中药通光藤中通光藤苷J的高效毛细管电泳分析

Determination of tenacissosides J in Marsdenia tenacissima by capillary zone electrophoresis

目的:建立中药通光藤中通光藤苷J的高效毛细管电泳(CZE)分析方法。方法:使用空心熔融石英毛细管(75μm×47 cm),用苯甲酸为内标,背景电解质为含20％乙腈的50 mmol/L硼砂缓冲液(pH 9.28),运行电压20 kV,温度25 C,重力进样,时间5 s,紫外检测波长214 nm,两次进样间用0.1 mol/L氢氧化钠溶液冲柱1 min,以水冲柱1min,再用电解液冲柱1min。结果:在15 min内可实现通光藤苷J的分离和测定,在43.43～1732.06 μg/ml范围内线性关系良好(r=0.998 5,n=6);加样回收率98.1％～104.7％,平均102.4％;日内RSD≤2.50％和日间 RSD≤5.16％;不同产地(云南昆明 X_1～X_4、贵州贞丰X_5)、不同化学部位(乙醚部位、乙酸乙酯部位、正丁醇部位、50％乙醇部位、95％乙醇部位)和不同制剂(片剂、糖浆、注射液)中通光藤苷J的含量均有显著不同。结论:本法简便、快速、准确,为科学评价通光藤药材质量提供了有效手段。

Objective; To determine the contents of tenacissosides J in Marsdenia tenacissima by capillary zone elec-trophoresis(CZE). Methods:Using benzoic acid as the internal standard (IS), the electrophoretic separation was achieved with 20% acetonitrile in 50 mmol/L borate buffer (pH 9. 28) as the running buffer and a voltage of 20 kV was applied to the 47 cm× 75 μm (ID) capillary. The analysis were introduced into capillary by siphon (5 s) and determined with on-column UV monitoring at 214 nm. Results: The determination could be completed within 15 min and the analytical results of samples demonstrated a good linear relationship within 43. 43-1 732. 06 μg/ml. The relative standard deviation (RSD) of intra-day was less than 2. 50% and that of inter-day was less 5. 16%. The recoveries were 98. 1%-104. 7%. Conclusion:CZE is accurate, simple and reliable,which can be applied to determine tenacissosides J in Marsdenia tenacissima.