混合型硅胶基质高效液相色谱填料的制备与表征

以自制的高纯硅胶微球为原料，通过与二甲基十八烷基甲氧基硅烷、γ-氨丙基三乙氧基硅烷、碘甲烷等一系列物质键合，合成了一种新型的反相/离子型混合硅胶基质色谱柱填料。经元素分析、红外光谱、²⁹Si固体核磁共振和差热热重等分析手段对硅胶基质混合固定相进行了表征；以甲醇和水作为二元流动相，对尿嘧啶、苯酚、对氯硝基苯和萘进行了色谱分离。结果表明，色谱峰的不对称因子为0.95~1.10， 萘的理论塔板数92000块/m，分离度均在4.0以上。

Preparation and characterization of a silica-based mixed stationary phase as an HPLC packing material

A new type of silica-based packing material for HPLC columns has been prepared. Home-made silica spheres with high purity were first functionalized with methoxy(dimethyl)octadecylsilane, 3-triethoxysilylpropylamine was then bonded to the C₁₈-functionalized silica, and finally followed by quaternization with iodomethane to form the final product. Elemental analysis, infrared spectroscopy and²⁹Si NMR spectroscopy were employed to characterize the mixed packing materials. A standard solution of uracil, phenol, 4-chloronitrobenzene and naphthalene was used to verify the chromatographic performance of the resulting packing material. With the asymmetry factor being 0.95 to 1.10, the theoretical plate number for naphthalene being more than 92000, and the resolution being over 4.0, the functionalized silica spheres were demonstrated to be a potential packing material for HPLC columns.