Acta Pharmaceutica, Vol. 68 No. 3, 2018.
Izvorni znanstveni članak
https://doi.org/10.2478/acph-2018-0024
Analysis of diclofenac in water samples using in situ derivatization-vortex-assisted liquid-liquid microextraction with gas chromatography-mass spectrometry
SENAR AYDIN
; Necmettin Erbakan University, Environmental Engineering Department, Konya, Turkey
MEHMET EMIN AYDIN
; Necmettin Erbakan University, Environmental Engineering Department, Konya, Turkey
FATMA BEDUK
; Necmettin Erbakan University, Environmental Engineering Department, Konya, Turkey
ARZU TEKINAY
; Necmettin Erbakan University, Environmental Engineering Department, Konya, Turkey
HAVVA KILIC
; Necmettin Erbakan University, Environmental Engineering Department, Konya, Turkey
Sažetak
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.
Ključne riječi
diclofenac; GC-MS; in situ derivatization; vortex-assisted liquid-liquid micro-extraction; water
Hrčak ID:
195716
URI
Datum izdavanja:
30.9.2018.
Posjeta: 1.108 *