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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

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Abstract

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, r 2 ≥ 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.

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Acknowledgements

The authors wish to thank Universiti Sains Malaysia for facilitations and the Ministry of Education Malaysia for their financial supports through research votes (Short Term Grant 304.CIPPT.6313197 and Fundamental Research Grant Scheme- 203.CIPPT.6711484).

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Authors and Affiliations

  1. Integrative Medicine Cluster, Advanced Medical and Dental Institute (AMDI), Universiti Sains Malaysia, Bertam, 13200, Kepala Batas, Penang, Malaysia

    Nurshazliana Othman, Vuanghao Lim, Muggundha Raoov Ramachandran & Noorfatimah Yahaya

  2. Department of Chemistry, Faculty of Science, Universiti Teknologi Malaysia, 81310 UTM, Johor Bahru, Johor, Malaysia

    Mohd Marsin Sanagi

  3. Department of Chemistry, Faculty of Science, Universiti Putra Malaysia, 43400 UPM, Serdang, Selangor Darul Ehsan, Malaysia

    Sazlinda Kamaruzaman

  4. Division of Chemical Engineering, Graduate School of Engineering Science, Osaka University, 1-3 Machikaneyama, Toyonaka, Osaka, 560-8531, Japan

    Yuichiro Hirota & Norikazu Nishiyama

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  1. Nurshazliana Othman
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  2. Vuanghao Lim
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Correspondence to Noorfatimah Yahaya.

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Othman, N., Lim, V., Ramachandran, M.R. et al. 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, 1553–1562 (2017). https://doi.org/10.1007/s10337-017-3386-z

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