罗氟司特中有关物质的鉴定和含量测定

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,5 μm),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10~180 μg·mL^-1(r=0.9999,n=7),定量限为0.24 μg·mL^-1,检测限为0.07 μg·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.

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