El-Saharty Yasser Shaker, Metwally Fadia H, Refaat Mohamed, El-Khateeb Sonia Zaki
Cairo University, Faculty of Pharmacy, Analytical Chemistry Department, El-Kasr El-Aini St, ET-1 1562 Cairo, Egypt.
J AOAC Int. 2007 Jan-Feb;90(1):102-12.
A binary mixture of hyoscine butylbromide and ketoprofen was determined by 4 different methods. The first involved determination of hyoscine butylbromide and ketoprofen using the ratio-spectra first-derivative spectrophotometric technique at 211 and 234 nm over the concentration ranges of 2-14 and 5-45 microg/mL with mean accuracies 99.84 +/-0.92 and 99.98+/- 0.64%, respectively. The second method utilized second-derivative spectrophotometry over the concentration ranges of 2-14 and 5-35 microg/mL with mean accuracies 99.32+/- 1.06 and 99.55+/-1.15%, respectively. The third method was based on the resolution of the 2 components by bivariate calibration depending on a simple and rapid mathematical algorithm and quantitative evaluation of the absorbances at 206 and 254 nm over concentration ranges of 2-16 and 5-35 microg/mL; mean accuracies of 100.21+/-1.30 and 100.19 +/-1.07% were obtained for hyoscine butylbromide and ketoprofen, respectively. The fourth method was reversed-phase liquid chromatography using 0.05 M ammonium dihydrogen phosphate-acetonitrile-methanol (20 + 30 + 6, v/v) as the mobile phase with ultraviolet detection at 220 nm over concentration ranges of 1-90 and 5-70 microg/mL; mean accuracies were 99.92+/-1.02 and 99.61+/- 0.98%, respectively. The suggested procedures were checked using laboratory-prepared mixtures and were successfully applied for the analysis of pharmaceutical preparations. The methods retained their accuracy and precision when the standard addition technique was applied. The results obtained by applying the proposed methods were statistically analyzed and compared with those obtained by the manufacturer's method.
采用4种不同方法对丁溴东莨菪碱和酮洛芬的二元混合物进行了测定。第一种方法是运用比率光谱一阶导数分光光度法，分别在211和234nm波长下测定丁溴东莨菪碱和酮洛芬，其浓度范围分别为2 - 14μg/mL和5 - 45μg/mL，平均准确度分别为99.84±0.92%和99.98±0.64%。第二种方法是利用二阶导数分光光度法，浓度范围分别为2 - 14μg/mL和5 - 35μg/mL，平均准确度分别为99.32±1.06%和99.55±1.15%。第三种方法基于双变量校准对两种成分进行分离，依靠一种简单快速的数学算法，并在206和254nm波长下对浓度范围为2 - 16μg/mL和5 - 35μg/mL的吸光度进行定量评估；丁溴东莨菪碱和酮洛芬的平均准确度分别为100.21±1.30%和100.19±1.07%。第四种方法是反相液相色谱法，使用0.05M磷酸二氢铵 - 乙腈 - 甲醇（20 + 30 + 6，v/v）作为流动相，在220nm波长下进行紫外检测，浓度范围分别为1 - 90μg/mL和5 - 70μg/mL；平均准确度分别为99.92±1.02%和99.61±0.98%。使用实验室配制的混合物对所建议的方法进行了检验，并成功应用于药物制剂的分析。当应用标准加入法时，这些方法仍保持其准确度和精密度。对应用所提出方法获得的结果进行了统计分析，并与制造商方法获得的结果进行了比较。
