g/L (S/N= 3) using selective loll monitoring This method was applied to the determination of the four pharmaceutically active compounds in tap water and wastewater collected from a drain in the vicinity of a hospital (C) 2009 Elsevier B.V. All rights reserved