Acta Pharm. 68 (2018) 313-324

full paper

Original research paper

Analysis of diclofenac in water samples using in situ derivatization-vortex-assisted liquid-liquid microextraction with gas chromatography-mass spectrometry

SENAR AYDIN, MEHMET EMIN AYDIN, FATMA BEDUK, ARZU TEKINAY and HAVVA KILIC

sozcan@konya.edu.tr

Necmettin Erbakan University, Environmental Engineering Department, Konya, Turkey

Accepted March 9, 2018

Published online March 19, 2018

A novel micro-extraction technique for a rapid and sensitive analysis of diclofenac (DCF) in water samples has been developed. DCF was derivatized and extracted simultaneously using vortex-assisted liquid-liquid micro-extraction (VALLME) prior to gas chromatography with mass spectrometry detection. The effects of extraction solvent volume, extraction and derivatization time and ionic strength of the sample were studied using 2³ factorial experimental design. The optimum extraction conditions were as follows: 200 µL of chloroform, 25 µL of N-methyl-N-trimethylsilyl-trifluoroacetamide (MSTFA) derivatization reagent, vortex extraction and derivatization time 5 min at 3000 rpm. The extraction recovery for different fortification levels was 98 %. Also, the proposed micro-extraction method exhibited results comparable with the solid phase extraction of real water samples. The proposed one-step VALLME and derivatization method is simpler and faster than the conventional extraction and derivatization methods used for the determination of DCF in real water samples.

Keywords: diclofenac, GC-MS, in situ derivatization, vortex-assisted liquid-liquid micro-extraction, water