高效液相色谱法测定咪唑立宾片的含量及有关物质

Determination of the related substance and content of Mizoribine Tablets by HPLC

建立高效液相色谱法测定咪唑立宾片的含量及有关物质。采用Venusil HILIC色谱柱(250 mm×4.6 mm,5μm),以0.03%磷酸溶液-乙腈(体积比为10∶90)为流动相,流量为1.0 mL/min,有关物质检测波长为220 nm,含量测定波长为279 nm,柱温为25℃。结果表明,咪唑立宾质量浓度和色谱峰面积在1.5~500μg/mL范围内线性良好,相关系数为0.999 9,平均回收率为99.9%,检出限为0.6μg/mL,定量限为1.5μg/mL。咪唑立宾与辅料和破坏实验产生的杂质峰均能达到良好的分离。所建立的方法专属性强、快速、灵敏,适用于测定咪唑立宾片的含量及有关物质。

A high performance liquid chromatography method was established to determine content of mizoribine and the related substance in mizoribine tablets.The method was carried out on Venusil HILIC column(250 mm×4.6 mm,5μm),phosphoric acid aqueous solution(0.3 mL/L)-acetonitrile(10/90)was used as mobile phase at a flow rate of 1.0 mL/min,the detection wavelength was 279 nm for mizoribine and 220 nm for related substance.The column temperature was 25℃.The results showed that the mass concentration of mizoribine had a good linear relationship with the chromatographic peak area in therange of 1.5-500μg/mL,and the correlation coefficient was 0.9999.The average recovery rate of the test sample was 99.9%.The LOD and LOQ were 0.6μg/mL and 1.5μg/mL,respectively.The separation of mizoribine from the impurities producted by the forced degradation was achieved.The established method is specific,rapid and sensitive,which is suitable for the determination of the related substance and content of mizoribine.