Centre for Metabolomics and Bioanalysis (CEMBIO), Facultad de Farmacia, Universidad CEU San Pablo, Campus Montepríncipe, Boadilla del Monte, 28668 Madrid, Spain.
Plant Physiology, Pharmaceutical and Health Sciences Department, Facultad de Farmacia, Universidad CEU San Pablo, Campus Montepríncipe, Boadilla del Monte, 28668 Madrid, Spain.
J Pharm Biomed Anal. 2019 Feb 5;164:47-56. doi: 10.1016/j.jpba.2018.10.014. Epub 2018 Oct 7.
Triterpene saponins are important chemical constituents in blackberry leaves and have significant antimicrobial activity, among other healthful properties. In this study, a new UHPLC-MS method was optimized with outstanding efficiency for a non-targeted metabolic approach and comprehensive analysis of bioactive compounds in blackberry leaves (Rubus cv. Loch Ness). With minimum sample treatment, phenols and triterpene saponins, among others, were separated according to their elution times. Once separated, the major triterpene saponins were classified by their aglycone moieties and their structures tentatively identified based on their accurate mass spectra in positive and negative ESI mode. By the use of UHPLC coupled to a TOF, a high-resolution and accuracy mass analyzer, reliable molecular formulas of the detected compounds were predicted, and along with the generated MS spectra in full scan mode, allowed the tentative identification and classification of the most abundant triterpene saponins presented the samples analyzed. A rapid and comprehensive strategy to study the complex saponin profile is presented. Unlike other LC-MS/MS methods, the proposed method requires just one mass analyzer, and to our knowledge, this is the first systematic study on triterpene saponins in blackberry leaves.
三萜皂苷是黑莓叶中的重要化学成分，具有显著的抗菌活性和其他有益特性。在这项研究中，优化了一种新的 UHPLC-MS 方法，该方法具有出色的效率，可用于非靶向代谢方法和黑莓叶中生物活性化合物的综合分析（Rubus cv. Loch Ness）。通过最小的样品处理，根据其洗脱时间分离出酚类和三萜皂苷等物质。一旦分离出来，根据其在正、负离子 ESI 模式下的精确质谱，将主要的三萜皂苷按其糖苷部分进行分类，并根据其结构对其结构进行初步鉴定。通过使用 UHPLC 与 TOF 连接，高分辨率和精度质量分析仪，可以预测检测到的化合物的可靠分子公式，并结合全扫描模式生成的 MS 光谱，允许对分析样品中存在的最丰富的三萜皂苷进行初步鉴定和分类。提出了一种快速而全面的策略来研究复杂的皂苷谱。与其他 LC-MS/MS 方法不同，该方法仅需要一个质量分析仪，据我们所知，这是黑莓叶中三萜皂苷的首次系统研究。
