HPLC分离西沙必利有关物质的方法学研究

 目的建立西沙必利有关物质分离的HPLC方法。方法采用二元泵，在室温下以流速1.0 mL·min-1进行线性梯度洗脱，以(A)乙腈(B)0.05 mol·L-1磷酸盐缓冲液(pH7.5)组成流动相，检测波长为275 nm，进样量10μL或20μL。结果与氟哌啶醇分离度＞3，西沙必利、有关物质Ⅰ和有关物质Ⅱ线性良好(r=0.999)。最小检出量有关物质Ⅰ为0.025μg·mL-1，有关物质Ⅱ为0.05μg·mL-1，日内日间差异分别为6.9%和6.6%。结论本法灵敏、专属，可有效分离有关物质及降解产物，可用于有关物质及降解产物检查。

Study on a high-pressure liquid chromatographic method for the separation of substances related to cisapride

OBJECTIVE To study a high pressure liquid chromatographic method for the separation of substances related to cisapride with UV detection.METHOD The analyses were performed using a high pressure double pump at room temperature by a linear gradient elution.The flow rate was 1.0 mL·min-1.The mobile phase was consisted of (A) acetonitrile and (B) phosphate buffer (0.05 mol·L-1,pH7.5).The monitoring wavelength was 275 nm.The injection volume was 10μL or 20μL.RESULTS The resolution factor between the peaks due to cisapride and haloperidol was at least 3.0.The calibration curves of cisapride,related substance Ⅰ and related substance Ⅱ were all linear (r=0.999).The detection limits were 0.025 μg·mL-1for related substance Ⅰ and 0.05 μg·mL-1 for related substance Ⅱ respectively.good results were obtained for the day to day and within day reproducibilities (6.9% and 6.6%,respectively).CONCLUSION The method was proved to be sensitive and selective for the separation of the available impurites from cisapride and from each other.It may be applied to analyze in pharmaceutical preparations for the examination of the impurities and degradation products.