论文部分内容阅读
目的建立罗氟司特起始原料(4-二氟甲氧基-3-羟基苯甲醛)中的杂质控制方法。方法采用Vision HT C18柱(250 mm×4.6 mm,5μm),甲醇-0.01 mol·L-1磷酸二氢钾溶液(40∶60)为流动相,检测波长254 nm,柱温30℃,进样体积20μL。结果样品的线性范围为0.1028~0.6168μg·ml-1(r=0.999),平均回收率为99.75%,RSD=0.57%。结论所用方法能有效地控制4-二氟甲氧基-3-羟基苯甲醛中的3,4-二羟基苯甲醛杂质,可得到高纯度的罗氟司特。
OBJECTIVE To establish an impurity control method in roflumilast starting material (4-difluoromethoxy-3-hydroxybenzaldehyde). Methods The mobile phase consisted of a Vision HT C18 column (250 mm × 4.6 mm, 5 μm), methanol-0.01 mol·L-1 potassium dihydrogen phosphate solution (40:60), detection wavelength 254 nm and column temperature 30 ℃. Volume 20μL. Results The linear range of the sample was 0.1028-0.6168μg · ml-1 (r = 0.999). The average recovery was 99.75% and the RSD was 0.57%. Conclusion The method used can effectively control 3,4-dihydroxybenzaldehyde impurity in 4-difluoromethoxy-3-hydroxybenzaldehyde and obtain high purity roflumilast.