A simple and effective method has been proposed in this work for combination of immunoaffinity extraction with MALDI MS. In this method, an antibody is attached to the surface of a MALDI probe tip via a thin nitrocellulose film, This allows the corresponding antigen to be selectively captured and concentrated on the probe tip from complex plasma solution for MALDI MS analysis, The whole procedure can be completed within 1 h, This combination offers several excellent performance features in the analysis of SNX-111, a therapeutic peptide, It combines the high specificity of affinity chromatography with the high sensitivity of mass spectrometry in a rapid analysis, Direct mass detection provides unambiguous determination by the observation of signals at characteristic m/z values. This method has been used successfully to determine the therapeutic peptide at relevant doses.