气固顶空-气相色谱法测定纺织品中N,N-二甲基甲酰胺与N,N-二甲基乙酰胺

Determination of DMF and DMAC in Textiles by Gas Solid Headspace Combined with GC

摘要: 采用气固顶空-气相色谱法同时测定纺织品中N,N-二甲基甲酰胺(DMF)和N,N-二甲基乙酰胺(DMAC)的残留量。样品经剪碎后,称取0.5 g,在120 ℃顶空温度下加热30 min,顶空气体采用CAM色谱柱分离,以氮磷检测器(NPD)进行检测。以基体匹配校正法消除基质效应,外标法定量。DMF、DMAC的质量在0.2~400 μg范围内与峰面积呈线性关系,检出限均为0.1 μg·g-1。两种物质的加标回收率在88.4%~95.3%之间,相对标准偏差(n=6)在2.4%~3.5%之间。

Abstract: Gas solid headspace combined with gas chromatography was applied for simultaneous determination of residual DMF and DMAC in textiles. After being cut to pieces, 0.5 g of sample was heated at the headspace temperature of 120 ℃ for 30 min. Then the headspace gas was separated with CAM column and detected with NPD. The matrix effect was eliminated by matrix-matching calibration. External standard method was used for quantification. Linear relationship between the peak area and the weight of DMF and DMAC was in the range of 0.2-400 μg, with detection limits (3S/N) of 0.1 μg·g-1. Recovery rates measured by standard addition method were in the range of 88.4%-95.3% with RSD′s (n=6) in the range of 2.4%-3.5%.