摘要
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 an HPLC method for the quantitative determination of roflumilast in the presence of degradation products,and to identify the structures of main degradation impurities. Methods： A C18 （125 mm×4.0 mm,5 μm） column was adopted with a mobile phase of phosphate buffer and acetonitrile at the flow rate of 1.0 mL·min-1 and detected at 247 nm. Results： An excellent separation was achieved for roflumilast and its related substances. The LOQ and LOD were 0.24 μg·mL-1 and 0.07 μg·mL-1,respectively. A linear response （r=0.9999） was observed for samples ranging from 10 to 180 μg·mL-1. The structures of degradation products under acidity,alkaline and oxidative conditions were identified,too. Conclusion： The method is shown to be simple,precise,accurate and can be applied to the determination of roflumilast.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2013年第10期1726-1730,共5页
Chinese Journal of Pharmaceutical Analysis
