姜黄素键合硅胶固定相的制备、表征及色谱性能

通过γ-［(2,3)-环氧丙氧］丙基三甲氧基硅烷(KH-560)偶联剂将具有抗菌功能的植物有效成分姜黄素键合到硅胶上,制备了姜黄素液相色谱键合硅胶固定相(CCSP)。采用元素分析、红外光谱和热分析对该固定相结构进行了表征。以甲醇和水为二元流动相,不同的中性、酸性和碱性化合物为溶质探针,并用ODS柱作参比,对固定相的色谱性能及保留机理进行了研究。研究结果表明,姜黄素键合固定相不仅具有良好的反相色谱性能,同时由于配体结构中所含有的基团形成了含芳环的共轭体系,从而引入了n-π和π-π作用位点,所含的羟基和β-二羰基与溶质之间存在偶极-偶极和氢键作用,与ODS相比,该固定相在极性化合物分离中占优势,且分析速度较快。

Preparation, Characterization and Chromatographic Performance of Curcumin Bonded Silica Stationary Phase

A curcumin bonded silica stationary phase (CCSP) for high performance liquid chromatography was prepared by using gamma-glycidoxypropyltrimethoxysilane (KH-560) as coupling reagent. Its structure was characterized by elemental analysis, Fourier transform infrared spectroscopy and thermal analysis. The chromatographic performance and the retention mechanism on the new packing material were evaluated by using neutral, acidic and basic compounds as solute probes and methanol-water as binary mobile phases. A comparative study with ODS was carried out as well. The results showed that CCSP appeared to be excellent reversed-phase stationary phase with versatile chromatographic functions. The curcumin ligand bonded on silica gel can provide n-pi and pi-pi action sites for different analytes because of its integrated conjugated system. Additionally, the polar hydroxyl and carbonyl groups of curcumin facilitated dipoledipole and hydrogen-bonding interactions between the ligand and solutes in the effective separation process. In comparison with ODS, CCSP has the advantages in fast separation of polar compounds because of its weaker hydrophobicity and various synergistic sites.