Rapid method for quantification of nine sulfonamides in bovine milk using HPLC/MS/MS and without using SPE

•A confirmatory HPLC–MS/MS method for nine sulfonamides in milk.•Extraction protocol is simple and cheap.•Milk samples could be extracted and analysed within less than 3h.•Limit of detection was below 26μg/kg for all sulfonamides.•Of 100 compliant milk samples analysed two results positive for sulfo...

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Veröffentlicht in:Food chemistry 2013-12, Vol.141 (3), p.2294-2299
Hauptverfasser: Nebot, Carolina, Regal, Patricia, Miranda, Jose Manuel, Fente, Cristina, Cepeda, Alberto
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Sprache:eng
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Zusammenfassung:•A confirmatory HPLC–MS/MS method for nine sulfonamides in milk.•Extraction protocol is simple and cheap.•Milk samples could be extracted and analysed within less than 3h.•Limit of detection was below 26μg/kg for all sulfonamides.•Of 100 compliant milk samples analysed two results positive for sulfonamides. Sulfonamides are antimicrobial agents widely employed in animal production and their residues in food could be an important risk to human health. In the dairy industry, large quantities of milk are monitored daily for the presence of sulfonamides. A simple and low-cost extraction protocol followed by a liquid chromatographic–tandem mass spectrometry method was developed for the simultaneous detection of nine sulfonamides in whole milk. The method was validated at the maximum residue limits established by European legislation. The limits of quantification obtained for most sulfonamides were between 12.5 and 25μgkg−1, detection capabilities ranged from 116 to 145μgkg−1, and recoveries, at 100μgkg−1, were greater than 89±12.5%. The method was employed to analyse 100 raw whole bovine milk samples collected from dairy farms in the northwest region of Spain. All of the samples were found to be compliant, but two were positive; one for sulfadiazine and the other for sulfamethoxipyridazine.
ISSN:0308-8146
1873-7072
DOI:10.1016/j.foodchem.2013.04.099