Magnetic Solid-Phase Extraction Based on Magnetite-Multiwalled Carbon Nanotubes of Non-Steroidal Anti-Inflammatories from Water Followed by LC-ESI-MS/MS.

An analytical method based on liquid chromatography-electrospray ionization-tandem mass spectrometry detection (LC-ESI-MS/MS) has been developed for the determination of pharmaceutical compounds in water samples. Five non-steroidal anti-inflammatory drugs (NSAIDs) namely Naproxen, Ketoprofen, Piroxicam, Diflunisal and Celecoxib were investigated. Magnetic solid phase extraction (MSPE) was used for sample pre concentration of water samples and magnetic carbon nanotubes (Fe3O4-MWCNTs) were considered as solid phase extraction sorbent. Important parameters influencing the extraction efficiency such as nature and volume of eluent, sample pH and adsorbent mass were optimized. The developed MSPE method involved 75 mg of Fe3O4-MWCNTs sorbent, 5 mL of water sample at pH = 4 and 5 mL of 10% ammonia in methanol in the elution step. Under the optimized extraction conditions, linearity, detection and quantification limits and reproducibility were evaluated. The proposed method was successfully applied to the analysis of NSAIDs in surface waters, and mean recoveries of all the NSAIDs were above 90% with relative standard deviations < 17%. The detection and quantification limits were comprised between 0.05-3.6 ng.mL-1 and 0.2-11.9 ng.mL-1, respectively.