GC-MS内标法测定纺织品中富马酸二甲酯及控制点分析

GC-MS Internal Standard Method for Determination of Dimethyl Fumarate in Textile and its Control Points Analysis

采用气相色谱-质谱联用仪（GC/MS）内标法对纺织品中富马酸二甲酯（DMF）进行分析检测。样品用乙酸乙酯超声波浴萃取,经浓缩净化定容后,通过GC/MS的保留时间及特征离子进行定性和定量分析。探讨了天然纤维和人造纤维样品基质对检测结果的影响。结果表明,天然纤维对低浓度DMF的回收率有较大影响,在加标1μg/mL浓度下回收率仅为10%~20%,加标5μg/mL浓度下的回收率提升至70%左右,加标10μg/mL浓度时可达到99%,相对标准偏差为2.67%。最后,分析了影响检测实验数据的关键点。该方法对检测皮革中的富马酸二甲酯具有一定的借鉴意义。

GC/MS internal standard method for the determination of dimethyl fumarate （DMF） in textile was developed in which DMF in textile was extracted with ethyl acetate by ultrasonic treatment and the qualitative and quantitative analysis of DMF was carried out by comparison of retention time and specific fragment ions respectively. The influence of different fiber matrixes on quantitative analysis of DMF was studied. The results indicated that DMF was hardly detected when low concentration existed in natural fibers. The recovery rate was only 10%-20% when 1 μg/mL DMF was added, and it was about 70% when 5 μg/mL DMF added. Finally control points of DMF determination procedure were also analyzed. This method has valuable reference to detect dimethyl fumarate in leather oroducts.