顶空-气相色谱-质谱法测定富马酸二甲酯(DMF)胶囊中硫酸二甲酯(DMS)的定性、定量分析方法

Qualitative and Quantitative Analysis of Dimethyl sulfate(DMS) in Dimethyl Fumarate(DMF) Capsule by Headspace GC-MS

采用气相色谱-质谱法对富马酸二甲酯(DMF)胶囊中残留硫酸二甲酯(DMS)进行测定。并采用顶空富集方法,与溶剂萃取富集法比较,此文中提出的顶空分离法具有不需用大量萃取溶剂,简化了操作步骤,加快了分析速度等优点。质谱中选择EI离子源-选择离子检测模式。方法简单、快速、选择性好,硫酸二甲酯(DMS)的质量浓度在一定范围内与其峰面积呈线性关系。同时考察了方法的最低检测浓度和重复性。

A method of headspace GC-MS was used for the analysis of residual Dimelhyl sulfate （DMS） in Dimethyl fumarate（DMF） capsule, the proposed rnethod showed its advantages of avoiding the use of relatively large amount of solvent making the operation much simpler and the analysis much taster, while the results obtained were in consistency with those obtained by the solvent extraction method. EI-SIM was adopted in MS. The method is simple, fast and selective. The mass concentration of Dimethyl sulfate （DMS） is linearly related to its peak area in a certain range. The minimum detection concentration and repeatability of the method were also investigated.