Determination of sulfonamides in milk after precolumn derivatisation by micellar liquid chromatography |
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Authors: | Raviolo Mónica Ana Rambla-Alegre Maria Clausell-Tormos Jenifer Capella-Peiró Maria-Elisa Carda-Broch Samuel Esteve-Romero Josep |
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Affiliation: | a Àrea de Química Analítica, Q.F.A., Universitat Jaume I, Campus Riu Sec, 12080 Castelló, Spain b Dpto. de Farmacia, Fac. de Ciencias Químicas, Universidad Nacional de Córdoba, Córdoba, Argentina c Institut de Science et d’Ingénierie Supramoléculaires (ISIS), Université Louis Pasteur, Strasbourg, France |
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Abstract: | A simple method to identify and determine six sulfonamides (sodium sulfacetamide, sulfamethizole, sulfaguanidine, sulfamerazine, sulfathiazole and sulfamethoxazole) in milk by micellar liquid chromatography (MLC) is reported. The assay makes use of a precolumn diazotisation-coupling derivatisation including the formation of an azo dye that can be detected at 490 nm. Furthermore, the use of MLC as an analytical tool allows the direct injection of non-purified samples. The separation was performed with an 80 mM SDS-8.5% propanol eluent at pH 7. Analysis times are below 16 min with a complete resolution. Linearities (r > 0.9999), as well as intra- and inter-day precision (below 2.7%), were studied in the validation of the method. The limits of detection and quantification ranged from approximately 0.72 to 0.94 and 2.4 to 3.1 ng mL−1, respectively. The detection limit was below the maximum residue limit established by the European Community. Finally, recoveries in spiked milk samples were in the 83-103% range. |
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Keywords: | Sulfonamides Azo dye precolumn derivatisation Micellar liquid chromatography Milk |
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