Department of Pharmaceutical Analytical Chemistry, Faculty of Pharmacy, University of Tanta, Tanta, Egypt.
J Pharm Biomed Anal. 2013 Sep;83:249-59. doi: 10.1016/j.jpba.2013.04.013. Epub 2013 Apr 19.
A simple, precise, rapid, stability-indicating reversed phase high performance liquid chromatographic method with photodiode array detection was developed and validated for the determination of mebeverine hydrochloride in combination with sulpiride or with diloxanide furoate and metronidazole in the presence of their corresponding degradation products. Optimum separation was achieved in less than 10 min using an X-Bridge C18 column (150 mm × 4.6 mm i.d., 3.5 μm particle size); elution was accomplished via the application of a dual-mode solvent and flow rate gradient system. This elution system enables the separation of nine components within a cycle time of 15 min and with a resolution greater than 2.5. Detection was conducted at 230 nm, and purity assessment was performed using a photodiode array detector. The method has been validated with respect to specificity, linearity, accuracy, precision, limit of quantitation, limit of detection, robustness and ruggedness. The validation criteria were met in all cases. The developed HPLC method was successfully applied to commercial tablets. It was shown that this method is very sensitive to the determination of the degradation products, downward to 0.1 w/w% levels, which is far below the limits for testing these degradation products within their corresponding intact drugs.
建立并验证了一种简单、准确、快速、具有稳定性指示的反相高效液相色谱法，并用光电二极管阵列检测，用于在相应降解产物存在的情况下同时测定盐酸美贝维林与舒必利，或与地美硝唑和甲硝唑的含量。采用 X-Bridge C18 柱（150mm×4.6mmID，3.5μm 粒径），在 10min 内即可完成最佳分离；通过应用双模式溶剂和流速梯度系统实现洗脱。该洗脱系统可在 15min 内完成 9 个成分的分离，且分辨率大于 2.5。在 230nm 处进行检测，并使用光电二极管阵列检测器进行纯度评估。该方法已针对专属性、线性、准确性、精密度、定量限、检测限、耐用性和重现性进行了验证。在所有情况下均符合验证标准。所开发的 HPLC 方法已成功应用于市售片剂。结果表明，该方法对降解产物的测定非常敏感，可检测至 0.1w/w%的水平，远低于在相应完整药物中测试这些降解产物的限度。
