烟台大学学报（自然科学与工程版）2017，Vol.30Issue(2)：117-123,7.DOI:10.13951/j.cnki.37-1213/n.2017.02.007
非水毛细管电泳法测定利培酮原料药有关物质
Non-aqueous Capillary Electrophoresis for Determination RelatedSubstances of Risperidone Raw Material
摘要
Abstract
A non-aqueous capillary electrophoresis method is established for the determination of risperidone related substances.The single factor experiment combined with response surface methodology is used to optimize the conditions of capillary electrophoresis system of risperidone and its impurities separation methods.The optimal conditions for electrophoresis are as follows: uncoated silica capillary column (38.5 cm×50 μm), 200 mmol/L Tris-150 mmol/L Cit in methanol as buffer, the separation voltage of 25 kV, the separation temperature of 20 °C, the detection wavelength of 260 nm, the injection pressure of 50 mbar and the injection time of 5 s.The proposed method is validated by assessing the precision, linearity, limit of detection, limit of quantitation, accuracy and stability.The results show that risperidone and its impurities can basically fulfill the baseline separation.The impurities labeled as A, B, C, D, E, H, K and G are linear in the corresponding concentration range(r>0.9990, n=6).The detection limits for impurities of A, B, C, D, E, H, K and G are 0.31, 0.29, 0.23, 0.28, 0.26, 0.38, 0.25 and 0.23 μg/mL, respectively;their respective quantification limits are 0.91, 0.90, 0.82, 0.88, 0.85, 0.96, 0.84 and 0.81 μg/mL, and the average recovery rates are in the range of 96.5%-108.3%.The relative standard deviation value for migration time and the ratio of peak area of intra-assay and inter-assay are less than 3.0%.It is beneficial for determination of risperidone related substances, and the results demonstrate that the method is less solvent consumption, simple, rapid and accurate.关键词
非水毛细管电泳/利培酮原料药/有关物质/响应面分析法Key words
non-aqueous capillary electrophoresis(NACE)/risperidone/impurity/response surface methodology分类
医药卫生引用本文复制引用
谭燕美,宫菲菲,董敏,由春娜,刘万卉..非水毛细管电泳法测定利培酮原料药有关物质[J].烟台大学学报（自然科学与工程版）,2017,30(2):117-123,7.基金项目
国家"重大新药创新"科技重大专项资助项目(2013ZX09402201). （2013ZX09402201）
