高效液相色谱法测定罗氟司特药品中罗氟司特和4种杂质
HPLC Determination of Roflumilast and 4 Impurities in Roflumilast Drug
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摘要: 提出了高效液相色谱法测定罗氟司特药品中罗氟司特和4种杂质.样品以乙腈溶解,采用Welch Ultimate XB-C18色谱柱为分离柱,以0.01 mol·L-1磷酸氢二钾溶液(用磷酸调节pH为4.0)与乙腈以体积比50比50组成的混合溶液为流动相,在检测波长215 nm处进行测定.罗氟司特和4种杂质在一定的质量浓度范围内与其峰面积呈线性关系.方法的测定下限(10S/N)在0.04~0.22 ng之间.加标回收率在101%~102%之间,测定值的相对标准偏差(n=9)均小于2.0%.Abstract: HPLC was applied to the determination of Roflumilast and 4 impurities in Roflumilast drug.The sample was dissolved with acetonitrile.Welch Ultimate XB-C18 chromatographic column was used as stationary phase,and a mixture of 0.01 mol·L-1 K2HPO4 solution (adjusted pH to 4 with phosphoric acid) and acetonitrile (50+50) was used as mobile phase.UV-detection at 215 nm was adopted in the determination.Linear relationships between values of peak area and mass concentration of Roflumilast and the 4 impurities were kept in definite ranges.Low limits of determination (10S/N) found were ranged from 0.04 to 0.22 ng.Values of recovery found by standard addition method were in the range of 101%-102%,and values of RSD′s (n=9) less than 2.0%.