Optimization of DIC-Tripolium Ecofriendly Extraction Process: Recovery of Hesperidin from Orange Byproducts, Antioxidant and α-Amylase Inhibition of Extracts.

This study aimed to investigate the effect of an innovative ecofriendly process-instant controlled pressure drop technology, also known as "détente instantanée contrôlée" or DIC-coupled with Tripolium extraction (DIC-Tripolium), on the hesperidin recovery, and antioxidant and antidiabetic activities of orange byproduct extracts. A DIC pretreatment was applied to partially dried orange byproducts (~16% wet basis). A central composite rotatable design (CCRD), composed of 13 experimental trials (four factorial points, four-star points, and five repetitions for the central point), was followed by a Tripolium process consisting of successive intermittent extraction periods using ethanol/water solvent at 20 ± 1 °C, 5 kPa for 5 min and m/v ratio = 5 g/50 mL. The DIC pretreatment, coupled with the Tripolium process, increased the extractability of hesperidin (from 1.55- to 4.67-fold compared to untreated DIC orange byproducts). The radical scavenging activities of the extracts were also enhanced or preserved in different DIC-Tripolium extracts. The α-Amylase inhibition percentage varied between 55.6 ± 0.02 and 88.30 ± 0.01% according to DIC-Tripolium conditions. The multi-criteria optimized condition of DIC-Tripolium extraction, allowing for the maximization of the hesperidin content, radical scavenging activities, iron chelating activity, and α-amylase inhibition of extracts, corresponds to a DIC saturated steam pressure of 599.4 kPa and a DIC pretreatment time of 38 s.

Intensifying Effect of Instant Controlled Pressure Drop (DIC) Pre-Treatment on Hesperidin Recovery from Orange Byproducts: In Vitro Antioxidant and Antidiabetic Activities of the Extracts.

The orange byproduct is a widely accessible and valuable source of functional phenolic compounds, particularly hesperidin. Hesperidin extraction remains a challenging phase in its valorization chain due to its low solubility and limited extractability in solvents. This work aims to examine the effect of conventional solvent extraction (CSE) compared to emerging and innovative extraction methods: accelerated solvent extraction (ASE) and ultrasound-assisted extraction (UAE) when applied with or without a pretreatment process of instant controlled pressure drop (DIC) to intensify extraction, antioxidant, and antidiabetic activities. The total phenols, flavonoids, hesperidin contents, radical scavenging activities, iron chelating activity, and in vitro α-amylase inhibition of the extracts were determined for CSE (80%, 70 °C), UAE (ethanol 80%, 70 °C, 200 W), and ASE (ethanol 60%, 100 °C, 100 bars) with or without DIC pretreatment (pressure = 0.4 MPa, total thermal time = 30 s). The hesperidin amounts obtained were 0.771 ± 0.008 g/100 g DM, 0.823 ± 0.054 g/100 g DM, and 1.368 ± 0.058 g/100 g DM, for CSE, UAE, and ASE, respectively. DIC pretreatment of orange byproducts increased hesperidin recovery by 67%, 25.6%, and 141% for DIC-CSE, DIC-UAE, and DIC-ASE, respectively. The DPPH and ABTS radical scavenging and iron chelating activities of extracts were also significantly enhanced, and the in vitro antidiabetic activity of extracts was preserved.

Improvement of Sinapine Extraction from Mustard Seed Meal by Application of Emerging Technologies.

Sinapine is a phenolic compound found in mustard (Brassica juncea) seed meal. It has numerous beneficial properties such as antitumor, neuroprotective, antioxidant, and hepatoprotective effects, making its extraction relevant. In this study, the extraction of sinapine was investigated using three methods: (i) from a mustard seed meal defatted by a supercritical CO2 (SC-CO2) pretreatment, (ii) by the implementation of high-voltage electrical discharges (HVEDs), (iii) and by the use of ultrasound. The use of SC-CO2 pretreatment resulted in a dual effect on the valorization of mustard seed meal, acting as a green solvent for oil recovery and increasing the yield of extracted sinapine by 24.4% compared to the control. The combination of ultrasound and SC-CO2 pretreatment further increased the yield of sinapine by 32%. The optimal conditions for ultrasound-assisted extraction, determined through a response surface methodology, are a temperature of 75 °C, 70% ethanol, and 100% ultrasound amplitude, resulting in a sinapine yield of 6.90 ± 0.03 mg/g dry matter. In contrast, the application of HVEDs in the extraction process was not optimized, as it led to the degradation of sinapine even at low-energy inputs.

Unlocking the access to oxidized coenzyme A via a single-step green membrane-based purification.

A new membrane-based strategy to purify oxidized coenzyme A ((CoAS)2) from adenosine triphosphate (ATP), adenosine diphosphate (ADP) and adenosine monophosphate (AMP) has been developed. Commercially available membranes were screened and studied (permeate flux and overall compounds retention) which allowed the identification of one efficient membrane (GK from Suez Water Technologies & Solutions). Different total compounds concentrations solutions were used in the system in order to find the following working conditions: 4 bars with a total compounds solution of 5.19 g L-1. Applying these conditions to a dia-filtration set-up allowed us to reach 68% pure (CoAS)2 in 4.8 diafiltration volumes (DV) and a 95% (CoAS)2 purity can be predicted in 8.5 DV. A comparative study of green metrics-i.e. process mass index (PMI)-of the classic chromatography vs the membrane-based one demonstrated the great advantages of the latter in terms of sustainability. This strategy unlocks the access to the essential and central cofactor that is coenzyme A.

Optimization of Extraction Conditions to Improve Chlorogenic Acid Content and Antioxidant Activity of Extracts from Forced Witloof Chicory Roots.

Chlorogenic acids are major phenolic constituents in many herbal medicines and exhibit various bioactivities that explain the growing interest in extracting chlorogenic acids from biomass. In this context, the present study aims to maximize 3-O-Caffeoylquinic acid (3-CQA) and 3,5-O-di-caffeoylquinic acid (3,5-diCQA) contents from forced witloof chicory roots and to analyze the extraction kinetic modelling. First, the solid-liquid ratio, ethanol concentration, extraction time and temperature were studied. The extraction conditions were optimized to maximize the extraction of these compounds. The maximum yields reached 5 ± 0.11 and 5.97 ± 0.30 mg/g dry matter (DM) for 3-O-Caffeoylquinic acid and 3,5-O-di-caffeoylquinic acid, respectively, in less than 6 min at 70 °C. Extraction with water as a solvent was assessed with the aim of proposing a second greener and less-expensive solvent. This extraction is very fast from 90 °C, with a maximum of 6.22 ± 0.18 mg/gDM of 3-O-Caffeoylquinic acid, and instantaneous for 3,5-O-di-caffeoylquinic acid with a maximum of 6.44 ± 0.59 mg/gDM. In the second step, response surface methodology was employed to optimize the ultrasound-assisted extraction of antioxidants. The higher antioxidant activities were found at temperatures from 40 °C and at percentages of ethanol in the range of 35-70%.

Optimization of the Accelerated Solvent Extraction of Caffeoylquinic Acids from Forced Chicory Roots and Antioxidant Activity of the Resulting Extracts.

Forced chicory roots (FCR) are the main but also the least valued by-products of Belgian endive culture. However, they contain molecules of interest for industry such as caffeoylquinic acids (CQAs). This study aims to investigate accelerated solvent extraction (ASE) as a green technique to recover chlorogenic acid (5-CQA) and 3,5-dicaffeoylquinic acid (3,5-diCQA), the main CQAs. A D-optimal design was used to determine the influence of temperature and ethanol percentage on their extraction. Optimal extraction conditions were determined using response surface methodology (RSM) and allow the recovery of 4.95 ± 0.48 mg/gDM of 5-CQA at 107 °C, 46% of ethanol and 5.41 ± 0.79 mg/gDM of 3,5-diCQA at 95 °C, 57% of ethanol. The antioxidant activity of the extracts was also optimized by RSM. The highest antioxidant activity was achieved at 115 °C with 40% ethanol (more than 22mgTrolox/gDM). Finally, correlation between the antioxidant activity and the amount of CQAs was determined. FCR can be a great source of bioactive compounds with potential use as biobased antioxidant.

Selective Extraction of Sinapic Acid Derivatives from Mustard Seed Meal by Acting on pH: Toward a High Antioxidant Activity Rich Extract.

The aim of this paper is to study the effect of the pH on the extraction of sinapic acid and its derivatives from mustard seed meal. Solutions of acidic pH (pH 2), basic pH (pH 12) and distilled water (uncontrolled pH ~ 4.5) were tested at different percentages of ethanol. The maximum extraction yield for sinapic acid (13.22 µmol/g of dry matter (DM)) was obtained with a buffered aqueous solution at pH 12. For ethyl sinapate, the maximum extraction yield reached 9.81 µmol/g DM with 70% ethanol/buffered aqueous solution at pH 12. The maximum extraction yield of sinapine (15.73 µmol/g DM) was achieved with 70% ethanol/buffered aqueous solution at pH 2. The antioxidant activity of each extract was assessed by DPPH assay; the results indicated that the extracts obtained at pH 12 and at low ethanol percentages (<50%) exhibit a higher antioxidant activity than extracts obtained at acidic conditions. Maximum antioxidant activity was reached at pH 12 with buffer solution (11.37 mg of Trolox Equivalent/g DM), which confirms that sinapic acid-rich fractions exhibit a higher antioxidant activity. Thus, to obtain rich antioxidant extracts, it is suggested to promote the presence of sinapic acid in the extracts.

Elaboration of hemicellulose-based films: Impact of the extraction process from spruce wood on the film properties.

In this work, steam explosion (STEX), microwave assisted extraction (MAE) and high voltage electrical discharges (HVED) pretreatments have been evaluated for their impact on the physicochemical characteristics of extracted hemicellulosic polymers and on the resulting hemicellulose-based films. Extraction was carried out on spruce sawdust pre-soaked in water (WPS) or 1 M NaOH solution (SPS). The results have shown that STEX pretreatment gave the highest hemicellulose yields (64 and 66 mg g-1 of dry wood from WPS and SPS respectively) followed by MAE and HVED whilst MAE pretreatment produced the highest molecular mass (Mw~66 kDa of arabinoglucoronoxylans from SPS and 56 kDa for galactoglucomannans from WPS). A relatively high acetylation degree was found for STEX WPS (acetylation degree ≈ 0.35) and a high lignin content for STEX SPS (≈12%). Films have been produced by casting using sorbitol as plasticizer. Low oxygen barrier and light transmittance properties were observed for the films obtained from hemicelluloses extracted from SPS due to their high molecular mass and to intermolecular bonding of hemicelluloses and lignin.

High voltage electric discharges treatment for high molecular weight hemicelluloses extraction from spruce.

The aim of this work is to extract hemicelluloses polymers from spruce sawdust using High Voltage Electrical Discharges (HVED) pretreatment. HVED pretreatment was carried out in order to improve deconstruction of the wood matrix and to allow easier release of high molecular mass hemicelluloses. The results revealed the advantage of HVED activation step in the process of extraction. The yield of hemicellulose extraction increased with HVED treatment time. In fact, after 4 ms of HVED treatment time in 1 M NaOH solution, the yield obtained was higher as compared to the untreated sample (19 mg/g of dry matter and 15.8 mg/g of dry matter respectively). The molecular weights of extracted hemicelluloses are very high (55 kDa and 47 kDa for 4 ms of HVED-treatment in 1 M NaOH solution and water respectively). The use of different mediums of extraction with HVED pretreatment have revealed a selective solubilization of spruce hemicelluloses.