气质联用法同时测定鞋用材料中DMFo、DMAc和NMP三种残留溶剂的研究

Research on Simultaneous Determination of Residual DMFo,DMAc and NMP in Footwear Materials by GC-MS

N,N-二甲基甲酰胺(DMFo)、N,N-二甲基乙酰胺(DMAc)和N-甲基吡咯烷酮(NMP)是一类优良的溶剂,由于其潜在的生殖毒性,已被REACH列入高度关注物质。利用气质联用仪建立了同时测定鞋用材料(皮革、人造革/合成革、纺织材料)中DMFo、DMAc和NMP三种溶剂残留量的检测方法。以甲醇为提取试剂,在60℃下进行超声提取,GC/MS测定,外标法定量。以皮革、合成革、纺织材料为基质进行3个添加水平的6次平行试验,结果表明:添加浓度为(2.5~200)mg/kg时,样品中DMFo、DMAc和NMP的回收率在81.7%~100.2%之间,相对标准偏差(RSD,n=6)在0.6%~6.9%之间,方法检出限在(1.4~2.1)mg/kg之间,满足分析要求。该方法适用于鞋用材料中DMFo、DMAc和NMP残留量的日常检测,对相关检测标准的制定也具有一定的指导意义。

N,N-dimethyl formamide（DMFo）, N,N-dimethylacetamide（DMAc） and N-Methyl pyrrolidone（NMP） are excellent solvents. Due to their potential reproductive toxicity, DMFo,DMAc and NMP have been taken as substances of very high concern by REACH. A method for simultaneous determination of DMFo, DMAc and NMP in footwear materials（eg. leather, synthetic leather or artificial leather and textile）by gas chromatography mass spectrography（GC-MS） was established. Samples were extracted with methanol under ultrasonic, then analyzed by GC-MS and quantified by external standard method. The average recoveries of DMFo, DMAc and NMP（2.55 -200 mg/kg） in leather, synthetic leather or artificial leather and textile at three levels with six times parallel test were ranged from 81.7% to 100.2% with 0.6% to 6.9% of relative standard deviations（n=6）. The limit of detection of this method was（1.4- 2.0） mg/kg. The method is suitable for routine analysis of residual organic solvents in footwear materials, and it also has certain guiding significance to the development of relevant testing standards.