Chemically bonded silica stationary phases: Synthesis, physicochemical characterization, and molecular mechanism of reversed phase HPLC retention
Chemically bonded silica stationary phases: Synthesis, physicochemical characterization, and molecular mechanism of reversed phase HPLC retention
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DOI：
10.1021/ac9612032
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发表时间：
1997-08-15
影响因子：
7.4
通讯作者：
Kaliszan, R
中科院分区：
文献类型：
--
作者：
Buszewski, B;GadzalaKopciuch, RM;Kaliszan, R
制备了两种用于高效液相色谱的化学键合相：常规的C18和AP(N-酰基氨基丙基硅胶)，这是一种在疏水链上含有特定相互作用中心的新型固定相，用孔度计、电感耦合等离子体原子发射光谱、元素分析、固态CP/MAS核磁共振和层析等物理化学技术表征了化学改性前后固定相的表面性质。为了研究水有机条件下反相高效液相色谱的保留机理，选择了一系列结构不同的溶质，对测试溶质的保留参数和结构参数进行了多参数回归分析和回归分析定量结构-保留关系表明，典型的反相分配机制在C18相上占主导地位，而在AP相上不占主导地位，AP相由于结构上特定的偶极-偶极和与溶质的电荷转移相互作用而为保留提供了重要的输入。所提出的高效液相色谱AP相具有独特而有趣的保留性能，而对设计适当的一系列测试溶质的保留数据进行化学计量学分析似乎是一种方便、客观和定量的方法来证明一种新的相特异性。
Two types of chemically bonded phases for high-performance liquid chromatography (HPLC) have been prepared: a conventional C18 and AP (N-acylaminopropylsilica), a novel one that contains specific interaction sites localized in the hydrophobic chain, Surface properties of stationary phases, before and after chemical modification, have been characterized by several physicochemical techniques, such as porosimetry, ICP atomic emission spectroscopy, elemental analysis, solid state CP/MAS NMR, and chromatography, For the studies of the reversed-phase HPLC retention mechanism under hydroorganic conditions, a test series of structurally diverse solutes has been selected, Sets of retention parameters and structural descriptors of the test solutes were subjected to multiparameter regression analysis, The quantitative structure-retention relationships derived demonstrated the typical reversed-phase partition mechanism to predominate in the separation on the C18 phases but not on the AP phases, The AP phases were demonstrated to provide significant input to retention due to the structurally specific dipole-dipole and charge transfer interactions with the solutes. The proposed AP phases for HPLC possess distinctive and interesting retentive properties, and chemometric analysis of retention data of appropriately designed series of test solutes appears to be a convenient, objective, and quantitative method to prove a new phase specificity.