Lemus Gallego J M, Pérez Arroyo J
Facultad de Ciencias Qui;micas, Department of Analytical Chemistry and Food Technology, Universidad de Castilla-La Mancha, Ciudad Real 13071, Spain.
J Pharm Biomed Anal. 2003 Apr 1;31(5):873-84. doi: 10.1016/s0731-7085(02)00666-0.
A new, rapid and simple method is described and applied to resolve and quantify mixtures of prednisolone acetate, sulfacetamide and phenylefrine. The determination was accomplished by micellar electrokinetic capillary chromatography (MEKC) using a fused silica capillary (57 cm x 75 microm ID). The separation was carried out at 25 degrees C and 30 kV, using a 5 mM phosphate-5 mM borate buffer adjusted to pH 8.2, 40 mM sodium dodecylsulfate (SDS) as background electrolyte. Under these conditions, the run time was 6.5 min and the limits of quantification were about 0.5 mg l(-1) for every component. Repeatability and reproducibility studies achieved were showing no significant differences at 95% confidence level. Then, multivariate calibration regression spectrophotometric methods (PLS-1, PLS-2 and PCR) were applied providing, especially PLS-1, a clear example of the high resolving power of these techniques. The MEKC method has been applied for quantifying these compounds in different commercial pharmaceuticals products and the method gave good results when it is compared with the spectrophotometric method. The pharmaceutical preparations do not require any separation step by the two described procedures.
本文描述并应用了一种新的、快速且简单的方法来分离和定量醋酸泼尼松龙、磺胺醋酰和去氧肾上腺素的混合物。该测定通过胶束电动毛细管色谱法(MEKC)完成,使用熔融石英毛细管(57 cm×75 μm内径)。分离在25℃和30 kV下进行,使用pH值调至8.2的5 mM磷酸盐 - 5 mM硼酸盐缓冲液以及40 mM十二烷基硫酸钠(SDS)作为背景电解质。在这些条件下,运行时间为6.5分钟,各组分的定量限约为0.5 mg l⁻¹。重复性和再现性研究在95%置信水平下未显示出显著差异。然后,应用了多元校准回归分光光度法(PLS - 1、PLS - 2和PCR),特别是PLS - 1,清楚地展示了这些技术的高分辨能力。MEKC方法已用于定量不同商业药品中的这些化合物,与分光光度法相比,该方法取得了良好的结果。通过上述两种方法,药物制剂无需任何分离步骤。