HPLC分离阿立哌唑有关物质的方法学研究

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

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pH 5 6 ) (80∶2 0 )为流动相 ,流速为 1mL·min-1,检测波长为 2 5 7nm ,进样体积 10 μL。 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 4 2 0 0 ,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 。

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&middotmin-1. The detection wavelength was at 257 nm. RESULTS: Aripiprazole, intermediate I, II and degradation products were separated. The calibration curves of aripiprazole, intermediate I and II were linear (r = 0.999 0, 0.999 6, 0.999 8). The detection limits were 3.0 ng for intermediate I and 3.3 ng for intermediate II, 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.