Shrimaan Sureshdada Jain College of Pharmacy, Chandwad, Nashik 423101, India.
GES's Sir Dr. M.S. Gosavi College of Pharmaceutical Education and Research, Nashik 422005, India.
J Chromatogr Sci. 2024 Mar 23;62(3):273-280. doi: 10.1093/chromsci/bmad039.
The goal of this study is to provide a single, widely applicable high-performance liquid chromatographic (HPLC) technique for the determination of related substances in multicomponent oral solution of promethazine hydrochloride and dextromethorphan hydrobromide. For the assessment of impurities of promethazine hydrochloride and dextromethorphan hydrobromide in oral solution, a unique, sensitive, quick, stability-indicating gradient HPLC technique has been created. For chromatographic separation, an Agilent Eclipse XDB-C18, 250 mm × 4.6 mm, 5 μm column was used with a buffered mobile phase consisting of a mixture of potassium dihydrogen phosphate pH 3.0:acetonitrile (80:20) v/v as mobile phase A and potassium dihydrogen phosphate pH 3.0:acetonitrile:methanol (10:10:80) v/v/v as mobile phase B. The separation was performed at a flow rate of 1.2 mL/min and a detection wavelength of 224 nm. The temperature of the column oven was regulated at 40°C. With good sensitivity and resolution, all compounds were effectively separated on a reverse-phase HPLC column. Acid, base, photolytic, thermal, oxidative and humidity stress conditions significantly degraded dextromethorphan hydrobromide and promethazine hydrochloride. The developed technique was validated according to the criteria of the International Conference on Harmonization for all validation parameters such as specificity, accuracy, linearity, precision, the limit of detection, the limit of quantitation and robustness.
本研究的目的是提供一种单一的、普遍适用的高效液相色谱（HPLC）技术，用于测定盐酸异丙嗪和氢溴酸右美沙芬多组分口服溶液中的有关物质。为了评估盐酸异丙嗪和氢溴酸右美沙芬口服溶液中的杂质，我们开发了一种独特的、灵敏的、快速的、具有稳定性指示的梯度 HPLC 技术。对于色谱分离，使用了 Agilent Eclipse XDB-C18，250mm×4.6mm，5μm 柱，以缓冲的流动相作为流动相 A，流动相 A 由磷酸二氢钾 pH 3.0：乙腈（80:20）v/v 组成，以磷酸二氢钾 pH 3.0：乙腈：甲醇（10:10:80）v/v/v 作为流动相 B。分离在流速为 1.2mL/min 和检测波长为 224nm 的条件下进行。柱温箱温度设定为 40°C。在反相 HPLC 柱上，所有化合物均能有效分离，具有良好的灵敏度和分辨率。酸、碱、光解、热、氧化和湿度应激条件显著降解了氢溴酸右美沙芬和盐酸异丙嗪。所开发的技术根据国际协调会议的标准进行了验证，所有验证参数如专属性、准确性、线性、精密度、检测限、定量限和耐用性均符合要求。
