Abstract
A simple, rapid, and environmentally friendly microextraction termed COU-2-D-μ-SPE has been developed for the analysis of three penicillins (i.e., oxacillin, cloxacillin, and dicloxacillin) in milk samples. An ordered mesoporous carbon, COU-2, was synthesized and used as the sorbent in dispersive micro-solid phase for the extraction of selected penicillins prior to high-performance liquid chromatography-ultraviolet detection (HPLC-UV). Several important parameters, namely, pH value, salt addition, desorption solvent, extraction time, desorption time, and amount of COU-2, were investigated and optimized. Under the optimum extraction conditions, the method showed good linearity in the range of 10–5,000 μg L−1 (r 2 ≥ 0.9994), low limits of detection (2.0–3.3 μg L−1), acceptable reproducibility (relative standard deviation (RSD) 6.2–8.8 %, n = 9), and satisfactory relative recoveries (80.3–99.5 %) for studied penicillins in milk. The proposed COU-2-D-μ-SPE method has been successfully applied to six commercial milk samples, and the extraction of blank samples indicated that all samples were free from selected penicillin contamination.
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Acknowledgments
The authors wish to thank Universiti Teknologi Malaysia and the Ministry of Education Malaysia (MOE) for financial supports through research grant no. R.J130000.7809.4F177 and sponsorship for N. Yahaya through Advanced Medical and Dental Institute, Universiti Sains Malaysia Fellowship Program.
Conflict of Interest
Noorfatimah Yahaya declares that she has no conflict of interest. Mohd Marsin Sanagi declares that he has no conflict of interest. Takahito Mitome declares that he has no conflict of interest. Norikazu Nishiyama declares that he has no conflict of interest. Wan Aini Wan Ibrahim declares that she has no conflict of interest. Hadi Nur declares that he has no conflict of interest. This article does not contain any studies with human or animal subjects.
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Yahaya, N., Sanagi, M.M., Mitome, T. et al. Dispersive Micro-Solid Phase Extraction Combined with High-Performance Liquid Chromatography for the Determination of Three Penicillins in Milk Samples. Food Anal. Methods 8, 1079–1087 (2015). https://doi.org/10.1007/s12161-014-9991-7
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DOI: https://doi.org/10.1007/s12161-014-9991-7