Pressurized Liquid Extraction Research Articles

Economic assessment of emerging extraction techniques: hybridization of high-pressure extraction and low-frequency ultrasound to produce piceatannol-rich extract from passion fruit bagasse

Low-frequency ultrasound has been efficiently applied to intensify high-pressure extraction processes. However, large-scale hybridization still is challenging. This work aims to present an economic feasibility study of two different extraction processes to produce a piceatannol-rich extract from yellow passion fruit bagasse – process A (supercritical fluid extraction + pressurized liquid extraction – SFE+PLE) and process B (SFE+PLE assisted by ultrasound – SFE+PLE-US). The SuperPro Designer software was employed to estimate the manufacturing cost (COM), productivity, and economic return rates, calculated for each overall extraction curve and different scales (50, 200, and 500 L). Process A showed economically viable, while process B showed infeasible at a 20% minimum acceptable rate of return. The lowest COM and better economic return were obtained with process A at 75 °C, 500 L, and 90 min. In addition, a sensitivity study was carried out, indicating the possibility of selling the extract below the market price, representing a competitive differential to implement the extraction process at large scales. It is noteworthy that up to now, the economic feasibility of PLE-US on a large scale has not yet been performed, so this work represents a starting point for studies of PLE-US hybridization on large scales.

Valorization of tamarind seeds using high-pressure extraction methods to obtain rich fractions in fatty acid and phenolic compounds

Supercritical fluid extraction (SFE) and pressurized liquid extraction (PLE) were combined, in a biorefinery approach, to recover the nonpolar and polar fractions from tamarind seeds, which represent 25–40% of processed fruit. Total phenolic content (TPC), antioxidant capacity, and chemical composition were evaluated, and compared with values from Soxhlet (SOX) samples. The nonpolar lipid fraction, obtained by SFE with CO2, contains unsaturated and saturated fatty acids, similar to sample by SOX-hexane. The polar phenolic fraction, recovered by PLE-ethanol (60 °C / 10 MPa), presented high TPC (305.1 mg GAE·g-1) and antioxidant capacity, compared to SOX-ethanol sample. Combining SFE and PLE increased the TPC (421.8 mg GAE·g-1) and antioxidant capacity (2208.3–4412.5 µmol TEAC·g-1) of final extract. Chemical analysis confirmed high concentrations of organic acids and phenolic compounds (epicatechin, procyanidin and rutin) from ethanolic extracts. The biorefinery approach provides data for tamarind seeds fractionation, valuing this underestimated by-product by high-pressure methods.

Evaluation of Techniques for Intensifying the Process of the Alcoholic Extraction of Coffee Ground Oil Using Ultrasound and a Pressurized Solvent.

Ultrasound-assisted extraction (UAE) and pressurized liquid extraction (PLE) techniques were evaluated and compared with conventional extraction for obtaining spent coffee ground oil (SCGO). The use of absolute ethanol (ET0) and hydrated ethanol (ET6) as solvents, two levels of SCG mass ratio:solvent, 1:4 (U4) and 1:15 (U15), and ultrasound powers of 0, 200, 400, and 600 W were tested. ET0 and U15 resulted in higher extraction yields of SCGO (YSCGO, 82%). A positive effect of sonication on YSCGO was observed only for condition U4. UAE resulted in defatted solids (DS) with higher apparent density values, corroborating the increase in the amount of smaller diameter particles due to sonication. The micrographs showed changes in the surfaces of the solids from the UAE and PLE, although the crystalline structures of the DS were not altered. UAE and PLE, compared to conventional extraction, did not allow significant gains in terms of YSCGO and, consequently, in the number of contact stages in an extractor configured in cross-currents.

Neuroprotective potential of terpenoid-rich extracts from orange juice by-products obtained by pressurized liquid extraction.

Pressurized liquid extraction (PLE) conditions were optimized to improve the recovery of orange (Citrus sinensis) by-products terpenoids. The neuroprotective potential of the PLE extracts were tested against a set of in-vitro assay (antioxidant (ABTS), reactive oxygen/nitrogen species (ROS/RNS)) as well as enzymatic tests (acetylcholinesterase (AChE), butyrylcholinesterase (BChE) and lipoxygenase (LOX)). Gas chromatography coupled to high-resolution mass spectrometry (GC-q-TOF-MS) analysis revealed a higher enrichment in mono- and sesquiterpenoids of the PLE extracts with the highest neuroprotection capacity. In-silico molecular docking analysis showed the specific interaction of representative terpenoids with enzymes active sites. The results demonstrate that the selected extract at 100°C and 30 minutes possesses high antioxidant (ABTSIC50=13.5μgmL-1; ROSIC50 = 4.4μgmL-1), anti-cholinesterase (AChEIC50=137.1 vg L-1; BChEIC50=147.0μgmL-1) and anti-inflammatory properties (against IL-6 and LOXIC50=76.1μgmL-1), with low cytotoxicity and protection against L-glutamic acid in cell models.

Non-conventional techniques for the extraction of antioxidant compounds and lycopene from industrial tomato pomace (Solanum lycopersicum L.) using spouted bed drying as a pre-treatment

This study aimed to use the non-conventional microwave-assisted extraction (MAE) and pressurized liquid extraction (PLE) techniques for recovering bioactive compounds from tomato pomace, a valuable agro-industrial waste. The raw material was previously dried using a spouted bed dryer and then submitted to extraction with green solvents. A response surface methodology (RSM) performed the optimization of MAE and PLE. Next, the yield and the antioxidant activity results were maximized, and the lycopene content of the optimum MAE and PLE extracts was assessed by high-performance liquid chromatography (HPLC). Additionally, a fraction of raw material was oven dried as a comparison. The PLE extract exhibited the highest antioxidant activity, whereas the MAE extract showed the highest lycopene content (59.66 µg lycopene/g extract), which represents a 66.93% lycopene recovery compared to a standard technique with acetone. The remarkable results show that the non-conventional drying and extraction techniques were effective in valorizing this neglected material.

Pressurized aqueous solutions of deep eutectic solvent (DES): A green emergent extraction of anthocyanins from a Brazilian berry processing by-product

Deep eutectic solvents (DES) are emergent solvents with high extractability of bioactive compounds. Therefore, anthocyanin rich-fractions were recovered from jaboticaba peels by combining aqueous solutions of DES and pressurized liquid extraction (PLE). The extraction occurred at 10 MPa, 12 min, with conditions optimized through response surface methodology: 47% DES concentration, 90 °C, and 5.3 mL/min flow rate. PLE with different DES (choline chloride combined with propylene glycol or malic acid) solutions were compared to conventional solvents (water and acidified water) concerning yield, thermostability, antioxidant, anti-diabetic, and anti-obesity activities. DES solutions presented anthocyanin yields up to 50% higher than conventional solvents. ChCl:Ma, with the highest anthocyanin stability (Ea = 77.5 kJ.mol−1), was a promising solvent concerning color, anti-diabetic and anti-obesity potential. Environmental analysis by Green Certificate and EcoScale indicated PLE with DES solutions is a green and efficient approach to recover anthocyanin from jaboticaba peel, providing useful extracts.

Sustainable Extractions for Maximizing Content of Antioxidant Phytochemicals from Black and Red Currants.

Sustainable extraction techniques (ultrasound-assisted extraction (UAE), microwave-assisted extraction (MAE), and pressurized-liquid extraction (PLE)) were applied and compared with conventional solvent extraction to evaluate their efficiency in maximizing the bioactive compound content and antioxidant activity of black and red currants. The influence of ethanol concentrations (30%, 50%, 70%) were studied in all extraction methods, while different temperatures (30, 50, 70 °C/80, 100, 120 °C) were evaluated in UAE and PLE, respectively. Generally, higher total phenolics were determined in black currant extracts (1.93–3.41 g GAE/100 g) than in red currant extracts (1.27–2.63 g GAE/100 g). The results showed that MAE was the most efficient for the extraction of bioactives from black currants, with 3.41 g GAE/100 g and 0.7934 g CE/100 g, while PLE provided the highest TP and TF for black currant samples (2.63 g GAE/100 g and 0.77 g CE/100 g). Extracts obtained by MAE (10 min, 600 W, 30% ethanol) and PLE (50% ethanol, 10 min, 120 °C) had the highest antioxidant activity, as determined by various in vitro assays (DPPH, FRAP, and ABTS). In conclusion, sustainable extraction techniques can be considered an efficient tool to maximize the content of bioactive antioxidants from black and red currants.

Pressurized liquid extraction of phenolics from Pseuderanthemum palatiferum (Nees) Radlk. leaves: Optimization, characterization, and biofunctional properties

In this study, the pressurized liquid extraction (PLE) of total phenolic content (TPC), gallic acid (GA), and p-hydroxybenzoic acid (PHBA) from Pseuderanthemum palatiferum (Nees) Radlk. leaves was optimized using response surface methodology. The extract at the optimum conditions of TPC, namely OP, was characterized using GC–MS, HPLC, and spectrophotometry analysis. Furthermore, bio-functional properties of the OP, including antioxidant, antimicrobial, antihypertensive activities, and cytotoxicity against cancer and normal cell lines, were also investigated. The results showed that all extraction models were appropriate in predicting the extraction processes (p < 0.05) of the target compounds. In addition to TPC, GA, and PHBA, the OP also contains a high amount of other valuable components that contributed to its highly biological activities. Moreover, the OP was nontoxic on HaCaT cells with a concentration of no more than 1000 µg/mL. From the obtained results, PLE proved to be a suitable technique for the recovery of bioactive compounds from P. palatiferum leaves.

Application of Pressurized Liquid Extractions to Obtain Bioactive Compounds from Tuber aestivum and Terfezia claveryi

A PLE (pressurized liquid extraction) method was adjusted following a full-factorial experimental design to obtain bioactive-enriched fractions from Tuber aestivum and Terfezia claveryi. Temperature, time and solvent (water, ethanol and ethanol–water 1:1) parameters were investigated. The response variables investigated were: obtained yield and the levels of total carbohydrate (compounds, β-glucans, chitin, proteins, phenolic compounds and sterols). Principal component analysis indicated water solvent and high temperatures as more adequate parameters to extract polysaccharide-rich fractions (up to 68% of content), whereas ethanol was more suitable to extract fungal sterols (up to 12.5% of content). The fractions obtained at optimal conditions (16.7 MPa, 180 °C, 30 min) were able to protect Caco2 cells from free radical exposure, acting as antioxidants, and were able to reduce secretion of pro-inflammatory cytokines in vitro: IL-6 (50%), and TNFα (80% only T. claveryi ethanol extract), as well as reduce high inhibitory activity (T. aestivum IC50: 9.44 mG/mL).

Cosmeceutical Potential of Major Tropical and Subtropical Fruit By-Products for a Sustainable Revalorization.

The increasing production of tropical fruits followed by their processing results in tons of waste, such as skins or seeds. However, these by-products have been reported to be rich in bioactive compounds (BACs) with excellent properties of interest in the cosmeceutical industry: antioxidant, anti-aging, anti-inflammatory, antimicrobial and photoprotective properties. This review summarizes the tropical fruits most produced worldwide, their bioactive composition and the most important and studied therapeutic properties that their by-products can contribute to skin health, as well as the different approaches for obtaining these compounds using techniques by conventional (Soxhlet, liquid-liquid extraction or maceration) and non-conventional extractions (supercritical fluid extraction (SFE), ultrasound-assisted extraction (UAE), microwave-assisted extraction (MAE), pressurized liquid extraction (PLE) and two-phase aqueous system), followed by their identification by HPLC-MS or GC-MS analysis. Moreover, this work encompasses several studies that may prove the effects of seeds and skins from tropical fruits against oxidative stress, hyperpigmentation, acne, aging or UV radiation. Therefore, the investigation of functional components present in tropical fruit by-products under a circular bioeconomy model could be of great interest for the cosmeceutical industry and a very promising option for obtaining new cosmeceutical formulations.

Protein valorization from ora-pro-nobis leaves by compressed fluids biorefinery extractions

Ora-pro-nobis (Pereskia aculeata) leaves were selected as raw material for biorefinery application based on compressed fluid extractions with green solvents. The fractionation followed the sequential processes: (1) Supercritical fluid extraction (SFE) with CO2, (2) Gas expanded liquid extraction (GXL), using CO2:Ethanol, and pressurized liquid extraction (PLE) with ethanol, and (3) Subcritical water extraction (SWE). In vitro analysis of total phenolic and total carotenoid contents and antioxidant activity (DPPH and ORAC) were assessed, stipulating PLE method as the second step of the sequential extractions. Total protein and carbohydrate contents were evaluated from SWE samples. Phenolics profile from PLE and SWE samples was assessed by LC-DAD-ESI-MS/MS, identifying 8 phenolic compounds, with quercetin, isorhamnetin and kaempferol as the main detected flavonoids. SWE at 150 and 185 °C provided the highest protein recovery, as the third step in a sequential process.

Antioxidant activity of extracts obtained by high-pressure extraction procedures from Asparagus stipularis Forssk

Roots and rhizomes of Asparagus stipularis Forssk were separately extracted using supercritical CO2 extraction (SCCO2) and pressurized liquid extraction (PLE) and their Total Phenols Content and antioxidant potential was investigated. The results indicated that the roots and rhizomes are a potential source of natural antioxidants. The PLE method gave better extraction yields than SFE and its fractions present the highest antioxidant activity. Direct evaluation of antioxidant capacity using the QUENCHER procedure showed that also the solid residue of the plant material remaining after the SCCO2 and PLE may be of interest as a source of valuable phytochemicals.

Comparative study of factors affecting the recovery of proteins from malt rootlets using pressurized liquids and ultrasounds

Malt rootlets (MR) are a waste from brewing with high protein content. This work proposes to study the impact of extracting parameters on the recovery of proteins and the characteristics of extracts from MR using ultrasound-assisted extraction (UAE) and pressurized liquid extraction (PLE). A Box-Behnken experimental design was employed to study the effect of extracting parameters on the protein yield, while characterization comprised the study of antioxidant properties, the identification of extracted proteins using high-resolution tandem mass spectrometry, and the evaluation of the co-extraction of phenolic compounds. Protein extraction was promoted at an ultrasounds amplitude of 68%, for 20 min at 52 °C in UAE, while adding 33% ethanol resulted in the highest yield in PLE. While UAE extracted 53 ± 5% of MR proteins, PLE reached a 73 ± 7%, using more sustainable conditions. Significant antioxidant activities were observed in the PLE extract, although undermined by gastrointestinal digestion. Proteomic analysis detected 68 proteins from Hordeum vulgare in the UAE extract and 9 in the PLE extract. Proteins in MR are very different to that from barley grains or brewer's spent grains. PLE also co-extracted phenolic compounds while this was not significant by UAE.

Extraction and Pyrolysis-GC-MS analysis of polyethylene in samples with medium to high lipid content

While it is recognised that humans are constantly exposed to plastics, there are limitations in understanding the extent of this exposure, particularly dietary exposure. This lack of information is partly due to challenges with the analysis of complicated matrices. This study aimed to assess the impact of medium to high lipid content (&gt; 3%) food samples on the accurate quantification of polyethylene (PE), using pyrolysis-gas chromatography mass spectrometry, and develop an alternative sample processing strategy. Analysis of saturated, monounsaturated and polyunsaturated fats was demonstrated to form the same pyrolysis products as PE, producing a significant interference hindering quantification. An extraction protocol was developed that involves enzyme digestion to break the lipids into smaller chain fatty acids, removal of these interferences with pressurised liquid extraction washes, before a final extraction of the PE by pressurised liquid extraction. This new method was validated through the analysis of three medium- to high-fat content foods: cow’s milk, eggs and lamb meat, where PE recoveries were acceptable (104% to 127%). Method detection limits were also significantly reduced from 1.9 to 0.05 µg/injection (380 to 10 µg/g) with the new protocol, through the removal of matrix background. PE traces were observed in the three food matrices of 72-240 µg/g, significantly reduced as compared to samples extracted with the old method where concentrations of 12-32 mg/g were calculated, demonstrating the potential for overestimation of dietary exposure. Finally, a simple protocol is reported for future studies to (i) determine if an interference is present and (ii) sample processing methods to remove identified interferences.

Conventional and emerging techniques for extraction of bioactive compounds from fruit waste

Fruit residues (peel, seed, and pulp residues) have in their composition several compounds such as polyphenols, carotenoids, fibres, and lipids which, due to their functional properties, these compounds make them potential sources of natural additives. The great technological challenge is to use the most suitable techniques for extracting these compounds. In this paper, definitions, advantages, and disadvantages of conventional (maceration, soxhlet extraction, hydrodistillation) and emerging (Ultrasonic-Assisted Extraction (UAE), Microwave-Assisted Extraction (MAE), Supercritical Fluid Extraction (SFE), Pressurized Liquid Extraction (PLE), and Pulsed Electric Field (PEF)) techniques for the extraction of bioactive compounds from fruit residues will be shown. Some emerging techniques are based on non-thermal process, reduced use of energy and the implementation of no toxic solvents, being considered “green” or “clean” technologies. These ones are particularly interesting to extract heat-labile compounds. In addition, enzyme-assisted extraction and extractions through fermentation processes (submerged or solid-state fermentation) will be highlighted as alternative to promote the release of compounds from fruit residues not extracted by other techniques. These extractions techniques can enhance the content of bioactive compounds by increased their concentrations, as well as new compounds can be formed after these processes. It has been proven that the emerging techniques and fermentative processes, as alternative to conventional methods, are promising to extract bioactive compounds from fruit residues, since that these techniques improved extraction yields, reduced processing times, and reduced environmental damage are achieved.

Does size matter? Quantification of plastics associated with size fractionated biosolids

This study investigated the occurrence and contribution of plastic particles associated with size fractionated biosolids to the total concentration in biosolids (treated sewage sludge) samples collected from 20 wastewater treatment plants (WWTP) across Australia. This was achieved through sequential size fractionation of biosolids samples to quantify the mass concentration of 7 common plastics across a range of biosolids size fractions, including below 25 μm which has not been assessed in many previous studies. Quantitative analysis was performed by pressurized liquid extraction followed by pyrolysis coupled to gas chromatography - mass spectrometry. Of the total quantified plastics (Σ7plastics), the greatest proportion (27%) of the total mass were identified in the nominal <25 μm sized biosolids fraction. Polyethylene dominated the polymer mass in every size fraction, even though profiles varied between WWTPs. When comparing the sum of all sites for each sized biosolids fraction, the plurality of the polyethylene, polyvinyl-chloride, polystyrene, polypropylene, polycarbonate, and polyethylene-terephthalate concentrations were associated with the smallest size fraction (<25 μm). We confirm for the first time the presence of plastic particles in biosolids below a size fraction that is not captured by many methods. This is important, because of the potential greater significance of plastics in the low sizes to environmental and human health.

Quantification and Ecological Risk Assessment of Colloidal Fullerenes Nanoparticles in Sediments by Ultrasonic-Assisted Pressurized Liquid Extraction and High Performance Liquid Chromatography.

Fullerenes engineered nanomaterials are regarded as emerging environmental contaminants. This is as their widespread application in many consumer products, as well as natural release, increases their environmental concentration. In this work, an ultrasonic-assisted pressurized liquid extraction (UAPLE) method followed by high performance liquid chromatography with ultraviolet-visible detector (HPLC-UV-vis) was developed for extraction and determination of fullerene in sediments. The method was validated and found to be suitable for environmental risk assessment. Thereafter, the method was used for the determination of fullerene (C61-PCBM) in sediment samples collected from Umgeni River, South Africa. The current method allows for adequate sensitivity within the linear range of 0.01–4 µg g−1, method limit detection of 0.0094 µg g−1 and recoveries ranged between 67–84%. All the parameters were determined from fortified sediments samples. The measured environmental concentration (MEC) of fullerene in the sediment samples ranged from not detected to 30.55 µg g−1. To the best of our knowledge, this is the first report on the occurrence and ecological risk assessment of carbonaceous fullerene nanoparticles in African sediments and biosolids.

HRMS Characterization, Antioxidant and Cytotoxic Activities of Polyphenols in Malus domestica Cultivars from Costa Rica.

There is increasing interest in research into fruits as sources of secondary metabolites because of their potential bioactivities. In this study, the phenolic profiles of Malus domestica Anna and Jonagold cultivars from Costa Rica were determined by Ultra Performance Liquid Chromatography coupled with High Resolution Mass Spectrometry (HRMS) using a quadrupole-time-of-flight analyzer (UPLC-QTOF-ESI MS), on enriched-phenolic extracts from skins and flesh, obtained through Pressurized Liquid Extraction (PLE). In total, 48 different phenolic compounds were identified in the skin and flesh extracts, comprising 17 flavan-3-ols, 12 flavonoids, 4 chalcones, 1 glycosylated isoprenoid and 14 hydroxycinnamic acids and derivatives. Among extracts, the flesh of Jonagold exhibits a larger number of polyphenols and is especially rich in procyanidin trimers, tetramers and pentamers. Evaluating total phenolic content (TPC) and antioxidant activities using ORAC and DPPH procedures yields higher values for this extract (608.8 mg GAE/g extract; 14.80 mmol TE/g extract and IC50 = 3.96 µg/mL, respectively). In addition, cytotoxicity evaluated against SW620 colon cancer cell lines and AGS gastric cancer cell lines also delivered better effects for Jonagold flesh (IC50 = 62.4 and 60.0 µg/mL, respectively). In addition, a significant negative correlation (p < 0.05) was found between TPC and cytotoxicity values against SW620 and AGS adenocarcinoma (r = −0.908, and −0.902, respectively). Furthermore, a significant negative correlation (p < 0.05) was also found between the number of procyanidins and both antioxidant activities and cytotoxicity towards SW620 (r = −0.978) and AGS (r = −0.894) cell lines. These results align with Jonagold flesh exhibiting the highest abundance in procyanidin oligomers and yielding better cytotoxic and antioxidant results. In sum, our findings suggest the need for further studies on these Costa Rican apple extracts—and particularly on the extracts from Jonagold flesh—to increase the knowledge on their potential benefits for health.

Anti-Hyperalgesic Properties of Menthol and Pulegone.

Context: Menthol, the main monoterpene found in Mentha piperita L. (M. piperita) is known to modulate nociceptive threshold and is present in different curative preparations that reduce sensory hypersensitivities in pain conditions. While for pulegone, a menthol-like monoterpene, only a limited number of studies focus on its putative analgesic effects, pulegone is the most abundant monoterpene present in Calamintha nepeta (L.) Savi (C. nepeta), a plant of the Lamiaceae family used in traditional medicine to alleviate rheumatic disorders, which counts amongst chronic inflammatory diseases. Objectives: Here, we analyzed the monoterpenes composition of C. nepeta and M. piperita. We then compared the putative anti-hyperalgesic effects of the main monoterpenes found, menthol and pulegone, in acute inflammatory pain conditions. Methods: C. nepeta and M. piperita extracts were obtained through pressurized liquid extraction and analyzed by gas chromatography-mass spectrometry. The in vitro anti-inflammatory activity of menthol or pulegone was evaluated by measuring the secretion of the tumour necrosis factor alpha (TNF α) from LPS-stimulated THP-1 cells. The in vivo anti-hyperalgesic effects of menthol and pulegone were tested on a rat inflammatory pain model. Results: Pulegone and menthol are the most abundant monoterpene found in C. nepeta (49.41%) and M. piperita (42.85%) extracts, respectively. In vitro, both pulegone and menthol act as strong anti-inflammatory molecules, with EC50 values of 1.2 ± 0.2 and 1.5 ± 0.1 mM, respectively, and exert cytotoxicity with EC50 values of 6.6 ± 0.3 and 3.5 ± 0.2 mM, respectively. In vivo, 100 mg/kg pulegone exerts a transient anti-hyperalgesic effect on both mechanical (pulegone: 274.25 ± 68.89 g, n = 8; vehicle: 160.88 ± 35.17 g, n = 8, p < 0.0001), thermal heat (pulegone: 4.09 ± 0.62 s, n = 8; vehicle: 2.25 ± 0.34 s, n = 8, p < 0.0001), and cold (pulegone: 2.25 ± 1.28 score, n = 8; vehicle: 4.75 ± 1.04 score, n = 8, p = 0.0003). In a similar way, 100 mg/kg menthol exerts a transient anti-hyperalgesic effect on both mechanical (mechanical: menthol: 281.63 ± 45.52 g, n = 8; vehicle: 166.25 ± 35.4 g, n = 8, p < 0.0001) and thermal heat (menthol: 3.65 ± 0.88 s, n = 8; vehicle: 2.19 ± 0.26 s, n = 8, <0.0001). Conclusion: Here, we show that both pulegone and menthol are anti-inflammatory and anti-hyperalgesic monoterpenes. These results might open the path towards new compound mixes to alleviate the pain sensation.

Pressurized Liquid Extraction of Hemp Residue and Purification of the Extract with Liquid-Liquid Extraction

The first semi-continuous Pressurized Liquid Extraction (PLE) of hemp threshing residue with ethanol was carried out according to a 32 full factorial experimental design with pressure and temperature as independent variables at 8-10-12 MPa and 323-333-343 K, respectively. The total- and cannabidiol (CBD) yield curves were fitted to the modified two-parameter Brunner equation. Best results, concerning CBD, can be achieved at 12 MPa and 343 K. Solvent mass-consumption and operation time were considerably decreased compared to a previous supercritical fluid extraction study on the same material. Furthermore, the concentration profiles were evaluated to study the mass transfer. The winterized dry extracts were further studied in a methanol-hexane-water ternary system concerning CBD distribution ratio, showing high methanol dependency.