In order to address the difficulty in directly measuring dissolved methyl nitrite due to the lack of standard materials, an indirect quantitative method based on gas chromatography was established.  A GC system equipped with a six-port gas injection valve, liquid sampler, polar column, and hydrogen flame ionization detector were employed by the experimental setup. Under specific chromatographic conditions, the relative retention value of methyl nitrite relative to methanol was measured as 0.45, while that relative to ethanol was 0.38. The relative mass correction factor of methyl nitrite relative to methanol was determined to be 1.19, and that of dissolved methyl nitrite relative to ethanol was 2.45. By measuring the methanol content in the liquid and combining the above parameters, the indirect calculation of dissolved methyl nitrite content was achieved. The method features a simple principle and convenient operation, providing effective guidance for the quantitative analysis of dissolved methyl nitrite in chemical production.