Optimisation and validation of a capillary electrophoresis method for the simultaneous determination of diazepam and otilonium bromide

被引:20
作者
Furlanetto, S
Orlandini, S
Massolini, G
Faucci, MT
La Porta, E
Pinzauti, S
机构
[1] Univ Florence, Dept Pharmaceut Sci, I-50121 Florence, Italy
[2] Univ Pavia, Dept Pharmaceut Chem, I-27100 Pavia, Italy
关键词
D O I
10.1039/b103091b
中图分类号
O65 [分析化学];
学科分类号
070302 ; 081704 ;
摘要
A simultaneous assay of diazepam and otilonium bromide in coated tablets by capillary zone electrophoresis (CZE) was developed. The influence of various parameters (voltage, temperature, buffer concentration and pH, ethanol percentage) on analysis time and on the theoretical plates of the two peaks was investigated by means of experimental design. A response surface study was carried out by means of a 27-run D-optimal matrix. The best background electrolyte was found to be 0.13 M, pH 2.9 Britton-Robinson buffer, containing 10% v/v ethanol. Other optimised parameters were voltage (30 kV) and temperature (30 degreesC). The UV detector for quantitation of otilonium bromide and diazepam was set at 280 nm and 230 nm, respectively. Procaine hydrochloride was used as internal standard and run time was less than five minutes. Validation was performed, for drug substance and drug product, according to ICH3 guidelines. For drug product the recovery for otilonium bromide and diazepam ranged from 98.3% to 101.2% and from 97.1% to 99.0%, respectively; the RSD values found for otilonium bromide and diazepam ranged from 2.4% to 3.0% and from 1.1% to 4.5%, respectively.
引用
收藏
页码:1700 / 1706
页数:7
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