GC-MS测定聚氨酯产品中的N,N-二甲基甲酰胺  

Determination of N,N-Dimethylformamide in Polyurethane Products by Gas Chromatography-Mass Spectrometry

作　　者：胡苹 李大刚[1] 詹迎旭 HU Ping;LI Dagang;Zhan Yingxu(Department of Materials and Chemical Engineering,Liming Vocational University,Quanzhou 362000,China)

机构地区：[1]黎明职业大学材料与化学工程学院,福建泉州362000

出　　处：《皮革科学与工程》2021年第1期47-50,共4页Leather Science and Engineering

基　　金：2019黎明职业大学科研团队项目(LMTD201901)。

摘　　要：以乙酸乙酯为提取溶剂超声提取聚氨酯产品中的N,N-二甲基甲酰胺,提取液经滤膜过滤后,选择HP-INNOWAX色谱柱为固定相,在离子监测模式(SIM)下扫描,进行气相色谱—质谱法测定,并以保留时间和特征碎片的离子丰度比定性,外标法定量。结果表明,N,N-二甲基甲酰胺在0.2~10 mg/L浓度范围内呈良好的线性,方法检出限为0.46 mg/kg,在3个加标水平下的平均回收率为92.9%~98.7%,相对标准偏差(RSD,n=6)为6.5%~7.7%。该方法准确可靠、方便快捷,适用于实际聚氨酯产品中N,N-二甲基甲酰胺含量的测定。A method based on gas chromatography-mass spectrometry(GC-MS)was developed to determine the content of N,N-dimethylformamide(DMF)in polyurethane(PU)products.DMF in PU sample was ultrasonically extracted using ethyl acetate as solvent,and the extracting solution was then purified with membrane filter.Under the ion monitoring(SIM)mode,DMF was determined using GC-MS with HP-INNOWAX chromatographic column as the stationary phase.Retention time and the abundance ratio of the characteristic fragment ions were adopted for the qualitative analysis,while quantification analysis was performed using an external standard method.Results indicate that a linear calibration curve of DMF can be obtained in the range of 0.2-10 mg/L,and the detection limit is 0.46 mg/kg.The spiked average recoveries varied from 92.9%to 98.7%at three spiked levels with relative standard deviation(RSD,n=6)of 6.5%-7.7%.The present method is accurate,reliable and convenient,and could be applied in the determination of DMF in PU products.

关 键 词：GC-MS 聚氨酯 N N-二甲基甲酰胺 

分 类 号：TS57[轻工技术与工程—皮革化学与工程]