CAJ | 학술논문

目的:研究适用于毛细管电色谱乃至液相色谱的具有可定制选择性的固定相,以便利用这些新型的固定相,对于难以采用常规的固定相分离的物质实现选择性的分离.方法: 将商品球形硅胶颗粒(粒径5μm)与乙烯基三乙氧基硅烷通过在无水甲苯中回流18 h,进行硅烷化修饰.在硅烷化了的硅胶颗粒上,通过偶氮异丁腈作为引发剂,在正己醇和乙腈(1∶4)的混合溶剂中,80 ℃下反应18 h,引发苯乙烯-二乙烯基苯的链式聚合反应,以及苯乙烯-二乙烯基苯共聚物通过硅胶表面上的乙烯基键合到硅胶表面上的键合反应.所得到的包覆了这种高聚物的硅胶颗粒(PS-DES)本身也是一种非传统的毛细管电色谱用的固定相.所产生的PS-DES再和氯磺酸发生磺化反应,即得到磺酸型的强阳离子交换型固定相.结果: 将所制得的PS-DES固定相以及磺化的固定相各自填充到毛细管内,考察这些毛细管电色谱柱的色谱性能,发现前者表现出反相固定相的性质.由于所包覆高聚物中的苯基基团,这种固定相在色谱分离过程中引入了π-π电子相互作用,因此对芳香化合物表现出了独特的选择性,在其上成功地分析了一些芳香化合物以及极性的和碱性的药物. 在磺酸型的固定相上,则成功地分离了一些碱性药物,得到了较好的对称峰型,这些药物间可达到基线分离.结论:这些固定相有可能用于需要非常规选择性的分析课题(碱性药物的分离即是一例),由于不同于常规固定相的分离机制使分析工作者在一些情况下获得预期的分离效果.
목적:연구괄용우모세관전색보내지액상색보적구유가정제선택성적고정상,이편이용저사신형적고정상,대우난이채용상규적고정상분리적물질실현선택성적분리.방법: 장상품구형규효과립(립경5μm)여을희기삼을양기규완통과재무수갑분중회류18 h,진행규완화수식.재규완화료적규효과립상,통과우담이정정작위인발제,재정기순화을정(1∶4)적혼합용제중,80 ℃하반응18 h,인발분을희-이을희기분적련식취합반응,이급분을희-이을희기분공취물통과규효표면상적을희기건합도규효표면상적건합반응.소득도적포복료저충고취물적규효과립(PS-DES)본신야시일충비전통적모세관전색보용적고정상.소산생적PS-DES재화록광산발생광화반응,즉득도광산형적강양리자교환형고정상.결과: 장소제득적PS-DES고정상이급광화적고정상각자전충도모세관내,고찰저사모세관전색보주적색보성능,발현전자표현출반상고정상적성질.유우소포복고취물중적분기기단,저충고정상재색보분리과정중인입료π-π전자상호작용,인차대방향화합물표현출료독특적선택성,재기상성공지분석료일사방향화합물이급겁성적화감성적약물. 재광산형적고정상상,칙성공지분리료일사감성약물,득도료교호적대칭봉형,저사약물간가체도기선분리.결론:저사고정상유가능용우수요비상규선택성적분석과제(감성약물적분리즉시일례),유우불동우상규고정상적분리궤제사분석공작자재일사정황하획득예기적분리효과.
Objective: To develop new kinds of stationary phases suitable for applications in capillary electrochromatography (CEC), as well as in LC, which can be tailored to realize selective separations of solutes difficult to separate with conventional stationary phases. Methods:Purchased spherical silica particles (5 μm) were refluxed in anhydrous toluene with vinyl-triethoxysilane for 18 h, to modify the surface with vinylsilyl groups. The silylated silica particles were subsequently stirred in an n-henanol-acetonitril mixture (1∶ 4, volume fraction) for 18 h. Styrene and divinylbenzene in the mixture co-polymerized to form a crosslinked encapsulation layer on the silica surface, and bonded on the surface vinyl groups at the same time, both reactions were initiated by azo-iso-butyronitrile. The poly(Styrene-divinylbenzene) encapsulated silica(PS-DES) produced can be used as a non-conventional stationary phase for CEC itself. By sulphonation of the PS-DES phase with chlorosulphonic acid, strong cation-exchange stationary phase of sulphonic type was obtained. Results: The manufactured PS-DES as well as the sulphonated phases were respectively packed into capillaries,and the columns thus prepared were tested for their chromatographic characteristics. It was found that the PS-DES phase showed reversed-phase characteristics. Due to the phenyl groups in the encapsulated polymer, it introduced π-π electronic interaction between the solutes molecules and stationary phase during the chromatographic separation process, therefore it showed unique selectivity on separating aromatic compounds, also polar- as well as some alkaline drugs was analyzed on the column packed with the phase. It was demonstrated that the sulphonated phase could be used to prepare columns for the separation of alkaline drugs, symmetric peaks were obtained for them and base-line separation was realized. Conclusion: It is possible that these stationary phases prepared can be used for solving the analytical problems in which non-conventional selectivity are needed ( the analyses of alkaline drugs are examples). In some cases, the analysts can realize the anticipated separation results based on the different separation mechanism from that of the conventional stationary phases.