Microextraction by packed sorbent for the analysis of pharmaceutical residues in environmental water samples by in situ derivatization-programmed temperature vaporizer–gas chromatography–mass spectrometry

The present work describes the development and validation of a method for the determination of five non-steroidal anti-inflammatory drugs (NSAIDs: clofibric acid, ibuprofen, naproxen, diclofenac and ketoprofen) in water samples. The fully automated method includes in situ aqueous derivatization followed by analyte enrichment by microextraction by packed sorbent (MEPS) coupled directly to programmed temperature vaporizer–gas chromatography–mass spectrometry (PTV–GC–MS). The MEPS variables, such as sample volume, elution solvent, elution volume, fill and injection speed and washing steps were optimized. It was possible to use the MEPS polymer (silica-C18) 250 times. Ibuprofen-d3 was used as internal standard.The reproducibility of the method, calculated as the relative standard deviation (RSD), was below 10% for all compounds. Detection limits in ultrapure water were between 3.0 and 110 ng L−1 for ibuprofen and ketoprofen, respectively. External calibration was used in the determination of NSAIDs in several types of water samples, including tap, river, sea and influent and effluent wastewater. The results obtained revealed the presence of ibuprofen and naproxen in the influent wastewater sample and of naproxen in the effluent wastewater sample.

► Development of a method for determination of non-steroidal anti-inflammatory drugs.
► Fully automated method including derivatization and gas chromatography–mass spectrometry.
► Analyte enrichment by microextraction by packed sorbent (MEPS).