Department of Chemistry, University of Tennessee, Knoxville, TN 37996-1600, USA.
J Chromatogr A. 2013 Mar 22;1282:46-57. doi: 10.1016/j.chroma.2013.01.027. Epub 2013 Jan 25.
The adsorption behavior of nortriptylinium hydrochloride was investigated in detail on a new C18-bonded charged surface hybrid stationary phase (CSH-C18, Waters) at a constant W(S)pH of 2.60 (phosphate buffer dissolved in an acetonitrile/water mixture, 34/66, v/v) in order to promote strong repulsive electrostatic interactions between the surface of the packing material and the analyte molecules. This new stationary phase was recently designed to reduce the peak tailing of ionizable compounds in RPLC. Overloaded band profiles were recorded over a broad range of column loading factors (0.03-2.18%) and eluent ionic strengths (5-50mM). The experimental data were compared to those predicted by some electrostatically modified adsorption isotherms, including the Langmuir and the Moreau isotherms. For small loading factors (<0.1%), the electrostatic repulsion definitely plays a role on the adsorption behavior and the retention factors increase with increasing ionic strength due to the expected diminution of the Debye length through the bulk solution. Still this effect could not be consistently described by either of the above two electrostatic isotherm models over the whole range of ionic strengths. For higher loading factors (>0.1%), the compound was mostly adsorbed as a neutral species and the adsorption behavior was best represented by an apparent Langmuir-Moreau isotherm model.
详细研究了盐酸去甲替林在一种新型 C18 键合带电表面混合固定相(CSH-C18,Waters)上的吸附行为,在恒定的 W(S)pH 值为 2.60(磷酸盐缓冲液溶解在乙腈/水混合物中,34/66,v/v)的条件下,以促进固定相表面与分析物分子之间的强排斥静电相互作用。这种新型固定相最近被设计用于减少 RPLC 中可电离化合物的峰拖尾。在较宽的柱载因子(0.03-2.18%)和洗脱液离子强度(5-50mM)范围内记录了过载带轮廓。实验数据与一些静电修饰吸附等温线的预测数据进行了比较,包括 Langmuir 和 Moreau 等温线。对于较小的载因子(<0.1%),静电排斥肯定会对吸附行为产生影响,并且保留因子随着离子强度的增加而增加,这是由于通过整个溶液预计 Debye 长度的减小。尽管如此,在整个离子强度范围内,上述两种静电等温线模型都不能一致地描述这种效应。对于较高的载因子(>0.1%),化合物主要以中性物质的形式被吸附,吸附行为最好由表观 Langmuir-Moreau 等温线模型来表示。