高效液相色谱法测定尼群地平中3种杂质

Determination of three impurities in nitrendipine by high performance liquid chromatography

建立高效液相色谱法同时测定尼群地平原料中杂质A、B、C含量的分析方法。采用以十八烷基硅烷键合硅胶为填料的Agilent ZORBOX Eclipse XDB C;柱(250 mm×4.6 mm,5 μm),以乙腈–四氢呋喃–水(体积比为20∶24∶56)为流动相,等度洗脱,流量为1 mL/min,柱温为40 ℃,检测波长为235 nm。结果表明,尼群地平与各杂质峰相互之间分离良好,杂质A、B、C在相应的质量浓度范围内与色谱峰面积具有良好的线性关系,相关系数均大于0.999,检出限为0.152~0.171 ng,定量限为0.494~0.512 ng。平均加标回收率为92.38%~93.07%,测定结果的相对标准偏差小于2%(n=6)。该方法较为稳定,测定时不受溶剂等因素影响,可用于对尼群地平中3种杂质进行控制。

A method for simultaneous determination of impurities A,B and C in nitrendipine raw materials by high performance liquid chromatography was established.Agilent ZORBOX Eclipse XDB C;column(250 mm×4.6 mm,5 μm) with octadecylsilane bonded silica gel as filler was used.Acetonitrile tetrahydrofuran water(The volumeratio was 20∶24∶56) was used as the mobile phase.The flow rate was 1 mL/min,the column temperature was 40 ℃,andthe detection wavelength was 235 nm.The results showed that nitrendipine was well separated from each impurity peak,impurities A,B and C had a good linear relationship with the chromatographic peak area in the corresponding mass concentration range,and the correlation coefficients were more than 0.999.The detection limits were 0.152–0.171 ng and the quantitative limits were 0.494–0.512 ng.The average recoveries were 92.38%–93.07%,and the relative standard deviations were less than 2%(n=6).The method is stable and not affected by solvent and other factors.It can be used to control three impurities in nitrendipine.