Nemutlu Emirhan, Kir Sedef
Department of Analytical Chemistry, Faculty of Pharmacy, University of Hacettepe, 06100 Ankara, Turkey.
J Pharm Biomed Anal. 2003 Feb 26;31(2):393-400. doi: 10.1016/s0731-7085(02)00641-6.
A capillary zone electrophoresis assay for the analysis of meloxicam has been developed and validated. The influence of buffer concentration, buffer pH, methanol as organic modifier, capillary temperature, applied voltage and injection time was systemically investigated in a fused silica capillary (i.d. 50 microm, total length 44 cm and effective length 35.5 cm). Optimum results were obtained with a 100 mM borate buffer (pH 8.5) containing 5% methanol, capillary temperature 25 degrees C, applied voltage 20 kV and injection time 3 s hydrodynamic injection. The detection wavelength was set to 205 nm. Diflunisal was used as internal standard. The method showed good selectivity, accuracy, precision, linearity and sensitivity according to the evaluation of the validation parameters. The method was applied to the determination of six pharmaceutical preparations including two dosage forms. The relative standard deviation of 7 replicate analyses for each sample was less than 0.66%. The results were compared with a spectrophotometric method reported in literature and no significant difference was found statistically.
已开发并验证了一种用于分析美洛昔康的毛细管区带电泳测定法。在熔融石英毛细管（内径50微米，总长度44厘米，有效长度35.5厘米）中，系统研究了缓冲液浓度、缓冲液pH值、作为有机改性剂的甲醇、毛细管温度、施加电压和进样时间的影响。使用含5%甲醇的100 mM硼酸盐缓冲液（pH 8.5）、毛细管温度25℃、施加电压20 kV和进样时间3秒的流体动力学进样可获得最佳结果。检测波长设定为205纳米。双氯芬酸用作内标。根据验证参数的评估，该方法显示出良好的选择性、准确性、精密度、线性和灵敏度。该方法应用于六种药物制剂（包括两种剂型）的测定。每个样品7次重复分析的相对标准偏差小于0.66%。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。
