高效液相色谱法测定盐酸伐地那非原料药中的有关物质

Determination of related substances in Vardenafil hydrochloride by HPLC

目的建立高效液相色谱法(HPLC)测定盐酸伐地那非中的有关物质。方法采用反相HPLC,色谱柱为Agilent HC-C18(2),流动相A为0.5%三乙胺溶液(用磷酸调节pH至3.0)-乙腈(90∶10),流动相B为0.5%三乙胺溶液(用磷酸调节pH至3.0)-乙腈(10∶90),梯度洗脱,检测波长242 nm,以外标法计算已知杂质的含量,主成分自身对照法计算未知杂质的含量。结果盐酸伐地那非和杂质A、B、C、D、E、F、G 7个已知杂质的分离度均符合要求(≥1.5);盐酸伐地那非与7个杂质的浓度与峰面积呈良好的线性关系,相关系数均在0.998以上;杂质A、B、C、D、E、F、G杂质的平均回收率分别为99.8%、101.6%、102.4%、99.5%、100.5%、101.7%、103.6%,在99.5%~103.6%范围内,RSD分别为1.8%、0.6%、1.2%、1.4%、0.9%、1.5%、0.9%,均<2%。结论该方法准确、灵敏、精密度良好,可定量分析7个工艺杂质和降解杂质,可作为盐酸伐地那非原料有关物质的检测方法。

Objective To establish HPLC method for the determination of the related substances in Vardenafil hydrochloride.Methods An RP-HPLC method was used,the column was Agilent HC-C18(2),the mobile phase A was 0.5%triethylamine solution(adjustedto pH 3.0 with phosphoric acid)-acetonitrile(90:10),the mobile phase B was 0.5%triethylamine solution(adjusted to pH 3.0 with phosphoric acid)-acetonitrile(10:90),gradient elution,detection wavelength 242 nm.The content of known impurities was calculated by externalstandard method,and the content of unknown impurities was calculated by principal component self-control method.Results The separation of Vardenafil hydrochloride and seven known impurities A,B,C,D,E,F and G all met the requirements(≥1.5);there was a good linearrelationship between the concentration and peak area of vardenafil hydrochloride and seven impurities,and the correlation coefficientswere all above 0.998;The average recoveries of impurities A,B,C,D,E,F and G were 99.8%,101.6%,102.4%,99.5%,100.5%,101.7%and 103.6%,respectively.Within the range of 99.5%-103.6%,RSD were 1.8%,0.6%,1.2%,1.4%,0.9%,1.5%and 0.9%,respectively,all less than 2%.Conclusion The method is accurate,sensitive and precise.It can be used for the quantitative analysis of seven processimpurities and degradation impurities.It can be used for the determination of related substances in vardenafil hydrochloride.