Method development in pharmaceutical analysis employing capillary electrochromatography

被引:28
作者
Angus, PDA
Victorino, E
Payne, KM
Demarest, CW
Catalano, T
Stobaugh, JF
机构
[1] Univ Kansas, Dept Pharmaceut Chem, Lawrence, KS 66067 USA
[2] Univ Kansas, Ctr Bioanalyt Res, Lawrence, KS 66067 USA
[3] Searle Res & Dev, Skokie, IL USA
关键词
capillary electrochromatography; pharmaceuticals; polar neutral pharmaceuticals; pharmaceutical analysis;
D O I
10.1002/elps.1150191206
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
Capillary electrochromatography (CEC) has been employed to explore method development for a series of structurally related polar neutral compounds of pharmaceutical relevance. Capillaries with dimensions of 75 mu m ID x 25 cm length (34.5 cm total) were packed with Spherisorb ODS-1, Hypersil phenyl, and Hypersil MOS (all 3 mu m particles) and were compared in the reversed-phase mode in order to determine which phase provided the best initial performance and thus serve as the phase of choice for additional method development experiments. The various separation parameters examined for their effect on efficiency, k', resolution, and linear velocity included percent and type of organic modifier, buffer concentration, voltage, and temperature. All separations were conducted with an acidic mobile phase (aqueous mobile phase component, pH 3.0). The separation efficiencies obtained were on the order of 200 000-260 000 plates/m, which equates to reduced plate heights of 1.22 for columns packed with Spherisorb, ODS-1. Repeatable column-to-column separation performance was demonstrated.
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页码:2073 / 2082
页数:10
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