气相色谱-质谱法测定富马酸二甲酯时内标物的选择  

Selection of Internal Standards in the Determination of Dimethyl Fumarate by GC-MS

作　　者：谢月亮[1] 凌萍[1] 潘城[1] 沈洪涛[1] 李思源[1] 杨万颖[1] 

机构地区：[1]深圳市计量质量检测研究院,深圳518055

出　　处：《理化检验（化学分册）》2011年第7期791-793,796,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：国家标准制定项目(No.20091134-T-607)

摘　　要：探讨了当采用气相色谱-质谱法测定富马酸二甲酯(DMFU)时内标物的选择问题。采用HP-5MS毛细管色谱柱,在50℃～300℃范围内程序升温分离及采用在50～400amu范围内全扫描方式和选择离子监测模式检测。试验结果表明:以丙二酸二甲酯(DMM)、丙二酸二乙酯(DEM)和戊二酸二甲酯(DMG)作为内标物,既能保持DMFU与3种内标物有良好的分离度,又能保持长久的稳定性,且3种内标物与DMFU的保留时间差均小于2.8min。DMFU的线性范围均为0.005～5.0mg·L^(-1)。方法用于实际样品中DMFU的测定,以上3种物质作为内标,所得结果无显著差别,因此DMM、DEM、DMG均可作为比较理想的内标物用于日常用品中DMFU的检测。It was reported that in the determination of dimethyl fumarate（DMFU） by GC-MS,the use of dimethyl malonate（DMM）,diethyl malonate（DEM） and dimethyl glutarate（DMG） as internal standards was studied and discussed.HP-5MS capillary column with programmed temperature elevation（50℃-300℃） was used in GC separation, and whole scanning mode（in the range of 50-400 amu） as well as selected ions monitoring mode were used in MS detectioa It was found that①clear separation between DMFU and the 3 internal standards was obtained,②values of peak area of the DMFU were keeping in persistent stability③difference of retention times between DMFU and the 3 internal standards were less than 2.8 min.Linearity range of DMFU found were in the range of 0.005-5.0 mg·L^（-1）. The proposed method was applied to the determination of DMFU in substantial samples,the results obtained by using either one of the 3 internal standards showed no significant difference.Therefore,either of the 3 internal standards could be used for routine determination of DMFU in various daily-use products.

关 键 词：气相色谱-质谱法 内标物 富马酸二甲酯 丙二酸二甲酯 丙二酸二乙酯 戊二酸二甲酯 

分 类 号：O657.63[理学—分析化学]