National Center for Natural Products Research, Research Institute of Pharmaceutical Sciences, The University of Mississippi, MS 38677, USA.
J Pharm Biomed Anal. 2011 Dec 15;56(5):895-903. doi: 10.1016/j.jpba.2011.07.028. Epub 2011 Jul 29.
Analytical methods including HPLC, UPLC and HPTLC are presented for the determination of major alkaloid and triterpene saponins from the roots of Caulophyllum thalictroides (L.) Michx. (blue cohosh) and dietary supplements claiming to contain blue cohosh. A separation by LC was achieved using a reversed phase column, PDA with ELS detection, and ammonium acetate/acetonitrile gradient as the mobile phase. Owing to their low UV absorption, the triterpene saponins were detected by evaporative light scattering. The eight triterpene saponins (cauloside H, leonticin D, cauloside G, cauloside D, cauloside B, cauloside C, cauloside A and saponin PE) and the alkaloid magnoflorine could be separated within 35 min using HPLC method and within 8.0 min using UPLC method with detection limits of 10 μg/mL for saponins and 1 μg/mL for magnoflorine. The detection wavelength was 320 nm for magnoflorine and ELS detection was used for the eight saponins. The methods were also successfully applied to analyze different dietary supplements. For the products claiming to contain blue cohosh, there was a significant variability in the amounts of triterpene saponins detected. Calculations based on the analysis results for dietary supplements showed that maximum daily intake of alkaloid and saponins vary with the form (solids/liquids) and recommended doses according to the products label. Intakes varied from 0.57 to 15.8 mg/day for magnoflorine and from 5.97 to 302.4 mg/day for total saponins. LC-mass spectrometry coupled with electrospray ionization (ESI) method is described for the identification and confirmation of nine compounds in plant samples and dietary products. A HPTLC method was also developed for the fast chemical fingerprint analysis of C. thalictroides samples.
分析方法包括 HPLC、UPLC 和 HPTLC，用于测定 Caulophyllum thalictroides (L.) Michx.（蓝升麻）根中的主要生物碱和三萜皂苷以及声称含有蓝升麻的膳食补充剂。通过 LC 分离使用反相柱、PDA 与 ELS 检测以及作为流动相的乙酸铵/乙腈梯度来实现。由于它们的紫外吸收较低，三萜皂苷通过蒸发光散射检测。八种三萜皂苷（长春苷 H、莱菔素 D、长春苷 G、长春苷 D、长春苷 B、长春苷 C、长春苷 A 和皂苷 PE）和生物碱 Magnoflorine 可以在 35 分钟内使用 HPLC 方法分离，在 8.0 分钟内使用 UPLC 方法分离，检测限为 10 μg/mL 皂苷和 1 μg/mL Magnoflorine。Magnoflorine 的检测波长为 320nm，八种皂苷使用 ELS 检测。这些方法还成功应用于分析不同的膳食补充剂。对于声称含有蓝升麻的产品，检测到的三萜皂苷含量存在显著差异。基于膳食补充剂分析结果的计算表明，生物碱和皂苷的最大日摄入量随产品标签上的形式（固体/液体）和推荐剂量而变化。Magnoflorine 的摄入量从 0.57 到 15.8mg/天不等，总皂苷的摄入量从 5.97 到 302.4mg/天不等。描述了 LC-质谱法结合电喷雾电离（ESI）方法，用于鉴定和确认植物样品和膳食产品中的九种化合物。还开发了一种 HPTLC 方法用于快速分析 C. thalictroides 样品的化学指纹图谱。
