大黄酸键合硅胶固定相的简便制备及色谱性能评价

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,评价了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.

Simple Preparation and Evaluate Chromatographic Properties of Rhein Bonded Silica Gel Stationary Phase

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 stationary phase was investigated. The chromatographic performance of RBSP was also evaluated using the mixture of acidic, neutral and basic compounds as solute. The separating property was carried out using the bonded silica gel as a stationary phase of HPLC and methanol-water as the mobile phase by separating two kinds of soy isoflavones and several biological bases compared to C18. The chromatographic separation mechanism was also initially discussed. The results demonstrated that RBSP possessed good reversed-phase chromatographic behavior. At the same time, because the bonded stationary phase containing phenolic hydroxyl and amide groups can provide action sites for multiple compounds, it has the obvious advantage in separating polar compounds especially its fast separating rate. So the RBSP could be efficiently used for the separation of polar compounds.