Abstract: NMR is one of the most powerful qualitative analysis tools in the field of pharmacy. However, NMR can also be used for quantitative analysis, so a comprehensive experiment is designed to determine the main composition and relative content of fatty acids in edible oil by quantitative ¹³C-NMR without any pretreatment and high temperature process, with stable method and good reproducibility. By using the reverse gating decoupling carbon spectroscopy test experiment, the characteristic signal peaks of each fatty acid are found, and the composition of fatty acids, especially unsaturated fatty acids is qualitative analyzed. The content of fatty acids determined by the integration of characteristic signal peaks. Students could deeply master the qualitative and quantitative functions of NMR though the comprehensive experiment.