十八烷基键合硅胶的原子层沉积法封尾及其在碱性化合物分离中的应用

采用原子层沉积法对十八烷基键合硅胶进行端基封尾.以六甲基二硅氮烷为封端试剂,在250 ℃下与键合硅胶样品反应6 h,制备了对碱性化合物具有高惰性的反相色谱填料.分别以吡啶/苯酚和萘/阿米替林为分子探针,考察了经原子层沉积法和传统液相有机溶剂法封尾处理的十八烷基键合硅胶的色谱性能,并与商品十八烷基硅胶Zorbax SB-C18和Kromasil C18进行对比.结果表明,原子层沉积法封尾的十八烷基硅胶对碱性化合物的分离特性明显优于传统液相法,其色谱性能已超过Zorbax SB-C18,与Kromasil C18相当.本方法无需有机溶剂,操作简便,反应耗时短,易于放大生产,封尾反应完全,应用前景良好.

Endcapping of Octadecyl Bonded Silica by Atomic Layer Deposition for Separation of Basic Compounds

Atomic layer deposition has been employed for postsynthesis treatment of octadecyl bonded silica (ODS) as a typical reversed-phase stationary phase for high performance liquid chromatography (HPLC) ,in an effort to alleviate peak tailing for basic compounds. With hexamethyldisilazane( HMDS) as an endcapping agent,the ODS packing materials were heated to 250℃,and maintained at that temperature for 6 h,affording packing materials which are highly inert to basic compounds. Chromatographic performance in terms of retention factor and tailing factor of the resulting phases was evaluated using phenol/pyridine and naphthalene/ami-triptyline pairs as probes. The results were compared with those for the same packing treated by liquid phase method and for the commercial products including Zorbax SB-C_(18) and Kromasil C_(18). The separation characteristics of the ODS phase obtained by atomic layer deposition appear to be superior to that by liquid phase method and,comparable with or even better than the commercial products studied. Being solvent-free process amenable to mass production,the described method provides an economical and eco-friendly approach to manufacturing HPLC packing materials on industrial scale.