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Evaluation of the in-vivo concentration of monoclonal antibody (mAb) mixtures is a challenging task. Here we report the application of an LC-MS bioanalytical method to quantify in monkey serum the Sym004, an equimolar mixture of two monoclonal antibodies, 992 mAb and 1024 mAb. This method has been assessed accordingly to industry standards and it is based on the determination of two specific signature peptides that report the single mAbs concentrations and on another one peptide, common to the two mAbs, that measures the total concentration of the two target proteins.