Department of Quality Assurance, Anand Pharmacy College, Anand, India.
J Food Drug Anal. 2016 Jul;24(3):610-619. doi: 10.1016/j.jfda.2016.02.011. Epub 2016 Apr 11.
A high-performance thin-layer chromatographic method for simultaneous determination of nadifloxacin, mometasone furoate, and miconazole nitrate was developed and validated as per International Conference on Harmonization guidelines. High-performance thin-layer chromatographic separation was performed on aluminum plates precoated with silica gel 60F and methanol:ethyl acetate:toluene: acetonitrile:3M ammonium formate in water (1:2.5:6.0:0.3:0.2, % v/v) as optimized mobile phase at detection wavelength of 224 nm. The retardation factor (R) values for nadifloxacin, mometasone furoate, and miconazole nitrate were 0.23, 0.70, and 0.59, respectively. Percent recoveries in terms of accuracy for the marketed formulation were found to be 98.35-99.76%, 99.36-99.65%, and 99.16-100.25% for nadifloxacin, mometasone furoate, and miconazole nitrate, respectively. The pooled percent relative standard deviation for repeatability and intermediate precision studies was found to be < 2% for three target analytes. The effect of four independent variables, methanol content in total mobile phase, wavelength, chamber saturation time, and solvent front, was evaluated by fractional factorial design for robustness testing. Amongst all four factors, volume of methanol in mobile phase appeared to have a possibly significant effect on retention factor of miconazole nitrate compared with the other two drugs nadifloxacin and mometasone furoate, and therefore it was important to be carefully controlled. In summary, a novel, simple, accurate, reproducible, and robust high-performance thin-layer chromatographic method was developed, which would be of use in quality control of these cream formulations.
开发并验证了一种用于同时测定那氟沙星、莫米松糠酸酯和硝酸咪康唑的高效薄层色谱法，符合国际协调会议的指导原则。高效薄层色谱分离在预先涂有硅胶 60F 的铝板上进行，甲醇：乙酸乙酯：甲苯：乙腈：3M 甲酸铵在水中（1:2.5:6.0:0.3:0.2，%v/v）为优化的流动相，检测波长为 224nm。那氟沙星、莫米松糠酸酯和硝酸咪康唑的延迟因子（R）值分别为 0.23、0.70 和 0.59。市售制剂的准确度回收率分别为 98.35-99.76%、99.36-99.65%和 99.16-100.25%，用于那氟沙星、莫米松糠酸酯和硝酸咪康唑。重复性和中间精密度研究的汇总相对标准偏差（RSD）对于三个目标分析物均<2%。通过部分因子设计评估了四个独立变量（总流动相中甲醇的含量、波长、腔室饱和时间和溶剂前沿）对稳健性测试的影响。在所有四个因素中，与其他两种药物那氟沙星和莫米松糠酸酯相比，流动相中甲醇的体积似乎对硝酸咪康唑的保留因子有显著影响，因此需要仔细控制。总之，开发了一种新颖、简单、准确、重现性和稳健的高效薄层色谱法，可用于这些乳膏制剂的质量控制。
