Validation of a confirmatory method for the determination of residues of four nitrofurans in egg by liquid chromatography–tandem mass spectrometry with the software InterVal Original Research Article

A method for the detection and determination of nitrofuran derivatives in egg by liquid chromatography–tandem mass spectrometry (LC–MS/MS) was validated with the software InterVal and can be applied for the confirmation of nitrofuran metabolites in fresh or lyophilised eggs. The validation study comprises variations in operator, storage condition, breeding, equipment and duration of sample preparation. A comprehensive overview of the robustness of the method is obtained by analysing eight samples at six concentration levels. First results of short- and medium-term investigations for stability of analytes in solution show that standard solutions of nitrofuran metabolites are stable for at least 1 year when stored at +4 °C in the dark. The decision limit CCα expressed for the underivatised metabolite is 0.05 μg kg−1 for 3-amino-5-methyl-morpholino-2-oxazolidinone, 0.03 μg kg−1 for 3-amino-2-oxazolidinone, 0.20 μg kg−1 for semicarbazide and 0.22 μg kg−1 for 1-amino-hydantoin.