大黄酸键合硅胶固定相的简便制备及色谱性能评价simple preparation .pdf

2010 年第 68 卷 化 学 学 报 Vol. 68, 2010 第 2 期, 169～173 ACTA CHIMICA SINICA No. 2, 169～173 ·研究论文· 大黄酸键合硅胶固定相的简便制备及色谱性能评价 代永矿 彭敬东* 常晓娟 (西南大学化学化工学院 重庆 400715) 摘要 以大黄酸为原料, γ-氨丙基三乙氧基硅烷(KH-550)为偶联剂, 简便制备了一种新型羧基键合硅胶固定相(RBSP), 并用红外光谱、热重分析及元素分析对其结构进行表征. 考察了流动相中甲醇含量对键合固定相色谱性能的影响, 并 以含酸性、中性和碱性化合物的混合物为溶质, 评价 RBSP 的色谱性能. 以甲醇-水为流动相, 用 C18 柱作参比, 研 究了该键合硅胶作为 HPLC 固定相对两种大豆异黄酮化合物和几种生物碱基的分离, 并对其色谱分离机理进行了初步 探讨. 实验结果表明, 该固定相(RBSP)具有较好的反相色谱性能, 同时由于键合相中含有酚羟基及酰胺基团, 能为多 种溶质提供作用位点, 对极性化合物的分离具有明显优势, 且分离速度快, 可有效用于极性化合物的分离分析. 关键词 高效液相色谱; 大黄酸键合硅胶; 大豆异黄酮; 色谱固定相 Simple Preparation and Evaluate Chromatographic Properties of Rhein Bonded Silica Gel Stationary Phase Dai, Yongkuang Peng, Jingdong* Chang, Xiaojuan (School of Chemistry and Chemical Engineering, Southwest University, Chongqing 400715) Abstract Rhein was used as the raw material and γ-aminopropyltriethoxy silane (KH-550) as the coupling agent to simply prepare a new carboxy bonded silica gel (RBSP), which could be used as a stationary phase. The structure of RBSP was characterized by infrared spectroscopy, thermal analysis and elemental analysis. The effect of methanol content in the mobile phase on chromatographic performance of the bonded station- ary phase was investigated. The chromatographic performance of RBSP was also evaluated using the mix- ture of acidic, neutral and basic comp