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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.
A novel carboxy-bonded silica stationary phase (RBSP) was prepared by using rhein as raw material and γ-aminopropyl triethoxysilane (KH-550) as coupling agent. The infrared spectra, Elemental analysis was used to characterize its structure.The influence of methanol content in the mobile phase on the performance of the bonded stationary phase was investigated and the chromatographic performance of RBSP was evaluated by using a mixture of acidic, neutral and basic compounds as solute.Methanol - water as mobile phase, the C18 column was used as a reference to study the separation of the two isoflavone compounds and several alkaloids by immobilized silica gel as HPLC, and the chromatographic separation mechanism was also discussed. The results showed that the stationary phase (RBSP) has good reversed-phase chromatographic performance. At the same time, as the bonded phase contains phenolic hydroxyl groups and amide groups, it can provide sites for a variety of solutes and has obvious separation of polar compounds Advantages, and separation speed, can be effectively used for the separation of polar compounds.