Abstract
A liquid chromatography-mass spectrometry method for the simultaneous determination of nine sulphonamides (sulphadiazine, sulphathiazole, sulphapyridine, sulphamerazine, sulphamethizole, sulphasoxazole, sulphamethoxypyridazine, sulphamethoxazole and sulphadimethoxine) in honey samples was developed. Sample pretreatment included acidic hydrolysis, followed by solid-phase extraction on a Sep-Pack® C18. Separation is carried out in a C18 column and mobile phases consisting of acetic acid/methanol mixtures. Detection is performed by mass spectrometry with ion trap, using electrospray interface in the positive ionization mode. Method validation has been performed according to European Commission Decision 2002/657/EC criteria, in terms of linearity, trueness, precision, specificity, decision limit (CCα) and detection capability (CCβ). Linearity was obtained with an average coefficient of determination (R2) higher than 0.9995 in matrix. Typical recoveries in fortified honey samples ranged between 89 and 118 % at all levels tested (5, 10, 50 and 100 μg/kg). The method demonstrated good intra- and interbatch precision and accuracy. No interferences with the peaks of interest were observed throughout the chromatographic run. The method has been successfully applied to the analysis of raw honey samples. Forty-five (21 %) of 215 analysed were positive (range 6.7–140.8 μg/kg) for sulphonamides.
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