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目的:建立以高效液相色谱法测定罗氟司特中有关物质含量,并对主要降解杂质进行结构确证。方法:采用C18色谱柱(125.0 mm×4.0 mm,5μm),以磷酸盐缓冲液和乙腈为流动相,梯度洗脱,流速1.0 mL·min-1,检测波长247 nm。结果:线性范围为10～180μg·mL-1(r=0.9999,n=7),定量限为0.24μg·mL-1,检测限为0.07μg·mL-1。确定了酸、碱及氧化条件下主要降解产物的结构。结论:该方法准确、可行,精密度高,可用于罗氟司特有关物质的鉴定和含量测定。
OBJECTIVE: To establish a method for the determination of related substances in roflumilast by high performance liquid chromatography (HPLC) and to confirm the structure of the major degradation impurities. Methods: The mobile phase consisted of C18 column (125.0 mm × 4.0 mm, 5 μm), phosphate buffer and acetonitrile with a gradient of 1.0 mL · min-1 and a detection wavelength of 247 nm. Results: The linear range was 10-180μg · mL-1 (r = 0.9999, n = 7). The limit of quantification was 0.24μg · mL-1 and the limit of detection was 0.07μg · mL-1. The structure of major degradation products under acid, alkali and oxidation conditions was determined. Conclusion: The method is accurate, feasible and accurate. It can be used for the identification and determination of roflumilast related substances.