High Pressure Laboratory, Department of Chemistry, Faculty of Science, Universidad Nacional de Colombia, Carrera 30 #45-03, Bogotá, D.C., 111321, Colombia; Laboratory of Foodomics, Institute of Food Science Research, CIAL, CSIC, Nicolás Cabrera 9, 28049, Madrid, Spain.
Laboratory of Foodomics, Institute of Food Science Research, CIAL, CSIC, Nicolás Cabrera 9, 28049, Madrid, Spain.
J Chromatogr A. 2019 Jan 11;1584:155-164. doi: 10.1016/j.chroma.2018.11.055. Epub 2018 Nov 24.
In this work, a multi-analytical platform that allows obtaining and characterizing high-added value compounds from natural sources is presented, with a huge potential in traditional medicine, natural products characterization, functional foods, etc. Namely, the proposed multi-analytical platform is based on the combination of pressurized liquid extraction (PLE), liquid chromatography (LC) and gas chromatography quadrupole time-of-flight mass spectrometry GC-q-TOF-MS(/MS), in vitro assays and modelling tools for guiding extraction optimization. As case study, goldenberry or cape gooseberry fruit (Physalys peruviana L.) was selected. In particular, the potential of P. peruviana calyces, an important by-product of goldenberry processing, as promising source of bioactive compounds was evaluated. Selection of the most suitable solvent for PLE was based on the Hansen solubility parameters (HSP) approach using 4β-hydroxywithanolide E (4βHWE) and withanolide E (WE) as target compounds due to their bioactive potential. A surface response methodology was further applied for the optimization of the PLE parameters: temperature (50, 100 and 150 °C) and solvent composition (% EtOH in the mixture EtOH/EtOAc). The effects of the independent variables on extraction yield, withanolides content (4βHWE and WE), total phenolic content (TPC), total flavonoids content (TFC) and antioxidant activity (EC and TEAC) were evaluated in order to obtain withanolide-rich extracts from P. peruviana calyces. The extract obtained under optimal conditions (at 125 °C and 75% EtOH v/v) exhibited satisfactory extraction yield (14.7%) and moderate antioxidant activity (with an EC value of 77.18 μg mL and 1.08 mM trolox g), with 4βHWE and WE concentrations of 8.8 and 2.3 mg g, respectively. LC-q-TOF-MS/MS analysis of the extract allowed the quantitation of 4βHWE and WE and the tentative identification of several other withanolides structures. The obtained results demonstrate the great potential of this multi-analytical approach for developing valorisation strategies of food by-products under sustainable conditions, to obtain bioactive-enriched extracts with potential medicinal or health-promoting properties.
在这项工作中，提出了一种多分析平台，该平台允许从天然来源中获得和表征高附加值化合物，在传统医学、天然产物表征、功能性食品等领域具有巨大的潜力。具体来说，所提出的多分析平台基于加压液体提取（PLE）、液相色谱（LC）和气相色谱四极杆飞行时间质谱 GC-q-TOF-MS(/MS) 的组合，以及体外测定和建模工具用于指导提取优化。作为案例研究，选择了灯笼果或仙人掌果（Physalys peruviana L.）。特别是，评估了灯笼果萼片作为生物活性化合物有前途的来源的潜力，灯笼果萼片是灯笼果加工的重要副产物。基于 Hansen 溶解度参数 (HSP) 方法，选择最适合 PLE 的溶剂，使用 4β-羟基乌头原碱 E (4βHWE) 和乌头原碱 E (WE) 作为目标化合物，因为它们具有生物活性潜力。进一步应用表面响应方法优化 PLE 参数：温度（50、100 和 150°C）和溶剂组成（混合物中 EtOH 的百分比 EtOH/EtOAc）。评估了独立变量对提取产率、乌头原碱含量（4βHWE 和 WE）、总酚含量（TPC）、总黄酮含量（TFC）和抗氧化活性（EC 和 TEAC）的影响，以从灯笼果萼片中获得富含乌头原碱的提取物。在最佳条件下（125°C 和 75% EtOH v/v）获得的提取物具有令人满意的提取产率（14.7%）和中等抗氧化活性（EC 值为 77.18 μg mL 和 1.08 mM trolox g），4βHWE 和 WE 浓度分别为 8.8 和 2.3 mg g。提取物的 LC-q-TOF-MS/MS 分析允许定量 4βHWE 和 WE，并推测鉴定出其他几种乌头原碱结构。所得结果表明，这种多分析方法在可持续条件下开发食品副产物的增值策略、获得具有潜在药用或促进健康特性的富含生物活性的提取物方面具有巨大潜力。
