Yang Li, Wang Yun, Zhang Guangnong, Zhang Fang, Zhang Zijia, Wang Zhengtao, Xu Luoshan
Key Laboratory of Standardization of Chinese Medicines of Ministry of Education, Shanghai University of Traditional Chinese Medicine, Shanghai 201203, People's Republic of China.
Biomed Chromatogr. 2007 Jul;21(7):687-94. doi: 10.1002/bmc.801.
A novel high-performance liquid chromatographic method with mass spectrometry and diode array detection method for the simultaneous qualitative and quantitative analysis of bioactive phenols was developed. In total, nine chemically diverse phenols including five bibenzyls, three phenanthrenes and a coumarin were unambiguously identified in Dendrobium aurantiacum var. denneanum by comparison with the available references or reported data according to their retention behaviors, UV spectra and fragmentations of ESI-MS. The contents of the four main phenolic compounds, moscatilin, gigantol, moscatin and coumarin, in D. aurantiacum var. denneanum from the wild and various cultivated populations were determined by HPLC-UV. The sample preparation involved a rapid and simple procedure based on solid-phase extraction using a C(18) reversed-phase cartridge. The quantitative analysis was performed on a Beckman Coulter ODS column (5 microm, 250 x 4.6 mm) using a linear gradient elution system of acetonitrile-0.5% formic acid. The method was validated for linearity, limits of detection (LOD) and quantification (LOQ), precision and accuracy. Good results were obtained with respect to the overall intra- and inter-day variations (RSD less than 3.22%) and the percentage recoveries (ranging from 90.50 to 99.22%). Notable differences in the contents of phenols were observed among different cultivated populations. The samples colleted in April and May (spring), or October and November (autumn) accumulated much higher contents of phenols than those collected in other seasons.
开发了一种结合质谱和二极管阵列检测的新型高效液相色谱方法，用于生物活性酚类的同时定性和定量分析。通过与现有参考文献或报道数据比较，根据其保留行为、紫外光谱和电喷雾电离质谱（ESI-MS）的碎片，在滇金石斛中明确鉴定出总共9种化学结构不同的酚类，包括5种联苄、3种菲和1种香豆素。采用高效液相色谱-紫外检测法（HPLC-UV）测定了滇金石斛野生及不同栽培居群中4种主要酚类化合物，即毛兰素、大花蕙兰素、莫斯卡亭和香豆素的含量。样品制备采用基于C(18)反相柱固相萃取的快速简便方法。定量分析在贝克曼库尔特ODS柱（5μm，250×4.6mm）上进行，使用乙腈-0.5%甲酸线性梯度洗脱系统。该方法在线性、检测限（LOD）和定量限（LOQ）、精密度和准确度方面得到验证。在日内和日间总体变化（相对标准偏差小于3.22%）和回收率（90.50%至99.22%）方面均取得了良好结果。不同栽培居群的酚类含量存在显著差异。4月和5月（春季）或10月和11月（秋季）采集的样品中酚类积累量远高于其他季节采集的样品。
