Abstract
A new and sensitive method based on high performance liquid chromatography with laser-induced fluorescence detection has been developed for the determination of decoquinate in milk. Laser source was obtained with a He–Cd laser using a continuous excitation wavelength at 325 nm. Decoquinate exhibits moderate fluorescence, but it is increased using Ca(NO3)2 in the mobile phase. The chromatographic separation was performed on a Luna C18 5-mm reversed phase column, which solves the broadening of peaks and peak tailing compared with other columns tested. The mobile phase, delivered at 1 ml min−1, consisted of methanol–calcium nitrate (0.025 M)–acetonitrile (83/13/4 v/v/v). Decoquinate was successfully cleaned up from milk by solid-phase extraction using C18 cartridges. The method was found to be linear between 0.16 and 16.33 ng ml−1. The results of recovery studies were found to be satisfactory; an average recovery rate of 88.7% was obtained. The LOQ of decoquinate in milk was 0.16 ng ml−1. The intraday relative standard deviation (RSD) was 4%, and interday assay gave an RSD of 4.4%.
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Acknowledgements
Xesús Feás would also like to thank the Spanish Ministerio de Ciencia e Innovación (José Castillejo program for young researchers, Grant no: JC2008-00118). We thank Iberil (Lisboa, Portugal) for providing us decoquinate. Thanks are given to A Casa das Linguas (Lugo, Galicia) for their linguistic support.
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Feás, X., Vázquez, B.I., Iglesias, A. et al. Sensitive Determination of Decoquinate in Milk by High-Performance Liquid Chromatographic Coupled to Laser-Induced Fluorescence Detection. Food Anal. Methods 3, 138–143 (2010). https://doi.org/10.1007/s12161-009-9100-5
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DOI: https://doi.org/10.1007/s12161-009-9100-5