吗替麦考酚酯胶囊含量和有关物质的测定

Determination of mycophenolate mofetil and related substances in mycophenolate mofetil capsules by RP-HPLC

目的采用反相高效液相色谱法建立吗替麦考酚酯胶囊的有关物质测定法。方法色谱柱symmetry C18150*4.6mm,流动相为:乙腈-水-三乙胺磷酸缓冲液(取三乙胺10mL,加水990mL,混匀,磷酸调节pH值至5.4±0.1)(40∶40∶20);流速:1.0mL·min-1,检测波长为249nm;柱温45℃。结果制剂中辅料对主药测定无干扰,吗替麦考酚酯在60.2μg^602.4μg.mL-1浓度范围内,峰面积与浓度线性关系良好,相关系数r=0.99995;平均回收率为99.9%,变异系数为1.4%。溶液在冷藏5℃条件下,4h内稳定,24h降解产物明显增加,因此供试品溶液宜现配现用;麦考酚酸在4.6μg^46.05μg.mL-1范围内R=0.99995;平均回收率为98.5%;精密度测定变异系数为:0.46%。结论本法简便,准确,专属性强,可用于吗替麦考酚酯胶囊的有关物质检查和含量测定。

OBJECTIVE To establish a practical method of RP-HPLC for the determination of Mycophenolate Mofetil and related substance in Mycophenolate Mofetil Capsules.METHODS A RP-HPLC method was developed.Chromatographic condition included a symmetry C18 150×4.6mm column with mobile phase of Acetontril：water：triethylamine phosphate buffer solution（pH=5.4±0.1）（40∶40∶20）,the column temperature was 45℃ with the flow rate of 1.0 mL·min-1 and the detection wavelength of 249 nm.RESULTS The linear range of mycophenolate mofetil was 60.2μg～602.4μg·mL-1（r=0.99995）,The average recovery rate was 99.9%,RSD=1.4%.Solution at 5℃ cold storage conditions,the stability of 4 hours,24 hours a marked increase in degradation products,So injection the test solution of preparation to use;Results the linear range of Mycophenolate acid was 4.6μg～46.05μg·mL-1（r=0.99995）,The average recovery rate was 98.5%,RSD=0.46%.CONCLUSION This simple and reliable method is applied to determine assay and related substance of Mycophenolate Mofetil Capsules.