使用非水离子洗脱剂在硅胶柱上对碱性药物进行高效液相色谱分析。I. 影响保留、峰形和检测器响应的因素。

High-performance liquid chromatographic analysis of basic drugs on silica columns using non-aqueous ionic eluents. I. Factors influencing retention, peak shape and detector response.

作者信息

Flanagan R J, Jane I

出版信息

J Chromatogr. 1985 Apr 26;323(2):173-89. doi: 10.1016/s0021-9673(01)90383-8.

Abstract

The use of silica columns together with non-aqueous ionic eluents provides a stable yet flexible system for the high-performance liquid chromatographic analysis of basic drugs. At constant ionic strength, eluent pH influences retention via ionisation of surface silanols and protonation of basic analytes, pKa values indicating the pH of maximum retention. At constant pH, retention is proportional to the reciprocal of the eluent ionic strength for fully protonated analytes and quaternary ammonium compounds. The addition of water up to 10% (v/v) has little effect on retention if the protonation of the analytes is unaffected. Thus, it is likely that retention is mediated primarily via cation exchange with surface silanols. However, additional factors must play a part with compounds such as morphine which give tailing peaks at acidic or neutral eluent pHs.

摘要

硅胶柱与非水离子洗脱剂的联用为碱性药物的高效液相色谱分析提供了一个稳定且灵活的系统。在恒定离子强度下，洗脱剂pH值通过表面硅醇的离子化和碱性分析物的质子化影响保留时间，pKa值表明了最大保留时间时的pH值。在恒定pH值下，对于完全质子化的分析物和季铵化合物，保留时间与洗脱剂离子强度的倒数成正比。如果分析物的质子化不受影响，加入高达10%（v/v）的水对保留时间影响很小。因此，保留时间可能主要通过与表面硅醇的阳离子交换来介导。然而，对于吗啡等在酸性或中性洗脱剂pH值下出现拖尾峰的化合物，其他因素肯定也起了作用。