Rathnasekara Renuka, El Rassi Ziad
Oklahoma State University, Department of Chemistry, Stillwater, OK, 74078-3071, USA.
Oklahoma State University, Department of Chemistry, Stillwater, OK, 74078-3071, USA.
J Chromatogr A. 2017 Jul 28;1508:24-32. doi: 10.1016/j.chroma.2017.05.059. Epub 2017 Jun 1.
Two neutral polyhydroxylated silica bonded stationary phases, namely maltose-silica (MALT-silica) and sorbitol-silica (SOR-silica), have been introduced and chromatographically characterized in hydrophilic interaction liquid chromatography (HILIC) for a wide range of polar compounds. The bonding of the maltose and sorbitol to the silica surface was brought about by first converting bare silica to an epoxy-activated silica surface via reaction with γ-glycidoxypropyltrimethoxysilane (GPTMS) followed by attaching maltose and sorbitol to the epoxy surface in the presence of the Lewis acid catalyst BF.ethereate. Both silica based columns offered the expected retention characteristics usually encountered for neutral polar surface. The retention mechanism is majorly based on solute' differential partitioning between an organic rich hydro-organic mobile phase (e.g., ACN rich mobile phase) and an adsorbed water layer on the surface of the stationary phase although additional hydrogen bonding was also responsible in some cases for solute retention. The MALT-silica column proved to be more hydrophilic and offered higher retention, separation efficiency and resolution than the SOR-silica column among the tested polar solutes such as derivatized mono- and oligosaccharides, weak phenolic acids, cyclic nucleotide monophosphate and nucleotide-5'-monophosphates, and weak bases, e.g., nucleobases and nucleosides.
两种中性多羟基化硅胶键合固定相,即麦芽糖硅胶(MALT-硅胶)和山梨醇硅胶(SOR-硅胶),已被引入并在亲水作用液相色谱(HILIC)中针对多种极性化合物进行了色谱表征。麦芽糖和山梨醇与硅胶表面的键合是通过先将裸硅胶与γ-缩水甘油氧基丙基三甲氧基硅烷(GPTMS)反应转化为环氧活化硅胶表面,然后在路易斯酸催化剂三氟化硼乙醚存在下将麦芽糖和山梨醇连接到环氧表面来实现的。两种硅胶基柱都具有中性极性表面通常具有的预期保留特性。保留机制主要基于溶质在富含有机物的水-有机流动相(例如富含乙腈的流动相)和固定相表面吸附的水层之间的差异分配,尽管在某些情况下额外的氢键作用也对溶质保留有贡献。在测试的极性溶质如衍生化的单糖和寡糖、弱酚酸、环磷酸核苷酸和核苷酸-5'-单磷酸以及弱碱(如碱基和核苷)中,MALT-硅胶柱比SOR-硅胶柱表现出更强的亲水性,具有更高的保留率、分离效率和分辨率。