苯基异氰酸酯环糊精键合相的制备及色谱行为的研究  

Preparation of Phenyl Isocyanate-Functionalized β-Cyclodextrin and Study on Its Chromatographic Behavior as a Stationary Phase

作　　者：史坚[1] 邵芸[1] 邹公伟[1] 

机构地区：[1]南京大学化学系

出　　处：《色谱》1995年第6期444-446,共3页Chinese Journal of Chromatography

摘　　要：以ＤＧ－２硅胶为载体，３－氨基丙基三乙氧基硅烷作为烷胺化试刑，选择己二酰氯为空间臂给体，将苯基异氰酸酯β－环糊精键合至ＤＧ－２上。用三申基氧硅烷对制得的键合相进行末端封闭，并对末端封闭的键合相（相Ⅰ）和未进行末端封闭的键合相（相Ⅱ）的ＭｃＲｅｙｎｏｌｄｓ常数进行了研究。相Ⅰ与相Ⅱ的常数差值可以认为是活性氢贡献的。还测定了二甲苯异构体在相Ⅰ和相Ⅱ上的焓值与熵值。在相Ⅰ上的对、间和邻二甲苯的焓变值ΔＨ分别为－３３．８，－３９．８和－４５．６ｋＪ·ｍｏｌ￣（－１），其分离程度明显优于相Ⅱ。he pretreated silica gel DG-2 was alkylaminated with 3-aminopropyltriethoxysilane in benzene and pyri-dine under nitrogen atmosphere for 15h.The product was washed and dried under vacuum at 60℃ for about5h.The spacer hexanediacyl chloride was added dropwise to the tetrahydrofuran-pyridine solution of theproduct which was refluxed,and then an N,N-dimethylacetylamide-pyridine mixture of β-cyclodextrin(β-CD)was added in the same way. The silica gel immobilized β-CD was reacted further with phenyl iso-cyanate. The McReynolds constants were determined for the end-capping(phase Ⅰ)withtrimethylchlorosilane and non-end-capping(phase Ⅱ) functionalized β-CD. Differences of McReynolds con-stants of the two phases may be considered as a contribution of residual silanol groups. The enthalpies andentropies of xylene isomers were determined for both phase Ⅰ and Ⅱ.Higher selectivity for xylene isomerswas observed for phase Ⅰ than for the phase Ⅱ.On phase Ⅰ the enthalpy values of p,m,O-xylene were-33.8,-39.8 and-45.6 kJ·mol￣(-1) respectively.

关 键 词：气相色谱 苯基异氰酸酯 环糊精 键合固定相 

分 类 号：O657.71[理学—分析化学] O636.12[理学—化学]