苦橙花中酚类物质的绿色回收：天然深共熔溶剂-超声协同萃取、吸附纯化及UPLC/Q-TOF-MS/MS分析

IF 9.7 1区化学 Q1 ACOUSTICS

Ultrasonics Sonochemistry Pub Date : 2025-10-02 DOI:10.1016/j.ultsonch.2025.107597

Ziyu Lv , Jing Ma , Chi Wei , Jiaqi Wang , Dan Wang , Xinxin Cheng , Guoliang Chen , Luis A.J. Mur , Yanfeng Wang , Duo Cao

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引用次数: 0

摘要

苦橙花（BOF）是一种著名的药用和食用植物资源，富含酚类化合物，具有重要的保健和工业应用潜力。然而，有效的提取和纯化技术，以回收生物活性酚仍有待探索。为了解决这一问题，本研究旨在开发一种将天然深共熔溶剂-超声协同萃取（nads - use）与吸附净化相结合的生态友好型综合策略，以有效回收生物脱灰中总酚类物质（BOF- tp）。首先，从12种合成NADESs和3种常用溶剂中确定氯胆碱-乙二醇（ChCl-EG）为最佳提取溶剂。采用Box-Behnken设计（BBD），优化了NADES-USE的工艺参数（38%水溶液ChCl-EG， 18 mL/g, 345 W, 43 min, 55°C）， BOF-TP得率为104.58±0.34 mg/g，是传统溶剂的1.30 ~ 2.16倍。结果表明，AB-8树脂对BOF-TP的吸附-解吸性能最佳，吸附行为符合Langmuir等温线和拟二级动力学模型。热力学分析证实这是一个自发的、熵递减的放热物理吸附过程。利用突破曲线和梯度洗脱曲线建立了BOF-TP粗提取物的色谱纯化工艺，纯度为75.62±0.95%。最后，建立了UPLC-Q/TOF-MS/MS方法，对7种生物活性化合物进行了全面的化学表征和同时定量分析，为纯化的BOF-TP提取物的质量控制奠定了基础。总之，这项工作表明，NADES-USE和吸附纯化相结合，为生产高纯度的BOF-TP提取物提供了巨大的潜力，可进一步用于食品和制药应用。

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Green recovery of phenolics from bitter orange flowers: Natural deep eutectic solvent-ultrasound synergistic extraction, adsorptive purification, and UPLC/Q-TOF-MS/MS analysis

Bitter orange flowers (BOF), a renowned medicinal and edible botanical resource, are rich in phenolic compounds with significant potential for health and industrial applications. However, efficient extraction and purification techniques for recovering bioactive phenolics remain underexplored. To address this gap, this study aimed to develop an eco-friendly integrated strategy combining natural deep eutectic solvent-ultrasound synergistic extraction (NADES-USE) with adsorptive purification for efficient recovery of total phenolics from BOF (BOF-TP). First, choline chloride-ethylene glycol (ChCl-EG) was determined to be the optimal extraction solvent from 12 synthesized NADESs and 3 common solvents. Employing Box-Behnken design (BBD), the optimized parameters for NADES-USE (38 % aqueous ChCl-EG, 18 mL/g, 345 W, 43 min, and 55 °C) resulted in a BOF-TP yield of 104.58 ± 0.34 mg/g, which was 1.30 to 2.16 times higher than those achieved with conventional solvents. Then, AB-8 resin demonstrated optimal adsorption–desorption performance for BOF-TP, with adsorption behavior strongly conforming to Langmuir isotherm and pseudo-second-order kinetic models. Thermodynamic analysis confirmed a spontaneous, exothermic physisorption process with decreasing entropy. The breakthrough curves and gradient elution curves were utilized to establish a chromatographic purification process for crude BOF-TP extracts, achieving a purity of 75.62 ± 0.95 %. Finally, a validated UPLC-Q/TOF-MS/MS method facilitated comprehensive chemical characterization and simultaneous quantification of seven bioactive compounds, serving as a basis for the quality control of purified BOF-TP extracts. In conclusion, this work demonstrates that the combination of NADES-USE and adsorptive purification offers significant potential for producing highly purified BOF-TP extract for further use in food and pharmaceutical applications.

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来源期刊

Ultrasonics Sonochemistry 化学-化学综合

CiteScore

15.80

自引率

11.90%

发文量

361

审稿时长

59 days

期刊介绍： Ultrasonics Sonochemistry stands as a premier international journal dedicated to the publication of high-quality research articles primarily focusing on chemical reactions and reactors induced by ultrasonic waves, known as sonochemistry. Beyond chemical reactions, the journal also welcomes contributions related to cavitation-induced events and processing, including sonoluminescence, and the transformation of materials on chemical, physical, and biological levels. Since its inception in 1994, Ultrasonics Sonochemistry has consistently maintained a top ranking in the "Acoustics" category, reflecting its esteemed reputation in the field. The journal publishes exceptional papers covering various areas of ultrasonics and sonochemistry. Its contributions are highly regarded by both academia and industry stakeholders, demonstrating its relevance and impact in advancing research and innovation.