Murauer Adele, Bakry Rania, Schottenberger Herwig, Huck Christian, Ganzera Markus
Institute of Pharmacy, Pharmacognosy, University of Innsbruck, Innsbruck, Austria.
Institute for Analytical Chemistry and Radiochemistry, University of Innsbruck, Innsbruck, Austria.
Anal Chim Acta. 2017 Apr 22;963:136-142. doi: 10.1016/j.aca.2017.01.048. Epub 2017 Feb 2.
A methacrylate based monolith, containing the innovative zwitterionic monomer (3-allyl-1-imidazol)propane sulfonate, was prepared in 100 μm I.D. silica capillaries by UV initiated photo-polymerization. Composition of the porogen, i.e. a mixture of 1-propanol, 1,4 butanediol and water, was of great importance to obtain a homogeneous monolith with satisfactory permeability and good electrochromatographic performance. Morphology of the stationary phase was studied in Scanning Electron Microscopy and IR experiments, which revealed a good attachment to the capillary wall, flowthrough-pores in the range of 0.5-2 μm, and a continuous monolithic structure. The developed material was well suited for the analysis of six common phenolic acids (salicylic, cinnamic, syringic, rosmarinic, caffeic and chlorogenic acid) by CEC. Their separation was possible in less than 8 min with a mobile phase comprising a 12 mM aqueous ammonium acetate solution with pH 8.5 and acetonitrile, at an applied voltage of - 20 kV. The developed method was validated (R ≥ 0.995; LOD ≤ 3.9 μg mL, except for salicylic acid; recovery rates from 94 to 104%) and successfully used for the determination of phenolic acids in Coffea arabica samples. All of them contained cinnamic, syringic and caffeic acid, however only in unroasted coffee beans chlorogenic acid (0.06%) was found. The quantitative results were in good agreement to reported literature data.
通过紫外光引发光聚合反应,在内径为100μm的硅胶毛细管中制备了一种基于甲基丙烯酸酯的整体柱,该整体柱含有新型两性离子单体(3-烯丙基-1-咪唑)丙烷磺酸盐。致孔剂的组成,即1-丙醇、1,4-丁二醇和水的混合物,对于获得具有令人满意的渗透性和良好电色谱性能的均匀整体柱非常重要。通过扫描电子显微镜和红外实验研究了固定相的形态,结果表明其与毛细管壁附着良好,流通孔尺寸在0.5-2μm范围内,且具有连续的整体结构。所开发的材料非常适合通过毛细管电色谱法分析六种常见的酚酸(水杨酸、肉桂酸、丁香酸、迷迭香酸、咖啡酸和绿原酸)。在-20kV的施加电压下,使用由pH 8.5的12mM醋酸铵水溶液和乙腈组成的流动相,不到8分钟即可实现它们的分离。所开发的方法经过验证(R≥0.995;除水杨酸外,检测限≤3.9μg/mL;回收率为94%-104%),并成功用于测定阿拉伯咖啡豆中的酚酸。所有样品均含有肉桂酸、丁香酸和咖啡酸,然而,仅在未烘焙的咖啡豆中发现了绿原酸(0.06%)。定量结果与文献报道数据吻合良好。