Abstract: A gas chromatography-mass spectrometry (GC-MS) method was established for the determination of the residual amounts of five methylphenols in leather and textiles. The samples were ultrasonically extracted with methanol, and after standing and filtration, the extract liquors were separated by a capillary chromatographic column and qualitatively and quantitatively analyzed in selected ion monitoring mode. The experimental results indicate that a good linear relationship exists within the mass concentration range of 0.05–10.0 mg/kg, with correlation coefficients all exceeding 0.9997, and the limit of quantification was 0.1 mg/kg. The average recovery rates of the target compounds at three addition levels were 90.01%–106.18% (n=8) and the relative standard deviations were 2.09%–5.17%, indicating good precision. The test results were accurate and reliable, which could meet the needs of import and export testing and effectively protect human health and environmental safety.