Song Chunying, Zhang Huarong, Guo Zhimou, Yan Jingyu, Jin Gaowa, Liang Xinmiao
Key Lab of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, China.
University of Chinese Academy of Sciences, Beijing 100049, China.
Se Pu. 2020 May 8;38(5):547-553. doi: 10.3724/SP.J.1123.2019.09003.
A new method based on solid-phase extraction-ultraperformance liquid chromatography (SPE-UPLC) was developed for the determination of five protopanaxadiol ginsenosides in ginseng. The ginsenosides were extracted from ground ginseng samples using water-saturated -butanol and purified on a hydrophilic solid-phase extraction column. Chromatographic separation was achieved on an ACQUITY UPLC BEH Shield RP18 column (100 mm×2.1 mm, 1.7 μm) by linear gradient elution using an acetonitrile/water mobile phase. Five protopanaxadiol ginsenosides were detected by a photodiode array detector, and they showed a strong positive linear correlation (>0.999) in the range of 5-500 μg/mL. In addition, the instrument precision ranged between 0.95% and 2.62% (=6), with the sample stability between 0.90% and 2.15% (=8) within 22 h. Intra- and inter-day repeatabilities were 5.35%-6.47% (=6) and 5.56%-6.34% (=8), respectively. Sample recoveries and the corresponding relative standard deviations (RSDs) were 87.16%-101.92% and 1.54%-4.01% (=6), respectively. Hydrophilic chromatography materials were used in SPE, and the extract was directly loaded and purified without pretreatment. Besides, with the use of UPLC, the analysis time was greatly shortened. The developed method is simple and rapid, with high throughput, thus being suitable for the quantitative analysis of the five protopanaxadiol ginsenosides in ginsengs.
建立了一种基于固相萃取-超高效液相色谱（SPE-UPLC）的方法，用于测定人参中5种原人参二醇型人参皂苷。采用水饱和正丁醇从人参粉末样品中提取人参皂苷，并在亲水固相萃取柱上进行纯化。在ACQUITY UPLC BEH Shield RP18柱（100 mm×2.1 mm，1.7 μm）上，以乙腈/水为流动相进行线性梯度洗脱，实现色谱分离。用光电二极管阵列检测器检测5种原人参二醇型人参皂苷，在5-500 μg/mL范围内呈强正线性相关（>0.999）。此外，仪器精密度在0.95%-2.62%（n=6）之间，样品在22 h内的稳定性在0.90%-2.15%（n=8）之间。日内和日间重复性分别为5.35%-6.47%（n=6）和5.56%-6.34%（n=8）。样品回收率及其相应的相对标准偏差（RSD）分别为87.16%-101.92%和1.54%-4.01%（n=6）。SPE中使用亲水色谱材料，提取物无需预处理即可直接上样纯化。此外，使用UPLC大大缩短了分析时间。所建立的方法简便快速，通量高，适用于人参中5种原人参二醇型人参皂苷的定量分析。
