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 ÁL of chloroform, 25 ÁL 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