 ISSN 0235-7216 ISSN 2424-4538 (online) |
2007 m. Nr. 3 High-performance liquid chromatography–tandem mass
spectrometry for the determination of sulfonamides in eggs
High-performance liquid chromatography–tandem mass spectrometry (HPLC–MS/MS) method was developed for the determination of ten sulfonamides (SAs) in hen eggs. Conditions for reversed-phase HPLC and electrospray ionization MS/MS in the positive ion mode were optimized monitoring two characteristic mass transitions for each analyte. The egg samples were extracted with acetonitrile and defatted with n-hexane. Further solid-phase clean-up on a Strata-X polymeric cartridge was performed to obtain an extract suitable for the HPLC-MS/MS analysis. The calibration curves showed acceptable linearity in the concentration range from 1 to 45 μg/kg with correlation coefficients (r2) above 0.992. Using two labelled internal standards (sulfamethazine-13C6 and sulfamethoxazole-13C6) the mean recoveries of SAs from egg samples spiked at 10 μg/kg were in the range of 91–146%. The applicability of this technique was demonstrated by the analysis of hen eggs available from local poultry farms. Among the 10 samples analyzed, none of them were found positive for the sulfonamides studied. Keywords: high–performance liquid chromatography, tandem mass spectrometry, sulfonamides, eggs |
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