<abstract xmlns="http://www.w3.org/1999/xhtml"><p>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 2<sup>3</sup> factorial experimental design. The optimum extraction conditions were as follows: 200 μL of chloroform, 25 μL of <italic>N</italic>-methyl-<italic>N</italic>-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.</p></abstract>

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.

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

Acta Pharmaceutica

This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 3.0 License.

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

A novel micro-extraction technique for a rapid and sensitive analysis of diclofenac (DCF) in water samples has been developed. DCF was derivatized and...

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

Published Online: Jul 04, 2018

Page range: 313 - 324

Accepted: Mar 09, 2018

DOI: https://doi.org/10.2478/acph-2018-0024

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

© 2018 Senar Aydin et al., published by Sciendo

This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 3.0 License.

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

Published Online: Jul 04, 2018

Page range: 313 - 324

Accepted: Mar 09, 2018

DOI: https://doi.org/10.2478/acph-2018-0024

Keywordsdiclofenac, GC-MS, derivatization, vortex-assisted liquid-liquid micro-extraction, water

© 2018 Senar Aydin et al., published by Sciendo

This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 3.0 License.

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