Yardimci Ceren, Süslü Incilay, Ozaltin Nuran
Department of Analytical Chemistry, Faculty of Pharmacy, University of Hacettepe, 06100, Sihhiye, Ankara, Turkey.
Anal Bioanal Chem. 2004 May;379(2):308-11. doi: 10.1007/s00216-004-2539-8. Epub 2004 Feb 20.
A fast and simple micellar electrokinetic capillary chromatographic method was developed for the analysis of piribedil in pharmaceutical formulations. The effects of buffer concentration, buffer pH, sodium dodecyl sulphate (SDS) concentration, organic modifier, applied voltage and injection time were investigated. Optimum results were obtained with a 50 mM borate buffer at pH 8.0 containing 50 mM SDS by using a fused silica capillary (50 microm internal diameter, 72 cm effective length). The sample was injected hydrodynamically for 4 s at 50 mbar pressure and the applied voltage was +30 kV. The detection wavelength was set at 205 nm. Diflunisal was used as an internal standard. The analysis was performed at 25 degrees C and the total run time was 14 min. The method was suitably validated with respect to linearity range, limit of detection and quantification, precision, accuracy, specificity and robustness. The linear calibration range was 5-100 microg mL(-1) and the limit of detection was determined as 1 microg mL(-1). The method developed was successfully applied to the determination of piribedil in pharmaceutical formulations. The results were compared with a spectrophotometric method reported in the literature and no significant difference was found statistically.
建立了一种快速简便的胶束电动毛细管色谱法,用于分析药物制剂中的吡贝地尔。研究了缓冲液浓度、缓冲液pH值、十二烷基硫酸钠(SDS)浓度、有机改性剂、施加电压和进样时间的影响。使用内径50 μm、有效长度72 cm的熔融石英毛细管,在pH 8.0的50 mM硼酸盐缓冲液中加入50 mM SDS,获得了最佳结果。在50 mbar压力下以流体动力学方式进样4 s,施加电压为+30 kV。检测波长设定为205 nm。双氟尼酸用作内标。在25℃下进行分析,总运行时间为14 min。该方法在线性范围、检测限和定量限、精密度、准确度、特异性和稳健性方面得到了适当验证。线性校准范围为5-100 μg mL(-1),检测限确定为1 μg mL(-1)。所建立的方法成功应用于药物制剂中吡贝地尔的测定。将结果与文献报道的分光光度法进行比较,在统计学上未发现显著差异。