Journal
FOOD CHEMISTRY
Volume 145, Issue -, Pages 161-167Publisher
ELSEVIER SCI LTD
DOI: 10.1016/j.foodchem.2013.08.002
Keywords
Nitroimidazoles; Milk; SPE; Protein precipitation; Capillary electrophoresis
Funding
- Junta de Andalucia (Proyecto de Excelencia) [P08-AGR-4268]
- Plan Propio of the University of Granada
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A new sample treatment has been developed for the extraction of 5-nitroimidazole (5-NDZ) drugs in milk samples previous to their determination by micellar electrokinetic chromatography (MEKC). Fat removing and protein precipitation were simultaneously carried out by the addition of trichloroacetic acid (TCA) and subsequent centrifugation. Clean-up and off-line concentration were achieved by a novel solid-phase extraction (SPE) method employing mixed cation exchange (MCX) cartridges, obtaining an off-line concentration factor of 18. Analyses were performed in less than 18 min employing 20 mM phosphate buffer (pH 6.5) and 150 mM SDS as background electrolyte (BGE). During the separation procedure a temperature of 20 degrees C and a voltage of 25 kV (normal mode) were applied. Due to sweeping effects, an on-line concentration was achieved for all the studied compounds and detection limits lower than 1.8 mu g L-1 were obtained. This method has been successfully applied to milk samples of different origins, including raw ewe milk. (C) 2013 Elsevier Ltd. All rights reserved.
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