HPLC分离西沙必利有关物质的方法学研究

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)0.05mol·L^-1磷酸盐缓冲液(pH7.5)组成流动相，检测波长为275nm，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。

关键词：西沙必利；有关物质；高效液相色谱法；梯度洗脱

分类号：R917　文献标识码：A
文章编号：1001-2494(2001)03-0186-03

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

YAN Xiao-yan（Beijing Hospital,Ministry of Public Health,Beijing 100730,China）　
HU Xin（Beijing Hospital,Ministry of Public Health,Beijing 100730,China）　
CAO Guo-ying（Beijing Hospital,Ministry of Public Health,Beijing 100730,China）　
HE Xiao-rong（Beijing Hospital,Ministry of Public Health,Beijing 100730,China）　
SONG You-hua（Beijing Hospital,Ministry of Public Health,Beijing 100730,China）　
FU De-xing（Beijing Hospital,Ministry of Public Health,Beijing 100730,China）　

Abstract：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·mL^-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.
Keywords：ciaspride;related substances;HPLC;gradient elution

参考文献：

［1］　　McCallum RW,Chakrapani Prakash,Campoli-Richards DM,et al.Cisapride a preliminary review of its pharmacodynamic and pharmacokinetic properties and therapeutic use as a prokinetic agent.in gastrointestinal disorders［J］.Drug,1988,36:652.
［2］　　BP(1993)［S］.Addendum,1996:196.
［3］　　Preechagoon Y,Charles BG.Analysis of cisapride in neonatal plasma using high-performance liquid chromatography with a base-stable column and fluorescence detection［J］.J Chomatography B,1995,670:139.
［4］　　Woestenborghs R,Lorreyen W,Rompaey F,et al.Determination of cisapride in plasma and animal tissues by high-performance liquid chromatography［J］.J Chomatography B,1988,424:195.

收稿日期：1999年7月20日

出版日期：2001年3月1日