The invention discloses a detection method for high-precision detection of volatile organic compounds, which comprises the following steps of preparing a cerium-doped mesoporous molecular sieve, sequentially carrying out aminopropyl modification, perylene-3, 4, 9, 10-tetracarboxylic dianhydride grafting and octadecyl mercaptan modification on the cerium-doped mesoporous molecular sieve, and packaging to obtain a volatile organic compound detection film, and establishing a standard curve between the concentration of the volatile organic compounds and the fluorescence intensity of the detectionfilm by utilizing the fluorescence intensity difference of the detection film to the volatile organic compounds with different concentrations, so that the high-precision detection of the volatile organic compounds is realized. In the way, the rich pore structure in the molecular sieve can be used to efficiently adsorb and desorb the volatile organic compound, the perylene-3, 4, 9, 10-tetracarboxylic dianhydride is taken as a substrate, quantitative detection of the volatile organic compounds is realized by utilizing the fluorescence effect of the perylene-3, 4, 9, 10-tetracarboxylic dianhydride, and the sensitivity, accuracy and stability of detection are effectively improved by combining the synergistic effect of all groups, so that the application range is relatively wide.