Simultaneous determination of 16 sulfonamides in honey by liquid chromatography/tandem mass spectrometry.

JOURNAL OF AOAC INTERNATIONAL(2005)

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摘要
A method is described for the determination of 16 sulfonamides in honey. Samples are dissolved in phosphoric acid solution (pH2), cleaned up with 2 solid-phase extraction (SPE) cartridges, an aromatic sulfonic cation-exchange cartridge and an Oasis HLB SPE cartridge, and analyzed both qualitatively and quantitatively by liquid chromatography/tandem mass spectrometry (LC/MS/MS) under the selected conditions. Without exception, calibration curves were linear (r = > 0.995), when sulfamethizole was between 1.0 and 25.0 mu g/kg; sulfacetamide, sulfapyridine, sulfadiazine, sulfachloropyridazine, sulfamethoxazole, sulfamerazine, sulfisoxazole, sulfamonomethoxine, and sulfadoxine were between 2.0 and 50.0 mu g/kg; sulfamethoxypyridazine, sulfadimethoxine, and sulfathiazole were between 4.0 and 100.0 mu g/kg; sulfamethazine and sulfameter were between 8.0 and 200.0 mu g/kg; and sulfaphenazole was between 12.0 and 300.0 mu g/kg. Average recoveries at 4 fortification levels in the range of 1.0-300 mu g/kg in honey were 70.9-102.5%, and relative standard deviations were 2.02-11.52%. The limits of quantitation for the 16 sulfonamides were between 1.0 and 12.0 mu g/kg, with the LC/MS/MS method.
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