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An analytical method for the quantification and identity confirmation of streptomycin and dihydrostreptomycin residues in pasteurized milk using liquid chromatography (LC)-atmospheric pressure chemical ionization (APCI)-tandem mass spectrometry (MS-MS) was developed and validated. Method validation was performed according to the recommendations of the international agencies European Community and IUPAC, and the following parameters were evaluated: analytical curve, linearity, sensitivity, precision (intra- and inter-day repeatability), accuracy, and the limit of detection (LOD) and limit of quantification (LOQ). Simple sample preparation was followed by the LC-APCI-MS-MS analysis. The method presented adequate linearity with correlation coefficients above 0.99 for both analytes in the dynamic range of 50–400 μg/kg, and average accuracies between 84–110%. The LOD and LOQ were, respectively, 25 μg/kg and 50 μg/kg for both analytes. Method selectivity was verified by the absence of interfering peaks in the retention regions of the analytes and the internal standard when a blank sample was tested. The results qualified the method for the quantification and confirmation of the analytes in milk at concentrations inferior to the established maximum residue limits (200 μg/kg).

Development and Validation of an LC-APCI-MS-MS Analytical Method for the Determination of Streptomycin and Dihydrostreptomycin Residues in Milk