Stavrianidi Andrey, Stekolshchikova Elena, Porotova Anna, Rodin Igor, Shpigun Oleg
Chemistry Department, Lomonosov Moscow State University, 119991 Moscow, Russia.
Chemistry Department, Lomonosov Moscow State University, 119991 Moscow, Russia.
J Pharm Biomed Anal. 2017 Jan 5;132:87-92. doi: 10.1016/j.jpba.2016.09.041. Epub 2016 Sep 28.
Conventional liquid chromatographic methods coupled with ultraviolet detection with low-wavelength range are lacking selectivity and sensitivity to determine both polar and less polar ginsenosides. Also the lack of standard substances for such quality control methods is leading to development of the approaches using single standard for quantitative analysis of multi-component system (QAMS). The objective of present study was to establish and compare for the first time liquid chromatography-ultraviolet detection and liquid chromatography-mass spectrometry QAMS methods for the simultaneous determination of protopanaxatriol-type and protopanaxadiol-type ginsenosides in a variety of ginseng products. Sixteen polar and less polar ginsenosides were separated on a reversed-phase C18-column (150mm×2.0mm, 2.2μm) with a mobile phase consisting of 0.1% formic acid in water and acetonitrile. Components were then detected by means of ultraviolet and mass spectrometry detection. Characteristic sapogenin fragmentation signals with m/z 423 and 425 for two major groups of ginseng saponins allowed their simultaneous determination in a single chromatographic run, while the use of ultraviolet detection tends to give overvalued results. Structural correlation between the relative response factors and saponin structure was demonstrated. The method was linear (R >0.999) and sensitive (LODs, 0.01-0.03mg/mL) within the concentration range tested. Concentrations of individual ginsenosides and several quality control parameters were determined in ginseng root extracts and commercial ginseng products of different types (root slices, tablets and tea samples), and results showed that ginsenoside content can be successfully measured by means of QAMS approach.
传统的液相色谱方法结合低波长范围的紫外检测，在测定极性和低极性人参皂苷时缺乏选择性和灵敏度。此外，这种质量控制方法缺乏标准物质，导致了使用单一标准对多组分系统进行定量分析（QAMS）方法的发展。本研究的目的是首次建立并比较液相色谱-紫外检测和液相色谱-质谱QAMS方法，用于同时测定多种人参产品中原人参三醇型和原人参二醇型人参皂苷。在反相C18柱（150mm×2.0mm，2.2μm）上，以水和乙腈中含0.1%甲酸的流动相分离16种极性和低极性人参皂苷。然后通过紫外和质谱检测对各组分进行检测。两组主要人参皂苷的特征皂苷元碎片信号m/z 423和425，使得它们能够在一次色谱运行中同时测定，而使用紫外检测往往会得出高估的结果。证明了相对响应因子与皂苷结构之间的结构相关性。该方法在所测试的浓度范围内呈线性（R>0.999）且灵敏（检测限，0.01 - 0.03mg/mL）。测定了人参根提取物和不同类型（根片、片剂和茶样）的商业人参产品中各人参皂苷的浓度以及几个质量控制参数，结果表明通过QAMS方法可以成功测定人参皂苷含量。
