A method for simultaneous determination of residual N,N-dimethyl formamide (DMFo), N,N-dimethylacetamide (DMAc) and N-Methyl pyrrolidone (NMP) in leather by gas chromatography mass spectrography (GC-MS) is established. Residual solvents DMFo, DMAc and NMP are ultrasonically extracted at 60oC for 60 min, using methanol as the extraction solvent, followed by the analysis of GC-MS. The concentration of each residual solvent is calibrated by external standard method. The source of uncertainty in the whole process of the measurement is analyzed. Each component of uncertainty is estimated and composed. The combined and expanded uncertainties are given. The validity of this method is evaluated with the uncertainty estimation.%利用气质联用仪建立了同时测定皮革中DMFo、DMAc和NMP三种溶剂残留量的检测方法，以甲醇为溶剂，60℃超声提取60 min，GC-MS测定，外标法定量。对检测过程中不确定度的来源进行了分析，并对不确定度各个分量进行评定、合成，给出了该方法测量结果的合成不确定度和扩展不确定度，通过不确定度评定保证了检测方法的有效性。
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