National Center for Natural Products Research, Research Institute of Pharmaceutical Sciences, The University of Mississippi, MS 38677, USA.
J Pharm Biomed Anal. 2010 Jun 5;52(2):173-80. doi: 10.1016/j.jpba.2010.01.010. Epub 2010 Jan 15.
This paper describes the first analytical method for the determination of four flavonoids (sutherlandins A-D) and four cycloartanol glycosides (sutherlandiosides A-D) from the aerial parts of Sutherlandia frutescens (L.) R. Br. A separation by HPLC was achieved by using a reversed phase (RP-18) column, PDA with ELS detection, and a water/acetonitrile gradient as the mobile phase. The wavelength used for quantification of four flavonoids with the diode array detector was 260 nm. Owing to their low UV absorption, the cycloartanol glycosides were detected by evaporative light scattering. The method was validated for linearity, repeatability, limits of detection (LOD) and limits of quantification (LOQ). The limits of detection and limits of quantification of eight compounds were found to be in the range from 0.1 to 7.5 microg/mL and 0.5 to 25 microg/mL, respectively. The analysis of products showed considerable variation of 1.099-5.224 mg/average weight for the major compound, sutherlandioside B. The eight compounds in plant sample and products of S. frutescens were further confirmed by LC-ESI-TOF. This method involved the use of the M+H and M+Na ions in the positive ion mode with extractive ion monitoring (EIM).
本文描述了从南非钩麻（Sutherlandia frutescens（L.）R. Br.）的地上部分中分离和测定四种黄酮类化合物（sutherlandins A-D）和四种环阿尔廷醇糖苷（sutherlandiosides A-D）的第一个分析方法。采用反相（RP-18）柱、PDA 与 ELS 检测，以水/乙腈梯度作为流动相，通过高效液相色谱法（HPLC）进行分离。二极管阵列检测器用于定量测定四种黄酮类化合物的波长为 260nm。由于环阿尔廷醇糖苷的紫外吸收较低，因此通过蒸发光散射（ELSD）进行检测。该方法对线性、重复性、检测限（LOD）和定量限（LOQ）进行了验证。八种化合物的检测限和定量限范围分别为 0.1-7.5μg/mL 和 0.5-25μg/mL。对产物的分析表明，主要化合物 sutherlandioside B 的平均重量变化范围较大，为 1.099-5.224mg/average weight。LC-ESI-TOF 进一步证实了植物样品和南非钩麻产物中的八种化合物。该方法在正离子模式下使用M+H和M+Na离子，并采用提取离子监测（EIM）。
