一种用于检测麦考酚钠含量及有关物质的高效液相色谱法

High performance liquid chromatography for the determination of mycophenolate sodium and related substances

目的:建立一种HPLC法用于麦考酚钠的含量及有关物质的测定。方法:采用MACHEREY-NA⁃GEL EC 250/3 NUCLEOSIL 100-5 C18(250 mm×3 mm,5μm)色谱柱,Welch Ghost-Buster(4.6 mm×50 mm)为鬼峰捕集小柱,以磷酸二氢钾缓冲盐(磷酸调pH至2.0)为流动相A,乙腈为流动相B,流速0.8 mL/min梯度洗脱,检测波长为216 nm,柱温为50℃。结果:麦考酚钠的检测限为0.008 g/mL,定量限为0.025 g/mL,麦考酚钠和杂质B在0.024~120 g/mL与峰面积线性关系良好,相关系数r均不小于0.999(n=5),麦考酚钠的回收率为100%,杂质B的回收率为102%。结论:该方法操作简单,重复性较好,适用于麦考酚钠含量及有关物质的测定。

Objective:To establish a HPLC method for the determination of mycophenolate sodium and related substances.Methods:MACHEREY-NAGELEC 250/3NUCLEOSIL 100-5C18(250mm×3mm,5μm)chromatographic column was used,Welch Ghost-Buster(4.6 mm×50 mm)was used as trap column,potassium dihydrogen phosphate buffer salt(adjusted to pH 2.0 by phosphoric acid)was used as mobile phase A,acetonitrile was used as mobile phase B,and elution was conducted with the flow rate of 0.8 mL/min gradient.The detection wavelength was 216 nm.Results:The detection limit of mycophenolate sodium was 0.008 g/mL,the quantitation limit was 0.025 g/mL,the linear relationship between mycophenolate sodium and impurity B was good at 0.024-120 g/mL,the correlation coefficient r was not less than 0.999(n=5),the recovery of mycophenolate sodium was 100%,and the recovery of impurity B was 102%.Conclusion:This method is simple,reproducible and suitable for the determination of mycophenolate sodium and related substances.