HPLC分离阿立哌唑有关物质的方法学研究

 目的　建立阿立哌唑有关物质分离的HPLC。方法　采用反相C₈色谱柱,在室温条件下,以甲醇-1.5 %三乙胺(用醋酸调节pH5.6)(80∶20 )为流动相,流速为1mL·min^-1,检测波长为257nm,进样体积10μL。结果　阿立哌唑与中间体Ⅰ、中间体Ⅱ及其降解产物均能较好的分离,理论板数大于4200,且线性良好(r分别为0.9990,0.9996,0.9998)。中间体Ⅰ和中间体Ⅱ的最低检测限分别为3.0和3.3ng。日内、日间RSD分别为2.3%和3.1%。结论　本法可有效分离阿立哌唑有关物质及降解产物,灵敏度高 ,专属性强 ,可用于阿立哌唑有关物质及降解产物检查。

Study on a high-performance liquid chromatographic method for the separation of substances related to aripiprazole

OBJECTIVE To establish a high performance liquid chromatographic method for the separation of substances related to aripiprazole with UV detection. METHODS The chromatographic column of Inertsil C₈-3 was used The mobile phase consisted of methanol 1.5% triethylamine (80∶20, adjusted to pH 5.6 with acetic acid) and the flow rate was 1.0 mL·min^-1.The detection wavelength was at 257nm.RESULTS Aripiprazole,intermediateⅠ,Ⅱand degradation products were separated. The calibration curves of aripiprazole, intermediateⅠ and Ⅱ were linear (r=0.9990,0.9996,0.9998). The detection limits were 3.0 ng for intermediateⅠand 3.3 ng for intermediateⅡ, respectively. Good results were obtained for the within day and day to day validation(2.3% and 3.1%, respectively).CONCLUSION The method was proved to be sensitive and selective for the separation of aripiprazole It may be applied in pharmaceutical preparations for the examination of the impurities and degradation products.