环糊精衍生物涂渍毛细管柱的制备及分离性能  

Preparation and Separation Performance of Three New Gas Chromatography Capillary Columns Coated with Cyclodextrin Derivatives

作　　者：颜霞[1] 方智利[1] 林纯[1] 王国梁 范军[1] 郑盛润[1] 贾成俊[1] 章伟光[1] 

机构地区：[1]华南师范大学化学与环境学院,广州510006 [2]广州研创生物技术发展有限公司,广州510663

出　　处：《应用化学》2013年第8期957-962,共6页Chinese Journal of Applied Chemistry

基　　金：广东省中国科学院全面战略合作项目(2010B090300031);广东省国际合作项目(2010B050300021)

摘　　要：以3种环糊精衍生物分别涂覆在毛细管内壁制得气相色谱毛细管柱,以正十二烷为溶质,测得理论塔板数均在2800/m以上,柱效较高。研究了它们对一系列苯系物位置异构体的分离性能,探讨了硝基氯苯、硝基苯胺和苯二胺等化合物在不同柱上的拆分机理。底物分子和固定相之间的弱相互作用(如氢键、偶极相互作用和π-π堆积作用)等直接影响毛细管柱对底物的分离性能。对于苯二胺的位置异构体,在全对氯苯异氰酸酯化β-CD涂覆的毛细管柱(ACD)上的分离因子为1.88,在多叠氮β-CD衍生物涂覆的毛细管柱(NMCD)上的分离因子为1.41,但在单叠氮β-CD衍生物涂覆的毛细管柱(NSCD)上无法分开;对于硝基氯苯,在NMCD柱和ACD柱上的分离因子相近(前者为1.13/1.11;后者为1.08/1.15),在NSCD柱上则无分离趋势;对于硝基苯胺,在NMCD柱上无分离趋势。同时,苯环上不同取代基间电子效应则影响了异构体在气相色谱中出峰顺序。Three kinds of capillary columns were obtained by coating cyclodextrin derivatives onto inner surface of fused capillary. According to the literature＇s method, all the theoretical plate numbers are over 2800/m by using n-dodecane, indicating that they have high column efficiencies. Then, separation and mechanism of isomeric benzene derivatives, such as nitrochlorobenzene, nitroaniline, and phenylenediamine by capillary column gas chromatography have been investigated in detail. The interactions such as hydrogen bonding, dipolar-dipolar attraction and π-π stacking between analytes and stationary phases have significant effect on the separation performances of these capillary columns. For phenylenediamine, separation factors on the heptakis （ 6-azido-6-deoxy-2, 3-di-O-p-chlorophenylcarbamoylated ）-b-CD （ NMCD ） and per（p- chlorophenylcarbamoylated）-b-CD（ACD） columns are 1.41 and 1.88, respectively, however the positional isomers can not be separated on the NSCD column. For nitrochlorobenzene, the separation factors on the mono （6A-azido-6A-deoxy） per-acetylated-β-CD（NMCD） column are 1. 13 and 1.11, respectively, which are very close to those on the ACD column （1.08 and 1.15, respectively）, and three positional isomers of nitrochlorobenzene can not be separated on the NSCD column. In addition, the separation of nitroaniline can not be achieved. Meanwhile, the electronic effects derived from different groups of benzene derivatives contribute mainly to the elution order of all the analytes.

关 键 词：环糊精衍生物 毛细管柱气相色谱 固定相 苯系物位置异构体 色谱分离 

分 类 号：O657.7[理学—分析化学]