连续选择性超临界流体萃取（S3FE）金盏花中黄酮类和酯化三萜类化合物的研究

Exploring the Sequential-Selective Supercritical Fluid Extraction (S3FE) of Flavonoids and Esterified Triterpenoids from Calendula officinalis L. Flowers
Sirine Atwi-Ghaddar，Lydie Zerwette,  Emilie Destandau，Eric Lesellier

*Institute of Organic and Analytical Chemistry (ICOA), University of Orléans, CNRS UMR 7311, 45100 Orléans, France

Molecules 2023, 28(20), 7060; https://doi.org/10.3390/molecules28207060
Submission received: 12 September 2023 / Revised: 4 October 2023 / Accepted: 9 October 2023 / Published: 12 October 2023

(This article belongs to the Special Issue Innovation in Green Extraction and Processing—a Themed Issue in Memory of Professor Farid Chemat for His Outstanding Contributions to Green Chemistry (1968–2023))
 

Abstract
One of the many advantages of supercritical fluid extraction (SFE) is the possibility of using it in sequential and selective approaches. This is due to the use of a dynamic extraction mode in addition to the possibility of altering the composition of the modifier during the extraction process. In this study, the optimization of Calendula officinalis L. extraction of non-polar and polar compounds was achieved using three-level Box-Behnken designs (BBD). For non-polar compounds, the factors were pressure, temperature, and EtOH percentage. As for the polar compounds, the three variables were temperature, the total modifier percentage, and H2O added in the modifier as an additive. The recovery of selectively rich extracts in triterpendiol esters and narcissin was possible using a sequential two-step SFE. The first step was performed at 80 °C and 15% EtOH, and the second at 40 °C and 30% EtOH:H2O 80:20 v:v with a total of 60 min of extraction. Additionally, the SFE extraction of non-polar compounds was scaled up on a pilot-scale extractor, demonstrating similar results. Finally, the SFE results were compared to ultrasound-assisted extraction (UAE).

超临界流体萃取（SFE）的许多优点之一是可以在顺序和选择性方法中使用它。这是由于除了在提取过程中改变改性剂组成的可能性之外，还使用了动态提取模式。在本研究中，使用三级Box-Behnken设计（BBD）对金盏花提取非极性和极性化合物进行了优化。对于非极性化合物，影响因素是压力、温度和EtOH百分比。至于极性化合物，三个变量是温度、总改性剂百分比和作为添加剂添加到改性剂中的H2O。使用连续两步SFE可以回收三萜二醇酯和水仙花素中选择性富集的提取物。第一步在80°C和15%EtOH下进行，第二步在40°C和30%EtOH:H2O 80:20 v:v下进行，总共提取60分钟。此外，非极性化合物的SFE提取在中试规模的提取器上进行了放大，显示了类似的结果。最后，将SFE结果与超声辅助提取（UAE）进行比较。

Keywords:extraction scale-up; marigold; narcissin; Box-Behnken design

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3.3. SC-CO2 Extraction
For the analytical scale SFE, a Waters MV-10® ASFE (Milford, MA, USA) was used for all extractions. In total, 1 g of the plant powder was combined with 1 g of diatomaceous earth powder from Sigma-Aldrich (Merck, Semoy, France) in a stainless-steel extraction vessel (5 mL). To filter the extract and completely fill the extraction cell, cotton was positioned at the top and bottom parts. A continuous dynamic extraction was used with a 3 mL/min flow rate. The amount of modifier added was calculated based on this overall extraction flow.
For the pilot-scale extraction of non-polar compounds, an SFE process (Tomblaine, France) extractor was used. This extractor was equipped with a CO2 and co-solvent pump. A gravity separator (S1) and a cyclone separator (S2) were used to collect the extracts. The extraction conditions were set to a 60 °C temperature, 15 MPa pressure, a total flow of 60 mL/min, and 15 % of EtOH (96% purity) added as a modifier to the SC-CO2. One liter of the stainless-steel extraction vessel was used and filled with 100 g of plant material combined with 100 g of diatomaceous earth. The total duration of the EtOH-modified extraction was 57 min, where 6 fractions were weighed and collected from S1. Approximately 50 g of the extract was collected for each fraction (around 9 min for each fraction). A final step (fraction 7) of 90 min with 100% SC-CO2 was applied to dry the plant mass, removing the residual EtOH and collecting extract residues. At the end of extraction, the content of the S2 for the total extraction duration was collected for analysis.

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