Yehia Ali Mohamed, Essam Hebatallah Mohamed
Department of Analytical Chemistry, Faculty of Pharmacy, Cairo University, Cairo, Egypt.
J Sep Sci. 2016 Sep;39(17):3357-67. doi: 10.1002/jssc.201600438. Epub 2016 Aug 11.
A generally applicable high-performance liquid chromatographic method for the qualitative and quantitative determination of pharmaceutical preparations containing phenylephrine hydrochloride, paracetamol, ephedrine hydrochloride, guaifenesin, doxylamine succinate, and dextromethorphan hydrobromide is developed. Optimization of chromatographic conditions was performed for the gradient elution using different buffer pH values, flow rates and two C18 stationary phases. The method was developed using a Kinetex® C18 column as a core-shell stationary phase with a gradient profile using buffer pH 5.0 and acetonitrile at 2.0 mL/min flow rate. Detection was carried out at 220 nm and linear calibrations were obtained for all components within the studied ranges. The method was fully validated in agreement with ICH guidelines. The proposed method is specific, accurate and precise (RSD% < 3%). Limits of detection are lower than 2.0 μg/mL. Qualitative and quantitative responses were evaluated using experimental design to assist the method robustness. The method was proved to be highly robust against 10% change in buffer pH and flow rate (RSD% < 10%), however, the flow rate may significantly influence the quantitative responses of phenylephrine, paracetamol, and doxylamine (RSD% > 10%). Satisfactory results were obtained for commercial combinations analyses. Statistical comparison between the proposed chromatographic and official methods revealed no significant difference.
开发了一种普遍适用的高效液相色谱法，用于定性和定量测定含有盐酸去氧肾上腺素、对乙酰氨基酚、盐酸麻黄碱、愈创甘油醚、琥珀酸多西拉敏和氢溴酸右美沙芬的药物制剂。使用不同的缓冲液pH值、流速和两种C18固定相，对梯度洗脱的色谱条件进行了优化。该方法以Kinetex® C18柱作为核壳固定相，采用缓冲液pH 5.0和乙腈，流速为2.0 mL/min的梯度洗脱曲线进行开发。在220 nm处进行检测，并在所研究的范围内获得了所有组分的线性校准曲线。该方法按照国际协调会议（ICH）指南进行了全面验证。所提出的方法具有特异性、准确性和精密度（相对标准偏差<3%）。检测限低于2.0 μg/mL。使用实验设计评估定性和定量响应，以提高方法的稳健性。结果表明，该方法对缓冲液pH值和流速10%的变化具有高度稳健性（相对标准偏差<10%），然而，流速可能会显著影响去氧肾上腺素、对乙酰氨基酚和多西拉敏的定量响应（相对标准偏差>10%）。对市售组合制剂的分析获得了满意的结果。所提出的色谱方法与官方方法之间的统计比较显示无显著差异。
