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建立了气相色谱质谱联用法测定合成树脂乳液涂料中挥发性有机化合物含量的方法。合成树脂乳液涂料经甲醇提取、离心，上清液用 HP-5MS 色谱柱分离，质谱检测，内标法定量。优化条件下挥发性有机化合物回收率为85.84％～103.47％，相对标准偏差（RSD）为0.49％～1.86％，检出限为6.5～12.5 mg·L-1。该方法操作简单，准确度和精密度较高，是一种检测合成树脂乳液涂料中挥发性有机化合物含量的有效方法。“,”The determination method for volatile organic compounds in synthetic resin emulsion coats by gas chromatography-mass spectrometry with internal standard quantification was developed.Synthetic resin emul-sion coats were extracted by methanol,separated by HP-5MS column with mass spectrometric detection and in-ternal standard quantification.Under optimal conditions,the volatile organic compounds recovery was 85.84%~103.47%,the relative standard deviation(RSD)was 0.49%~1.86%,the detection limit was 6.5~12.5 mg ·L-1 .The method has features of simple operation,good accuracy and high precision,and can be applied to the determination of volatile organic compounds in synthetic resin emulsion coats.