高效液相色谱法测定氟伐他汀钠缓释片的有关物质

Determination of Related Substances in Fluvastatin Sodium Extended-release Tablets by HPLC

目的 建立氟伐他汀钠缓释片有关物质的高效液相色谱(HPLC)测定方法,为建立氟伐他汀钠缓释片的质量控制标准提供参考。方法 色谱柱为ZORBAX Eclipse Plus C18Rapid Resolution(75 mm×4.6 mm, 3.5μm);流动相A:pH值7.2缓冲液-甲醇乙腈混合液(体积比90:10),流动相B:pH值7.2缓冲液-甲醇乙腈混合液(体积比10:90),梯度洗脱;流速:2.0 mL·min^(-1);柱温:35℃;检测波长:305,365 nm;进样量:25μL。结果 主峰与各杂质峰均能达到完全分离;杂质A、B、C、D、E、F、G的检测限分别是0.069 5,0.032 5,0.059 3,0.074 0,0.050 3,0.048 6,0.026 3μg·mL^(-1),杂质A、B、C、D、E、F、G的定量限分别是0.2318,0.108 3,0.197 8,0.246 6,0.167 6,0.162 1,0.087 6μg·mL^(-1);在研究的浓度范围内与各自峰面积呈良好的线性关系,杂质A、B、C、D、E、F、G的线性浓度范围分别是0.231 8~6.0,0.108 3~1.2,0.197 8~1.2,0.246 6~3.0,0.167 6~1.2,0.162 1~3.0,0.087 6~1.2μg·mL^(-1);回收率89.8%~103.5%;供试品溶液在5℃中保存54 h稳定。结论 该方法简单、准确、可靠,能满足氟伐他汀钠缓释片有关物质的检测要求。

Objective To establish an HPLC method for determining related substances in fluvastatin sodium extended-release tablets and provide a basis for the specification of fluvastatin sodium extended-release tablets.Methods The analyte was gradient eluted on a C 18 column(ZORBAX Eclipse Plus C 18 Rapid Resolution,75 mm×4.6 mm,3.5μm)with mobile phase A pH 7.2 buffer and methanol-acetonitrile mixture(the volume ratio is 90:10)and mobile phase B pH 7.2 buffer and methanol-acetonitrile mixture(the volume ratio is 10:90).The flow rate was 2.0 mL·min^(-1).The column temperature was set at 35℃.The detective wavelengths were 305 nm and 365 nm,and the injection volume was 25μL.Results The impurity peaks were completely separated from the principal component peak.The detection limits for impurities A,B,C,D,E,F,and G were 0.0695,0.0325,0.0593,0.0740,0.0503,0.0486,and 0.0263μg·mL^(-1),respectively.The quantitation limits for impurities A,B,C,D,E,F,and G were 0.2318,0.1083,0.1978,0.2466,0.1676,0.1621 and 0.0876μg·mL^(-1) respectively.There was a good linear relationship between the concentration and peak area within the concentration range of the study,and the linearity concentration ranges of impurities A,B,C,D,E,F,and G were 0.2318-6.0,0.1083^(-1).2,0.1978^(-1).2,0.2466-3.0,0.1676^(-1).2,0.1621-3.0,0.0876^(-1).2μg·mL^(-1) respectively.The recovery was 89.8%^(-1)03.5%.The sample solution was stable in 54 h at 5℃.Conclusion The method is simple,accurate,and reliable for determining related substances in fluvastatin sodium extended-release tablets.