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Rapid ultrasound-assisted emulsification microextraction combined with COU-2 dispersive micro-solid phase extraction for the determination of azole antifungals in milk samples by HPLC-DAD

A rapid, simple, and efficient method using ultrasound-assisted emulsification microextraction combined with dispersive micro-solid phase extraction (USAE-D-µ-SPE) was developed for detection and quantification of three azole antifungals in milk samples by high-performance liquid chromatography diod...

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Main Authors:	Othman, N., Lim, V., Ramachandran, M. R., Sanagi, M. M., Kamaruzaman, S., Hirota, Y., Nishiyama, N., Yahaya, N.
Format:	Article
Published:	Friedr. Vieweg und Sohn Verlags GmbH 2017
Subjects:	QD Chemistry
Online Access:	http://eprints.utm.my/id/eprint/75924/ https://www.scopus.com/inward/record.uri?eid=2-s2.0-85028022917&doi=10.1007%2fs10337-017-3386-z&partnerID=40&md5=76fa0c04e89b2bd7eb59e9fcfb4bfd4c
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spelling	my.utm.759242018-05-30T04:10:57Z http://eprints.utm.my/id/eprint/75924/ Rapid ultrasound-assisted emulsification microextraction combined with COU-2 dispersive micro-solid phase extraction for the determination of azole antifungals in milk samples by HPLC-DAD Othman, N. Lim, V. Ramachandran, M. R. Sanagi, M. M. Kamaruzaman, S. Hirota, Y. Nishiyama, N. Yahaya, N. QD Chemistry A rapid, simple, and efficient method using ultrasound-assisted emulsification microextraction combined with dispersive micro-solid phase extraction (USAE-D-µ-SPE) was developed for detection and quantification of three azole antifungals in milk samples by high-performance liquid chromatography diode array detector. In this study, mesoporous carbon, COU-2, was used as sorbent in USAE-D-µ-SPE for the extraction and preconcentration of analytes. Several important experimental parameters, including type of deproteinized solvents, desorption time, type of extraction solvents, volume of extraction solvent, extraction time, emulsification time, sample pH, salt addition, and mass of COU-2 sorbent, were optimized using spiked milk samples. Under the optimum extraction and detection conditions, three azole antifungals, namely ketoconazole, clotrimazole, and miconazole, were determined within 20 min, with good linearity of matrix-matched calibration in the range of 0.5–5000.0 µg L−1 with coefficient of determination, r2 ≥ 0.9943. The method showed limits of detection and limits of quantification of all analytes in the range of 0.15–3.0 and 0.5–10.0 µg L−1, respectively. Good repeatability with RSDs <15% (n = 3) and satisfactory relative recoveries (83.3–111.1%) were obtained for spiked azole antifungal drugs in milk. The results reveal that the developed USAE-D-µ-SPE method was a simple, rapid, efficient, environmentally friendly, and practicable method for the determination of azole antifungals in milk samples. Friedr. Vieweg und Sohn Verlags GmbH 2017 Article PeerReviewed Othman, N. and Lim, V. and Ramachandran, M. R. and Sanagi, M. M. and Kamaruzaman, S. and Hirota, Y. and Nishiyama, N. and Yahaya, N. (2017) Rapid ultrasound-assisted emulsification microextraction combined with COU-2 dispersive micro-solid phase extraction for the determination of azole antifungals in milk samples by HPLC-DAD. Chromatographia, 80 (10). pp. 1553-1562. ISSN 0009-5893 https://www.scopus.com/inward/record.uri?eid=2-s2.0-85028022917&doi=10.1007%2fs10337-017-3386-z&partnerID=40&md5=76fa0c04e89b2bd7eb59e9fcfb4bfd4c
institution	Universiti Teknologi Malaysia
building	UTM Library
collection	Institutional Repository
continent	Asia
country	Malaysia
content_provider	Universiti Teknologi Malaysia
content_source	UTM Institutional Repository
url_provider	http://eprints.utm.my/
topic	QD Chemistry
spellingShingle	QD Chemistry Othman, N. Lim, V. Ramachandran, M. R. Sanagi, M. M. Kamaruzaman, S. Hirota, Y. Nishiyama, N. Yahaya, N. Rapid ultrasound-assisted emulsification microextraction combined with COU-2 dispersive micro-solid phase extraction for the determination of azole antifungals in milk samples by HPLC-DAD
description	A rapid, simple, and efficient method using ultrasound-assisted emulsification microextraction combined with dispersive micro-solid phase extraction (USAE-D-µ-SPE) was developed for detection and quantification of three azole antifungals in milk samples by high-performance liquid chromatography diode array detector. In this study, mesoporous carbon, COU-2, was used as sorbent in USAE-D-µ-SPE for the extraction and preconcentration of analytes. Several important experimental parameters, including type of deproteinized solvents, desorption time, type of extraction solvents, volume of extraction solvent, extraction time, emulsification time, sample pH, salt addition, and mass of COU-2 sorbent, were optimized using spiked milk samples. Under the optimum extraction and detection conditions, three azole antifungals, namely ketoconazole, clotrimazole, and miconazole, were determined within 20 min, with good linearity of matrix-matched calibration in the range of 0.5–5000.0 µg L−1 with coefficient of determination, r2 ≥ 0.9943. The method showed limits of detection and limits of quantification of all analytes in the range of 0.15–3.0 and 0.5–10.0 µg L−1, respectively. Good repeatability with RSDs <15% (n = 3) and satisfactory relative recoveries (83.3–111.1%) were obtained for spiked azole antifungal drugs in milk. The results reveal that the developed USAE-D-µ-SPE method was a simple, rapid, efficient, environmentally friendly, and practicable method for the determination of azole antifungals in milk samples.
format	Article
author	Othman, N. Lim, V. Ramachandran, M. R. Sanagi, M. M. Kamaruzaman, S. Hirota, Y. Nishiyama, N. Yahaya, N.
author_facet	Othman, N. Lim, V. Ramachandran, M. R. Sanagi, M. M. Kamaruzaman, S. Hirota, Y. Nishiyama, N. Yahaya, N.
author_sort	Othman, N.
title	Rapid ultrasound-assisted emulsification microextraction combined with COU-2 dispersive micro-solid phase extraction for the determination of azole antifungals in milk samples by HPLC-DAD
title_short	Rapid ultrasound-assisted emulsification microextraction combined with COU-2 dispersive micro-solid phase extraction for the determination of azole antifungals in milk samples by HPLC-DAD
title_full	Rapid ultrasound-assisted emulsification microextraction combined with COU-2 dispersive micro-solid phase extraction for the determination of azole antifungals in milk samples by HPLC-DAD
title_fullStr	Rapid ultrasound-assisted emulsification microextraction combined with COU-2 dispersive micro-solid phase extraction for the determination of azole antifungals in milk samples by HPLC-DAD
title_full_unstemmed	Rapid ultrasound-assisted emulsification microextraction combined with COU-2 dispersive micro-solid phase extraction for the determination of azole antifungals in milk samples by HPLC-DAD
title_sort	rapid ultrasound-assisted emulsification microextraction combined with cou-2 dispersive micro-solid phase extraction for the determination of azole antifungals in milk samples by hplc-dad
publisher	Friedr. Vieweg und Sohn Verlags GmbH
publishDate	2017
url	http://eprints.utm.my/id/eprint/75924/ https://www.scopus.com/inward/record.uri?eid=2-s2.0-85028022917&doi=10.1007%2fs10337-017-3386-z&partnerID=40&md5=76fa0c04e89b2bd7eb59e9fcfb4bfd4c
_version_	1643657198281162752
score	13.211869

Rapid ultrasound-assisted emulsification microextraction combined with COU-2 dispersive micro-solid phase extraction for the determination of azole antifungals in milk samples by HPLC-DAD

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