Emre Deniz, Ozaltin Nuran
Hacettepe University, Faculty of Pharmacy, Department of Analytical Chemistry, Ankara, Turkey.
J Chromatogr B Analyt Technol Biomed Life Sci. 2007 Mar 1;847(2):126-32. doi: 10.1016/j.jchromb.2006.09.036. Epub 2006 Oct 13.
A new micellar electrokinetic capillary chromatographic method has been developed to analyze the pharmaceutical preparations containing ternary combination of paracetamol (PAR), caffeine (CAF) and propyphenazone (PRO). Best results were obtained by using 20mM pH 9.0 borate buffer containing 30mM sodiumdodecylsulphate as the background electrolyte. Diflunisal (DIF) was used as internal standard (IS). The separation was performed through a fused silica capillary (50microm internal diameter, 44cm total length, 35.5cm effective length) at 25 degrees C with the application of 3s of hydrodynamic injection at 50mbar pressure and a potential of 29kV. Detection wavelength was 200nm. Under these conditions, the migration times were found to be 5.174min for PAR, 5.513min for CAF, 7.195min for DIF, and 9.366min for PRO. Linearity ranges for the method were determined as 2-200microgmL(-1) for PAR and CAF and 3-200microgmL(-1) for PRO. Limit of detections were found as 0.6microgmL(-1) for PAR and CAF and 0.8microgmL(-1) for PRO. According to the validation study, the developed method was proved to be accurate, precise, sensitive, specific, rugged and robust. Three pharmaceutical preparations, which are produced by different drug companies in Turkey, were analyzed by the developed method. One of the same preparations was also analyzed by the derivative ratio spectro zero-crossing spectrophotometric method reported in literature. No significant differences were found statistically.
已开发出一种新型胶束电动毛细管色谱法,用于分析含有对乙酰氨基酚(PAR)、咖啡因(CAF)和保泰松(PRO)三元组合的药物制剂。使用含有30mM十二烷基硫酸钠的20mM pH 9.0硼酸盐缓冲液作为背景电解质可获得最佳结果。双氟尼酸(DIF)用作内标(IS)。在25℃下,通过熔融石英毛细管(内径50μm,总长度44cm,有效长度35.5cm)进行分离,在50mbar压力下进行3s的流体动力学进样,并施加29kV的电压。检测波长为200nm。在这些条件下,PAR的迁移时间为5.174min,CAF为5.513min,DIF为7.195min,PRO为9.366min。该方法的线性范围确定为PAR和CAF为2 - 200μg/mL,PRO为3 - 200μg/mL。PAR和CAF的检测限为0.6μg/mL,PRO为0.8μg/mL。根据验证研究,所开发的方法被证明准确、精密、灵敏、特异、耐用且稳健。用所开发的方法分析了土耳其不同制药公司生产的三种药物制剂。还用文献报道的导数比光谱零交叉分光光度法分析了其中一种相同的制剂。统计学上未发现显著差异。