School of Food Engineering (FEA), University of Campinas (UNICAMP), Rua Monteiro Lobato, n.80, 13083-862 Campinas, São Paulo, Brazil.
School of Applied Sciences (FCA), University of Campinas (UNICAMP), Rua Pedro Zaccaria, n. 1300, 13484-350 Limeira, São Paulo, Brazil; Centro de Ciências da Natureza, Universidade Federal de São Carlos, Rod. Lauri Simões de Barros, km 12 - SP 189, Buri, SP 18290-000, Brazil.
Food Res Int. 2022 Oct;160:111711. doi: 10.1016/j.foodres.2022.111711. Epub 2022 Jul 20.
This study aimed to extract anthocyanins from dried and semi-defatted açaí pulp using green technologies based on the coupling of pressurized liquid extraction (PLE) with in-line purification through solid-phase extraction (SPE) and on-line analysis by high-performance liquid chromatography (HPLC). Critical parameters that affect the extraction efficiency and purification were investigated and optimized by response surface methodology (RSM). PLE was performed with acidified water at different pH (2.0, 4.5, and 7.0) and temperatures (40, 80, and 120 °C) at 15 MPa, 2 mL/min, and solvent-to-feed mass ratio equal to 40. SPE was optimized in a column packed with the adsorbent PoraPak™ Rxn. Different ethanol concentrations (50, 75, and 100 %) and temperatures (30, 40, and 50 °C) were evaluated for the anthocyanin's elution. The optimal conditions of the two experimental designs were determined by the RSM, firstly for PLE: 71 °C and pH 2; then using this PLE condition, the optimization of the SPE was obtained: 30 °C and 50 % ethanol. The developed PLE method provided similar anthocyanin yield to other techniques, and the coupling with SPE in-line produced an extract 5-fold more concentrated than PLE alone. Therefore, the system (PLE-SPE × HPLC-PDA) proved to be a powerful tool for monitoring the extraction process in real-time.
本研究旨在使用基于加压液体萃取(PLE)与在线固相萃取(SPE)净化和高效液相色谱(HPLC)在线分析相结合的绿色技术,从干燥和半脱脂的巴西莓果肉中提取花色苷。通过响应面法(RSM)研究并优化了影响萃取效率和净化效果的关键参数。在 15 MPa、2 mL/min 和溶剂-进料质量比等于 40 的条件下,用酸化水在不同 pH(2.0、4.5 和 7.0)和温度(40、80 和 120°C)下进行 PLE。SPE 在填充有吸附剂 PoraPak™ Rxn 的柱中进行优化。评估了不同乙醇浓度(50、75 和 100%)和温度(30、40 和 50°C)对花色苷洗脱的影响。通过 RSM 确定了两个实验设计的最佳条件,首先是 PLE:71°C 和 pH 2;然后,使用此 PLE 条件,优化了 SPE:30°C 和 50%乙醇。开发的 PLE 方法提供了与其他技术相当的花色苷产率,并且与 SPE 在线耦合产生的提取物比单独使用 PLE 浓缩了 5 倍。因此,该系统(PLE-SPE×HPLC-PDA)被证明是实时监测萃取过程的有力工具。