CAJ | 학술논문

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-C_(18)和Kromasil C_(18)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-C_(18),与Kromasil C_(18)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.
채용원자층침적법대십팔완기건합규효진행단기봉미.이륙갑기이규담완위봉단시제,재250 ℃하여건합규효양품반응6 h,제비료대감성화합물구유고타성적반상색보전료.분별이필정/분분화내/아미체림위분자탐침,고찰료경원자층침적법화전통액상유궤용제법봉미처리적십팔완기건합규효적색보성능,병여상품십팔완기규효Zorbax SB-C_(18)화Kromasil C_(18)진행대비.결과표명,원자층침적법봉미적십팔완기규효대감성화합물적분리특성명현우우전통액상법,기색보성능이초과Zorbax SB-C_(18),여Kromasil C_(18)상당.본방법무수유궤용제,조작간편,반응모시단,역우방대생산,봉미반응완전,응용전경량호.
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.