三白草中蜥尾草亭A和B的分离鉴定及其含量测定

目的：建立一种基于高效液相色谱同时测定三白草中蜥尾草亭（manassantin）A（MA）和B（MB）含量的方法，并对三白草不同部位的MA和MB含量进行比较。方法：采用硅胶柱色谱法和高效液相制备色谱法从三白草根中分离并鉴定MA和MB；采用高效液相色谱法测定含量，以Kromasil C₁₈色谱柱（250 mm×4.6 mm，5 μm）进行色谱分离，柱温25℃，流动相为甲醇-乙腈（1∶1）和水，梯度洗脱，流速1.0 mL·min^-1，检测波长280 nm。结果：MA和MB质量浓度均在0.001~0.051 mg·mL^-1范围内线性关系良好，相关系数分别为0.999 2和0.999 9；日内RSD分别为1.8%和1.5%；平均回收率（n=3）在96.2%~104.8%。3批不同部位三白草样品中MA含量：花序0.135%~0.138%，根0.079%~0.080%，叶0.082%~0.083%，茎0.034%；MB含量：花序0.118%~0.119%，叶0.083%~0.084%，根0.064%，茎0.038%。结论：本法适用于三白草中MA和MB的含量测定，亦为从植物原料中靶向性地高效制备MA和MB提供了技术支持。

Objective:To establish a method for simultaneous determination of manassantin A (MA) and B (MB) in Saururus chinensis by high performance liquid chromatography (HPLC),and to compare the contents of MA and MB in different parts of S. chinensis. Methods:MA and MB were isolated from the rhizomes of S. chinensis by using silica column and preparative high-performance liquid chromatography,followed by structure identification. The determination was performed on a C₁₈ (250 mm×4.6 mm,5 μm) column at 25. The mobile phase was composed of methanol-acetonitrile (1:1) and water with gradient elution at a flow rate of 1.0 mL·min^-1. The detected wavelength was set at 280 nm. Results:The calibration curves of MA and MB were both in a good linearity within the range of 0.001-0.051 mg·mL^-1,and the correlation coefficients were 0.999 2 for MA and 0.999 9 for MB. The RSD values for intraday precision were 1.8% and 1.5%,respectively. And the average recoveries (n=3) were in the range of 96.2%-104.8%. The contents of MA in different parts of 3 batches of S. chinensis samples were 0.135%-0.138% in inflorescence,0.079%-0.080% in rhizomes,0.082%-0.083% in leaves and 0.034% in stems;while the contents of MB were 0.118%-0.119% in inflorescence,0.083%-0.084% in leaves,0.064% in rhizomes and 0.038% in stems. Conclusion:The method established in the current study was suitable for the determination of MA and MB in S. chinensis,which should facilitate the targeted isolation and preparation of MA and MB from raw materials.