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    气相色谱-质谱法测定水性涂料中3种酰胺类化合物

    Determination of Three Kinds of Amides in Water Paint by Gas Chromatography-Mass Spectrometry

    • 摘要: 采用气相色谱-质谱法测定水性涂料中N,N-二甲基甲酰胺、N,N-二甲基乙酰胺和N-甲基乙酰胺的含量。1.000 0 g样品用10 mL二氯甲烷在40℃超声萃取40 min,萃取液经0.45 μm微孔滤膜过滤后,在HP-INNOWAX毛细管色谱柱(30 m×0.25 mm,0.25 μm)上分离,质谱分析中采用电子轰击离子源和选择离子监测模式。3种酰胺类化合物的质量浓度均在0.5~5.0 mg·L-1内与其峰面积呈线性关系,检出限(3S/N)在1.57~2.38 mg·kg-1之间。加标回收率为81.3%~104%,测定值的相对标准偏差(n=5)小于3.0%。

       

      Abstract: A method of gas chromatography-mass spectrometry was applied to determination of N,N-dimethylformamide, N,N-dimethylacetamide, and N-methylacetamide in water paint. The sample (1.000 0 g) was ultrasonically extracted with 10 mL of dichloromethane at 40℃ for 40 min. After being filtrated with 0.45 μm organic filter, the extracte was separated on a HP-INNOWAX (30 m×0.25 mm, 0.25 μm) capillary chromatographic column, and determined by mass spectrometry under electron impact ion source and selected ion monitoring mode. Linear relationships were found between values of peak area and mass concentration of the three kinds of amides in the same range of 0.5-5.0 mg·L-1, with detection limits (3S/N) in the range of 1.57-2.38 mg·kg-1. Test for recovery was made by standard addition method and the values of recovery found were in the range of 81.3%-104%, with RSDs (n=5) less than 3.0%.

       

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