Department of Pharmaceutical Analysis, Affiliated Hospital of Integrated Traditional Chinese and Western Medicine, Nanjing University of Chinese Medicine, Nanjing 210028, People's Republic of China; State Key Laboratory of Natural Medicines, Department of Chinese Medicines Analysis, China Pharmaceutical University, Nanjing 210009, PR China.
Department of Pharmaceutical Analysis, Affiliated Hospital of Integrated Traditional Chinese and Western Medicine, Nanjing University of Chinese Medicine, Nanjing 210028, People's Republic of China.
Food Chem. 2018 Apr 25;246:202-210. doi: 10.1016/j.foodchem.2017.10.151. Epub 2017 Nov 1.
In this study, a novel ultra-performance liquid chromatography coupled with quadrupole/time-of-flight mass spectrometry (UPLC-QTOF-MS/MS)-guidance strategy was proposed for preparation of sulfur-containing derivatives in sulfur-fumigated edible herbs. Being versatile in both chromatographic separation and mass spectrometric detection, UPLC-QTOF-MS/MS was inducted into each experimental step for multifaceted purposes including finding, tracking, purity determination and structural elucidation of targeted compounds as well as UPLC-HPLC chromatographic conditions transplantation, whereby the isolation and purification procedures were greatly facilitated. Using this strategy, a new sulfur-containing ginsenoside Rg derivative (named compound I) was obtained from sulfur-fumigated ginseng. The chemical structure of compound I was elucidated to be (3β, 6α, 12β)-3, 12-dihydroxydammar-25-ene-6, 20-diylbis-β-d-glucopyranoside, 24-sulfonic acid by QTOF-MS/MS, H-NMR and C-NMR analysis, and its generation mechanisms by sulfur-fumigation were accordingly discussed. The research deliverable suggests that the UPLC-QTOF-MS/MS-guidance strategy is promising for targeted preparation of sulfur-containing derivatives from sulfur-fumigated edible herbs.
在这项研究中，提出了一种新的超高效液相色谱-四极杆/飞行时间质谱（UPLC-QTOF-MS/MS）指导策略，用于制备硫磺熏制食用草药中的含硫衍生物。UPLC-QTOF-MS/MS 在色谱分离和质谱检测方面都具有多功能性，被引入到每个实验步骤中，用于多方面的目的，包括寻找、跟踪、目标化合物的纯度测定和结构阐明以及 UPLC-HPLC 色谱条件的移植，从而大大简化了分离和纯化过程。使用这种策略，从硫磺熏制的人参中获得了一种新的含硫人参皂苷 Rg 衍生物（命名为化合物 I）。通过 QTOF-MS/MS、H-NMR 和 C-NMR 分析，阐明了化合物 I 的化学结构为（3β,6α,12β）-3,12-二羟基达玛-25-烯-6,20-二醇双-β-D-吡喃葡萄糖苷，24-磺酸，并据此讨论了其硫磺熏制生成机制。研究结果表明，UPLC-QTOF-MS/MS 指导策略有望用于从硫磺熏制的食用草药中靶向制备含硫衍生物。
