HPLC分离西沙必利有关物质的方法学研究  

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

作　　者：闫小燕[1] 胡欣[1] 曹国颖[1] 何笑蓉[1] 宋友华[1] 傅得兴[1] 

机构地区：[1]卫生部北京医院药剂科,北京100730

出　　处：《中国药学杂志》2001年第3期186-188,共3页Chinese Pharmaceutical Journal

摘　　要：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 1.0mL·min-1进行线性梯度洗脱 ,以 (A)乙腈 (B) 0 .0 5mol·L-1磷酸盐缓冲液 (pH7.5 )组成流动相 ,检测波长为 2 75nm ,进样量 10 μL或 2 0 μL。 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 .0 2 5 μg·mL-1,有关物质Ⅱ为 0 .0 5 μg·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 。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 10 μL or 20 μL.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 -1 for 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.

关 键 词：西沙必利 有关物质 高效液相色谱法 梯度洗脱 HPLC 促胃肠动力药 稳定性 

分 类 号：R975[医药卫生—药品] R927.11[医药卫生—药学]