Kayesh Ruhul, Sultan Md Zakir
Department of Pharmaceutical Chemistry, Faculty of Pharmacy, University of Dhaka, Dhaka 1000, Bangladesh.
Centre for Advanced Research in Sciences, University of Dhaka, Dhaka 1000, Bangladesh
J Chromatogr Sci. 2015 May-Jun;53(5):687-93. doi: 10.1093/chromsci/bmu103. Epub 2014 Sep 2.
A rapid, sensitive and stability indicating ion-pair reversed-phase high-performance liquid chromatographic method was developed for simultaneous estimation of naproxen (NPX) and esomeprazole (ESP) in pharmaceutical preparations. In our study, this new method was used to overcome the instability problem of ESP during high-performance liquid chromatographic analysis in the presence of acidic drugs such as NPX. The method was validated according to ICH, FDA and USP guidelines with respect to accuracy, precision, specificity, linearity, solution stability, robustness, sensitivity and system suitability. The method was developed by using an isocratic condition of mobile phase comprising buffer [tetrabutylammonium hydroxide (0.0077 M) and n-heptane sulfonic acid-Na salt (0.002 M), pH 7.6], acetonitrile and methanol in a 60 : 20 : 20 v/v/v ratio at a flow rate of 1.5 mL/min over a C-18 (Octadecyl-silica, 5 µm, 250 × 4.6 mm) column at ambient temperature. The recovery for both drugs was found to be >99% which demonstrated the accuracy of this method. Intra- and inter-day precision studies of the new method were less than the maximum allowable limit [% relative standard deviation (RSD) ≤2.0 according to FDA]. The method showed linear response with a correlation coefficient (r(2)) value of 0.999 for both drugs. More importantly, ESP was quite stable in diluting solvent and mobile phase in the presence of NPX for >3 days. Therefore, it was found to be an accurate, reproducible, sensitive and highly stability-indicating method and can be successfully applied for routine analysis of simultaneous assay of NPX and ESP in pharmaceutical dosage forms.
建立了一种快速、灵敏且具有稳定性指示功能的离子对反相高效液相色谱法，用于同时测定药物制剂中的萘普生（NPX）和埃索美拉唑（ESP）。在我们的研究中，该新方法用于克服在存在如NPX等酸性药物的情况下，ESP在高效液相色谱分析过程中的不稳定性问题。该方法根据国际人用药品注册技术协调会（ICH）、美国食品药品监督管理局（FDA）和美国药典（USP）的指南，在准确度、精密度、特异性、线性、溶液稳定性、稳健性、灵敏度和系统适用性方面进行了验证。该方法采用等度洗脱条件，流动相由缓冲液[氢氧化四丁基铵（0.0077 M）和正庚烷磺酸钠盐（0.002 M），pH 7.6]、乙腈和甲醇按60 : 20 : 20 v/v/v比例组成，流速为每分钟1.5 mL，在室温下通过C-18（十八烷基硅烷键合硅胶，5 µm，250×4.6 mm）色谱柱进行分离。两种药物的回收率均大于99%，证明了该方法的准确性。新方法的日内和日间精密度研究均低于最大允许限度[根据FDA，相对标准偏差（RSD）≤2.0%]。该方法对两种药物均显示出线性响应，相关系数（r²）值为0.999。更重要的是，在存在NPX的情况下，ESP在稀释溶剂和流动相中超过3天相当稳定。因此，该方法被认为是一种准确、可重现、灵敏且具有高度稳定性指示功能的方法，可成功应用于药物剂型中NPX和ESP同时测定的常规分析。
