[Objective] This study focused on the optimization of the sample pretreatment process for the determination of iodine content in food by gas chromatography stipulated in“GB 5009.267—2020 Food Safety National Standard Determination of Iodine in Food”,aiming to reduce the detection cost,shorten the detection time,and improve the detection efficiency and accuracy. [Method] Replace the separatory funnel with a centrifuge tube to reduce the sample weighing,increase the number of vortexing and centrifugation,and optimize the amount of butanone added to explore the optimal detection method. [Result] The optimized gas chromatography method demonstrated excellent performance in terms of recovery rate,precision,repeatability and detection limit when compared with the gas chromatography method specified in the national standard. [Conclusion] By overcoming the cumbersome problem of pretreatment,the optimized gas chromatography method was possible to accurately and quickly determine the iodine content in milk,and it was suitable for the large-scale detection of iodine content in milk.