Abstract: At present, the experimental teaching of instrumental analysis is plagued by several issues, such as being largely limited to single confirmatory experiments, relatively independent content, and a lack of integration with scientific research hotspots. Aiming at the above problems, a comprehensive instrumental analysis experiment for undergraduate students was designed. This experiment covers the synthesis and characterization of materials, as well as the investigation of adsorption and detection methods of phosphopeptides. Firstly, a multifunctionalized magnetic material was prepared. The physicochemical properties of the magnetic material were characterized by means of Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), thermogravimetric analysis (TGA), and other instrumental techniques. Subsequently, the magnetic material was used as the carrier of the magnetic solid phase extraction (MSPE) platform to enrich phosphopeptides. Combined with matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS), the detection of low-abundance phosphopeptides in defatted milk samples was achieved. This experiment effectively integrates scientific research hotspots into basic undergraduate teaching. Through the combined application of multiple instruments and interdisciplinary integration, students’ comprehensive experimental skills and ability to solve complex practical problems have been significantly enhanced.

Key words: comprehensive experiment, instrumental analysis, mass spectrometry, magnetic solid phase extraction (MSPE), phosphopepties