Siddiqui Farhan Ahmed, Arayne M Saeed, Sultana Najma, Qureshi Faiza
University of Karachi, Department of Chemistry, Karachi-75270, Pakistan.
J AOAC Int. 2011 Jan-Feb;94(1):150-8.
A method is described for the simultaneous determination of paracetamol, tizanidine, and diclofenac in mixtures. The method was based on HPLC separation of the three drugs followed by UV detection at 254 nm. The separation was carried out on a Hypersil ODS, C18 (250 x 4.6 mm id, 10 microm particle size) column using the mobile phase aqueous 0.2% ammonium carbonate-methanol (60 + 40, v/v) at a flow rate of 1 mL/min. The linear regression analysis data were used for the regression curve in the range of 170-10 000 ng/mL for paracetamol, 120-10 000 ng/mL for tizanidine, and 20-10 000 ng/mL for diclofenac. No chromatographic interference from tablet excipients was found. In order to check the selectivity of the proposed method, degradation studies were carried out using hydrolysis (acid, basic, and neutral), thermolysis, and oxidation. The developed method, after being validated in terms of precision, robustness, recovery, LOD, and LOQ, was successively applied to the analysis of pharmaceutical formulations and human serum.
描述了一种同时测定混合物中对乙酰氨基酚、替扎尼定和双氯芬酸的方法。该方法基于三种药物的高效液相色谱分离，随后在254nm处进行紫外检测。分离在Hypersil ODS C18柱（250×4.6mm内径，10μm粒径）上进行，使用流动相0.2%碳酸铵水溶液-甲醇（60 + 40，v/v），流速为1mL/min。线性回归分析数据用于对乙酰氨基酚在170 - 10000ng/mL范围内、替扎尼定在120 - 10000ng/mL范围内以及双氯芬酸在20 - 10000ng/mL范围内的回归曲线。未发现片剂辅料的色谱干扰。为了检验所提出方法的选择性，使用水解（酸、碱和中性）、热解和氧化进行了降解研究。所开发的方法在精密度、稳健性、回收率、检测限和定量限方面经过验证后，相继应用于药物制剂和人血清的分析。
