In order to investigate plant physiological process of leaf senescence and aging, Fourier transform infrared (FTIR) spectroscopy was used to study the young, mature, and old yellow leaves from seven species of evergreen trees. The spectra of the leaves from different growing period are different in the region of 1 800～700 cm-1. The absorption ratios A1 070/A2 927, A1 070/A1 160 were used to evaluate the relative changes of polysaccharides, and A1 318/A2 922 was used to estimate the change of calcium oxalate during leaf senescence. Decomposition and curve-fitting analysis was performed in the region of 1 800～1 500 cm-1. The sub-band absorption ratio H1 650/H1 740 was used to evaluate the relative changes of protein in the leaves. The results show that the accumulation and mobilization of polysaccharides, protein, and calcium oxalate during leaf growing period were different in different plant species. This study demonstrates the potential of mid-infrared spectroscopy for investigation of plants senescence, as well as physiological and biochemical changes of plants.