Packed-column supercritical fluid chromatography of a new dihydropyridine drug based on direct injection of emulsion samples

被引:15
作者
Karlsson, L
Gyllenhaal, O
Karlsson, A
Gottfries, J
机构
[1] Analytical Chemistry, Astra Hässle AB
关键词
direct injection; injection methods; emulsion samples; pharmaceutical analysis; experimental design; central composite design; dihydropyridines;
D O I
10.1016/0021-9673(96)00366-4
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
In this paper, a method based on direct injection in packed-column supercritical fluid chromatography (SFC) for the determination of a dihydropyridine drug in emulsion samples is described. To optimize the chromatographic system, an experimental design approach with four factors was applied. The parameters studied were modifier-carbon dioxide ratio, flow-rate, column temperature and back-pressure. A face-centred central composite design (CCF) yielded a model with good fit and high predictive power. Using plates per second as the response parameter, a fast method for quantitative determination of the analyte was developed. Within the experimental space investigated, the concentration of the polar component in the mobile phase and the flow-rate were found to be the important parameters. Peak compression effects, resulting in high apparent peak numbers (>80 000 versus a nominal value of 7000) were encountered when emulsion samples were injected.
引用
收藏
页码:193 / 199
页数:7
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