This paper investigates the significance of element speciation analysis, the various hyphenated techniques used in element speciation analysis, and their application in real samples. This involves a variety of separation technologies, such as high-performance liquid chromatography, ion chromatography, size exclusion chromatography, gas chromatography, and capillary electrophoresis, as well as various detection methods, such as inductively coupled plasma mass spectrometry, inductively coupled plasma optical emission spectrometry, atomic fluorescence spectrometry, and atomic absorption spectrometry. Based on this, we developed teaching experiments, combined theory with practice, and further strengthened students' understanding, mastery, and application of knowledge.