Pressurized Liquid Extraction Research Articles

Valorization of Guabirobeira leaf extracts (Campomanesia xanthocarpa) through pressurized liquid extraction and aqueous infusion: Assessment of phytochemical composition, antibacterial, and antioxidant activities

AbstractBACKGROUNDThe leaves of guabirobeira contain important phenolic and flavonoid compounds, known for their antioxidant, anti‐inflammatory, antibacterial, and antinociceptive activities. The purpose of this work was to obtain extracts from guabirobeira leaves through aqueous infusion (AI) and pressurized liquid extraction with water (PLE‐W), ethanol (PLE‐E), and a combination of water:ethanol ratio 1:1, v/v (PLE‐W:E). Subsequently, to identify the chemical compounds using liquid chromatography coupled with mass spectrometry, and to study the antioxidant activity in rat brain cells, thiobarbituric acid reactive substances (TBARS) and reactive oxygen species (ROS) antibacterial activity against Gram‐negative and Gram‐ positive bacteria is also seen.RESULTSAccording to the findings, all four extracts contained a significant amount of phytochemical compounds. Among them, the PLE‐W:E extract showed a higher concentration of flavonoids, demonstrating significant antioxidant activity in in vitro assays of TBARS and ROS in rat brain cells. It also exhibited antibacterial activity against both bacteria (Gram‐positive and Gram‐negative).CONCLUSIONAs a result, it can be concluded that guabirobeira leaf extracts hold promise as a potential source of bioactive compounds. These extracts can be applied across various sectors, including cosmetics and skincare products, pharmaceuticals, food and beverages, natural preservatives, and functional materials. By exploring these potential applications, valuable contributions can be made to the field of sustainable chemistry and pharmacy, furthering the utilization of guabirobeira leaf extracts in diverse industries. This approach also aligns with the promotion of environmentally friendly and sustainable practices.This article is protected by copyright. All rights reserved.

Optimization of Pressurized Liquid Extraction (PLE) Parameters for Extraction of Bioactive Compounds from Moringa oleifera Leaves and Bioactivity Assessment

Moringa oleifera leaves are rich sources of bioactive compounds with potential health benefits, including antioxidants and anti-inflammatory agents. Pressurized liquid extraction (PLE) stands out as a promising technique for effectively extracting valuable compounds from natural sources. In this study, we aimed to optimize PLE parameters, such as temperature, extraction duration, and pressure, to maximize bioactive compound (polyphenols, flavonoids, and ascorbic acid) yield from M. oleifera leaves and evaluate their antioxidant and anti-inflammatory activities. According to the outcomes of this research, the maximum achieved total polyphenol content was 24.10 mg gallic acid equivalents (GAE)/g of dry weight (dw), and the total flavonoid content was increased up to 19.89 mg rutin equivalents (RtE)/g dw. Moreover, after HPLC-DAD analysis, neochlorogenic and chlorogenic acids, catechin and epicatechin, rutin, and narirutin were identified and quantified. As far as the optimum ascorbic acid content is concerned, it was found to be 4.77 mg/g dw. The antioxidant activity was evaluated by three different methods: ferric reducing antioxidant power (FRAP), the DPPH method, and the anti-hydrogen peroxide activity (AHPA) method, resulting in 124.29 μmol ascorbic acid equivalent (AAE)/g dw, 131.28 μmol AAE/g dw, and 229.38 μmol AAE/g dw values, respectively. Lastly, the albumin denaturation inhibition was found to be 37.54%. These findings underscore the potential of PLE as an efficient extraction method for preparing extracts from M. oleifera leaves with the maximum content of bioactive compounds.

Advanced sample preparation and chromatographic techniques for analyzing plant-based bioactive chemicals in nutraceuticals

Since ancient times, humanity has used plants to cure diseases or maintain health. Nowadays, obtaining the bioactive components of plants and researching their effects continues at great speed. Plant-derived chemicals are studied with great interest in the food, pharmaceutical and cosmetic industries. The complexity of city life limits access to plants in their natural habitat. Nutraceuticals are indispensable products of our age to protect health. Many methods have been developed and successfully applied for extracting crude plant extracts and pure active substances included in nutraceuticals from plant tissues and their quantitative analysis. This study compiled the methods for obtaining plant extracts and active ingredients and the techniques developed for analyzing bioactive compounds. The extraction methods of plant-based bioactive chemicals (maceration, Soxhlet extraction, decoction, infusion, hydro distillation, ultrasound-assisted extraction (UAE), microwave-assisted extraction (MAE), enzyme-assisted extraction (EAE), pressurized liquid extraction (PLE), and supercritical fluid extraction (SFE)) were explained in detail, and some important plant-based bioactive chemicals and source plants were summarized in table form. Additionally, the studies using different analytical techniques such as high-performance liquid chromatography (HPLC), gas chromatography (GC), thin layer chromatography (TLC), mass spectrometry (MS), and ultra-performance liquid chromatography (UPLC) were discussed. Finally, evaluating its effectiveness in the extraction of different bioactive compounds and the prospects for more environmentally friendly methods alternative to traditional solvents were emphasized. This review covers the latest practices and new trends in analyzing plant-based bioactive chemicals in nutraceuticals over the last three years.

Tetraselmis chuii Edible Microalga as a New Source of Neuroprotective Compounds Obtained Using Fast Biosolvent Extraction.

Tetraselmis chuii is an EFSA-approved novel food and dietary supplement with increasing use in nutraceutical production worldwide. This study investigated the neuroprotective potential of bioactive compounds extracted from T. chuii using green biobased solvents (ethyl acetate, AcOEt, and cyclopentyl methyl ether, CPME) under pressurized liquid extraction (PLE) conditions and supercritical fluid extraction (SFE). Response surface optimization was used to study the effect of temperature and solvent composition on the neuroprotective properties of the PLE extracts, including anticholinergic activity, reactive oxygen/nitrogen species (ROS/RNS) scavenging capacity, and anti-inflammatory activity. Optimized extraction conditions of 40 °C and 34.9% AcOEt in CPME resulted in extracts with high anticholinergic and ROS/RNS scavenging capacity, while operation at 180 °C and 54.1% AcOEt in CPME yielded extracts with potent anti-inflammatory properties using only 20 min. Chemical characterization revealed the presence of carotenoids (neoxanthin, violaxanthin, zeaxanthin, α- and β-carotene) known for their anti-cholinesterase, antioxidant, and anti-inflammatory potential. The extracts also exhibited high levels of omega-3 polyunsaturated fatty acids (PUFAs) with a favorable ω-3/ω-6 ratio (>7), contributing to their neuroprotective and anti-inflammatory effects. Furthermore, the extracts were found to be safe to use, as cytotoxicity assays showed no observed toxicity in HK-2 and THP-1 cell lines at or below a concentration of 40 μg mL-1. These results highlight the neuroprotective potential of Tetraselmis chuii extracts, making them valuable in the field of nutraceutical production and emphasize the interest of studying new green solvents as alternatives to conventional toxic solvents.

Integrated Process for Schizochytrium Oil Extraction, Enzymatic Modification of Lipids and Concentration of DHA Fatty Acid Esters Using Alternative Methodologies.

Marine microalgae Schizochytrium sp. have a high content of docosahexaenoic acid (DHA), an omega-3 fatty acid that is attracting interest since it prevents certain neurodegenerative diseases. The obtention of a bioactive and purified DHA fatty acid ester using a whole-integrated process in which renewable sources and alternative methodologies are employed is the aim of this study. For this reason, lyophilized Schizochytrium biomass was used as an alternative to fish oil, and advanced extraction techniques as well as enzymatic modification were studied. Microalgal oil extraction was optimized via a surface-response method using pressurized liquid extraction (PLE) obtaining high oil yields (29.06 ± 0.12%) with a high concentration of DHA (51.15 ± 0.72%). Then, the enzymatic modification of Schizochytrium oil was developed by ethanolysis using immobilized Candida antarctica B lipase (Novozym® 435) at two reaction temperatures and different enzymatic loads. The best condition (40 °C and 200 mg of lipase) produced the highest yield of fatty acid ethyl ester (FAEE) (100%) after 8 h of a reaction attaining a cost-effective and alternative process. Finally, an enriched and purified fraction containing DHA-FAEE was obtained using open-column chromatography with a remarkably high concentration of 93.2 ± 1.3% DHA. The purified and bioactive molecules obtained in this study can be used as nutraceutical and active pharmaceutical intermediates of marine origin.

Antioxidant Activity of Carob Tree (Ceratonia siliqua L.) Leaf Extracts Obtained by Advanced Extraction Techniques

Carob (Ceratonia siliqua L.) is a widely spread Mediterranean evergreen tree whose plant parts are rich in bioactive compounds with potential for application in functional food production. Carob leaves are the least explored part of the plant, and the main compounds of interest are polyphenols. Advanced extraction techniques, such as pressurized liquid (PLE), microwave-assisted (MAE) and ultrasound-assisted (UAE) extraction have not been sufficiently explored for their potential in extracting these compounds. Therefore, the aim of this paper was to optimize the parameters (temperature and time) of PLE, MAE and UAE of carob leaf polyphenols, characterize the individual compounds by ultra-high performance liquid chromatography tandem mass spectrometry (UPLC-MS2) and determine the antioxidant activity of the extracts. The optimal temperature and time were 160 °C/5 min for PLE, resulting in a total phenolic content of 68.21 mg of gallic acid equivalents (GAE) g−1. For MAE and UAE, the optimal conditions were 70 °C/10 min, under which total phenolic contents of 78.80 and 55.98 mg GAE g−1 were achieved, respectively. A total of 26 compounds, represented mainly by myricetin, quercetin-3-rhamnoside and gallic acid, were identified in extracts obtained by all three extraction techniques. All extracts showed high antioxidant activity (0.46–1.05 and 0.50–0.58 mmol TE g−1 for FRAP and DPPH, respectively), which correlated with the polyphenolic content and was affected by the concentration of ascorbic acid (0.03–0.52 mg mL−1), confirming that carob leaf extracts obtained by advanced extraction possess high potential for application in functional food products.

Pressurized liquid extraction of glucosinolates from Camelina sativa (L.) Crantz by-products: Process optimization and biological activities of green extract

The cultivation of Camelina sativa (L.) Crantz is rapidly increasing due to oil production resulting in a substantial volume of by-products, which still have an interesting composition in secondary metabolites, especially glucosinolates. Therefore, a green extraction procedure of glucosinolates by Pressurised Liquid Extraction was developed and optimized using a chemometric approach. Furthermore, the glucosinolates were purified by solid phase extraction, and a preliminary study on bioaccessibility and bioavailability study was carried out to evaluate the resistance of the glucosinolates to the digestive process. The application of pressurised liquid extraction to the recovery of glucosinolates from camelina sativa by-product, is a green, automatic, and rapid method, representing a valid alternative to conventional extraction method to obtain ingredients for food industries.

Supercritical fluid and pressurized liquid extraction of spent tucumã-do-Amazonas (Astrocaryum aculeatum) almonds

Supercritical fluid (SFE) and pressurized liquid (PLE) extraction were applied to tucumã-do-Amazonas (Astrocaryum aculeatum) almonds (TAA). SFE was performed with CO2 at different pressures and temperatures, and the extracts were characterized for global yield, fatty acid and triacylglycerol profile, carotenoids, tocols concentration and thermal behavior. PLE was applied to the SFE-defatted almond at different temperatures and ethanol:water mixtures. The PLE extracts were characterized for global yield, total phenolics and antioxidant capacity. SFE global yield was 33 g extract/100 g dry TAA at 25 MPa and 40 °C, containing mainly triacylglycerols from lauric and myristic acids. Regarding tocols, SFE at 25 MPa and 50 °C resulted in 58 µg/g extract. PLE from defatted TAA achieved 24 g extract/100 g defatted TAA and the greatest phenolic content and antioxidant capacities with 75% ethanol at 110 °C. Therefore, TAA is a potential source of valuable compounds to be extracted by SFE and/or PLE.

Green Approach to Enhance the Recovery of Polyphenols from Blackcurrant and Bilberry Leaves: Evaluation of Microwave-Assisted and Pressurized Liquid Extraction.

The aim of the present study was to evaluate microwave-assisted (MAE) and pressurized liquid extraction (PLE) for the recovery of polyphenols from blackcurrant and bilberry leaves and the preservation of their antioxidant activity. The extractions were carried out varying the solvent/solid (SS) ratio, temperature and time. During MAE, increasing the SS ratio increased the polyphenol concentration in the extracts from blackcurrant and bilberry leaves, while increasing the temperature had a positive effect only on bilberry polyphenols. During PLE, only a temperature increase was a determining factor for the isolation of blackcurrant leave polyphenols. Based on polyphenol recovery, optimal extraction parameters were established resulting in a yield of 62.10 and 56.06 mg/g dw in the blackcurrant and bilberry MAE extracts and 78.90 and 70.55 mg/g dw in the PLE extracts. The optimized extracts were profiled by UPLC ESI MS2, and their antioxidant capacity was evaluated through FRAP, DPPH, ABTS and ORAC assays. The characterization of the extracts by UPLC ESI MS2 confirmed flavonols as the predominant compounds in both blackcurrant and bilberry leaves, while flavan-3-ols and procyanidins were the main compounds responsible for high antioxidant capacity as confirmed by the ABTS and ORAC assays. Due to the extract composition and antioxidant capacity, PLE proved to be a technique of choice for the production of blackcurrant and bilberry leave extracts with high potential for use as value-added ingredients in the food and nutraceutical industry.

Comparing green extraction methods for the recovery of protein-rich fraction from peach seeds (Prunus persica)

Peach processing generates significant volume of coproducts, such as the underutilized peach seeds, which are rich in fatty acids and protein. The recovery of protein-rich fractions from peach seeds is highly relevant because of the increasing demand for alternative non-animal protein sources. This study aimed to investigate different extraction techniques for protein recovery from the underestimated peach seeds, and evaluate the functionalities of the protein fraction. The peach seeds were defatted using the supercritical fluid extraction (SFE-CO2), with oily recovery up to 29.53% ± 0.45. Then, the protein fraction was recovered using the following methods: heat-stirred extraction (HSE) as a conventional method, and, as alternative procedures, microwave-assisted extraction (MAE), pressure liquid extraction (PLE), and ultrasound-assisted extraction (UAE) using NaOH solution as solvent. The PLE provided the highest protein content (95.10 % ± 0.98), followed by the HSE technique (55.09% ± 0.35). Furthermore, the PLE showed the best performance in techno-functional properties of the protein fraction: emulsion activity, foaming, turbidity, free sulfhydryl content, hydrophobicity, and color, compared to the classical HSE technique. Therefore, it is suggested that PLE (10 min) method recovered an isolated protein with better functional properties, providing promising result for protein purification. Therefore, PLE can be considered an alternative method to add value to underestimated peach seeds, conferring the upcycling concept.

Deep eutectic solvent-based pressurized liquid extraction combined with dispersive liquid-liquid microextraction of organophosphorus pesticide residues in egg powder prior to high-performance liquid chromatography analysis.

Herein, a deep eutectic solvent (DES)-based miniaturized pressurized liquid extraction in combination with DES-based dispersive liquid-liquid microextraction (DLLME) was developed for the extraction of organophosphorus pesticides (parathion-methyl, triazophos, parathion, diazinon, and phoxim) from egg powder samples prior to their analysis by a high-performance liquid chromatography-diode array detector. In this work, first, the analytes' extraction was done by a pressurized liquid phase extraction for effective extraction of the analytes from the solid matrix, and then they were concentrated on a DLLME for more concentration of the analytes to reach low limits of detections. The use of DESs was done in both steps to omit the use of toxic organic solvents. Satisfactory results including high extraction recoveries (74-90%), great repeatability (relative standard deviations equal or less than 4.3% and 5.3% for intra- and inter-day precisions), and low limits of detection (0.11-0.29ng/g) and quantification (0.38-0.98ng/g) were attained under the optimum conditions. Lastly, the suggested approach was utilized for the determination of the studied pesticides in various egg powder samples marketed in Tabriz, Iran.

Multiresidue determination and predicted risk assessment of emerging contaminants in sediments from Kongsfjorden, Svalbard

The present work provides the first data on the occurrence of different classes of pharmaceuticals and personal care products (PPCPs) in surface marine sediments from an Arctic fjord (Kongsfjorden, Svalbard Islands, Norway). The target compounds included: ciprofloxacin; enrofloxacin; amoxicillin; erythromycin; sulfamethoxazole; carbamazepine; diclofenac; ibuprofen; acetylsalicylic acid; paracetamol; caffeine; triclosan; N,N-diethyl-meta-toluamide; 17β-estradiol; 17α-ethinyl estradiol and estrone. Sampling was performed in the late summer, when high sedimentation rates occur, and over 5 years (2018–2022). Based on the environmental concentrations (MECs) found of emerging contaminants and the relative predicted no-effect concentrations (PNECs), an environmental risk assessment (ERA) for sediments was performed, including the estimation of the Risk Quotients (RQs) of selection and propagation of antimicrobial resistance (AMR) in this Arctic marine ecosystem. Sediments were extracted by Pressurized Liquid Extraction (PLE) and the extracts were purified by Solid Phase Extraction (SPE). Analytical determination was conducted with liquid chromatography-high-resolution mass spectrometry (HPLC-HRMS). PPCPs were detected in the sediments along the fjord in all the years investigated, with overall concentrations similar in most cases to those reported in urbanized areas of the planet and ranging from a minimum of 6.85 ng/g for triclosan to a maximum of 684.5 ng/g for ciprofloxacin. This latter was the only antibiotic detected but was the most abundant compound (32 %) followed by antipyretics (16 %), hormones (14 %), anti-inflammatories (13 %), insect repellents (11 %), stimulants (9 %), and disinfectants (5 %). Highest concentrations of all PPCPs detected were found close to the Ny-Ålesund research village, where human activities and the lack of appropriate wastewater treatment technologies were recognized as primary causes of local contamination. Finally, due to the presence in the sediments of the PPCPs investigated, the ERA highlights a medium (0.1 < RQ < 1) to high risk (RQ > 1) for organisms living in this Arctic marine ecosystem, including high risk of the spread of AMR.

Pressurized liquid extraction assisted by high-intensity ultrasound to obtain hesperidin from lime waste: Integration of in-line purification and on-line chromatographic analysis

Hesperidin is a phenolic compound usually found in citrus fruits, which is known for its anti-inflammatory and antioxidant properties. This bioactive compound has already been used to formulate medications to treat chronic venous insufficiency. In this work, through a system which allows the in-line coupling of the pressurized liquid extraction (PLE) and high-intensity ultrasound (HIUS) with solid phase extraction (SPE), and analysis by high-performance liquid chromatography with UV–Vis detector (HPLC-UV) in on-line mode, a method was developed to obtain, separate, and quantify hesperidin from the industrial waste of lime. An eco-friendly approach with water and ethanol as extraction solvents was used. Parameters such as temperature (80, 100, and 120 °C) and HIUS power (0, 200, and 400 W) were evaluated regarding hesperidin yield. In this context, the higher hesperidin yield (18.25 ± 1.52 mg/g) was achieved using water at a subcritical state (120 °C and 15 MPa). The adsorbent SepraTM C-18-E isolated hesperidin from the other extracted compounds employing 50% ethanol in the SPE elution. The possibility ofon-lineanalysis coupling a high-performance liquid chromatograph to an ultraviolet detector (HPLC-UV) system was studied and shown to be a feasible approach for developing integrated technologies. Conventional extractions and their antioxidant capacities were evaluated, highlighting the advantages of the HIUS-PLE-SPE extractive method. Furthermore, the on-linechromatographic analysis showed the potential of the HIUS-PLE-SPE- HPLC-UV system to quantify the extracted compounds in real time.

Pressurized liquid extraction of soybean oil using intermittent process with ethanol and hexane as solvent: Extraction yield and physicochemical parameters comparison

AbstractThis research demonstrates pressurized liquid extraction (PLE) in an intermittent process in obtaining soybean oil using less solvent than conventional extraction. Temperature (T), solvent rinse volume (VS), contact time between the solvent and the matrix (St) in each cycle and number of cycles (C) were screened. Yield, fatty acids profile (FAs), and triacylglycerols were evaluated. After preliminary testing, T and St were tested for yield while VS, C, and P were fixed at 60% of total volume of the fixed bed extractor, 3 cycles, and 10.34 MPa respectively. The highest oil recoveries were 94.40% (85°C, 13 min, with hexane) and 86.16% (80°C, 12 min, with ethanol). The mass ratio of solvent/feeds resulted in a yield increase of 1.47% (hexane) and 3.99% (ethanol). The concentration of β‐sitosterol (≤182.78 mg/100 g of oil, hexane; ≤71.64 mg/100 g of oil, ethanol) and the fatty acid profile were not affected by the different solvents or process. The main fatty acids were linoleic (≤51.12%, ethanol; ≤40.31%, hexane) and oleic (≤24.98%, ethanol; ≤26.62%, hexane). The main triacylglycerols identified were LLO, LLL, and OOL. The results indicate that soybean oil can be obtained by a new process that uses a safe and renewable solvent, indicating that PLE in an intermittent process can replace conventional extraction without changing the main characteristics of the oil, with good yield using less solvent.Practical applicationsThe practical application of this research is related to the possibility of demonstrating the feasibility of PLE in obtaining soybean oil using pressurized ethanol. The solvent used in most oilseed extraction plants is commercial hexane, a toxic and non‐renewable solvent. The experiments were carried out with pressurized hexane to demonstrate the economy of solvents and compare with the results obtained when pressurized ethanol was used as a solvent. The ethanol study aimed to show high extraction yields, even using a polar solvent in soybean oil extraction. High yields and oil characterization showed that it is possible to use a green and clean technology to obtain vegetable oils.

Grape Pomace Rich-Phenolics and Anthocyanins Extract: Production by Pressurized Liquid Extraction in Intermittent Process and Encapsulation by Spray-Drying.

A considerable number of grape pomaces are generated annually. It represents a rich source of bioactive compounds, such as phenolic compounds and anthocyanins. Pressurized liquid extraction (PLE) has emerged as a green technology for recovering bioactive compounds from vegetal matrixes. In our study, PLE parameters (temperature, number of cycles, and rinse volume) have been studied to produce grape pomace extracts with high bioactive content using an experimental design. The experimental data obtained were adjusted to linear and quadratic models. The first-order model was better in predicting anthocyanins contents (TA, R2 = 0.94), whereas the second-order model was predictive for total phenolic compounds (TPC, R2 = 0.96). The main process parameter for the recovery of bioactive compounds was temperature, and the results showed opposing behaviors concerning TPC and TA, as it is difficult to optimize conditions for both. The extract containing the higher concentration of TPC (97.4 ± 1.1 mg GAE/g, d.b.) was encapsulated by spray-drying using maltodextrin as wall material. Particles presented with a spherical shape (~7.73 ± 0.95 μm) with a recovery yield of 79%. The results demonstrated that extraction followed by encapsulation of grape pomace extract is a good strategy to simplify future applications, whether for food, cosmetics or pharmaceutical fields.

Exploring a Sustainable Process for Polyphenol Extraction from Olive Leaves.

Olive leaves are residues from pruning and harvesting and are considered an environmental management problems. Interestingly, these residues contain high polyphenol concentrations, which can be used to treat chronic diseases. However, these compounds are a technological challenge due to their thermolability and reactivity during extraction. Thus, this study assessed the use of pressurized liquid extraction (PLE) with green solvents like water-ethanol and water-glycerol mixtures (0-15%) at 50 °C and 70 °C to yield polyphenol-rich antioxidant extracts with reduced glucose and fructose content. The use of 30% ethanol at 70°C presented the highest polyphenol content (15.29 mg gallic acid equivalent/g dry weight) and antioxidant capacity, which was expressed as IC50 (half maximal inhibitory concentration): 5.49 mg/mL and oxygen radical absorbance capacity (ORAC): 1259 μmol Trolox equivalent/g dry weight, as well as lower sugar content (glucose: 3.75 mg/g dry weight, fructose: 5.68 mg/g dry weight) compared to water-glycerol mixtures. Interestingly, ethanol exhibits a higher degree of effectiveness in recovering flavanols, stilbenes and secoiridoids, while glycerol improves the extraction of phenolic acids and flavonols. Therefore, to enhance the efficiency of polyphenol recovery during the PLE process, it is necessary to consider its solvent composition and chemical structure.

Occurrence of high production volume chemicals and polycyclic aromatic hydrocarbons in urban sites close to industrial areas. Human exposure and risk assessment

Evaluating the occurrence of high production volume chemicals (HPVCs) and polycyclic aromatic hydrocarbons (PAHs) in the air is important because they carry a carcinogenic risk and can lead to respiratory or endocrine problems. Examples of HPVCs are organophosphate esters, benzosulfonamides, benzothiazoles, phthalate esters (PAEs), phenolic antioxidants and ultraviolet stabilizers. In this paper we develop a multi-residue method for determining HPVCs and PAHs in air samples via pressurized liquid extraction followed by gas chromatography-mass spectrometry. Air samples were collected by active sampling with high volume samplers using quartz fiber filter for the particulate matter (PM10) and polyurethane foams for gas phase. The compounds found at the highest concentrations were PAEs, with a concentration of up to 24 ng m−3 of DEHP in gas phase and up to 109 ng m−3 of DEHA in PM10. Non-carcinogenic risk assessment results ranged from 9.7E-05 to 9.5E-03 for most of the compounds studied. On the other hand, the results for carcinogenic risk showed that PAHs made the highest contribution.

Characterization, Antioxidant and Cytotoxic Evaluation of Demethoxycurcumin and Bisdemethoxycurcumin from Curcuma longa Cultivated in Costa Rica

The biological activities of curcuminoids, the main polyphenol constituents of Curcuma longa (turmeric), have been the subject of many studies in recent years. However, these studies have focused on the major active compound, curcumin (CUR), while other important constituents, demethoxycurcumin (DMC) and bisdemethoxycurcumin (BDM) have been less studied and reported in the literature regarding their bioactivity as well as their isolation and solid-state characterization. Hence, in this study, DMC and BDM were isolated using pressurized liquid extraction (PLE) followed by column chromatography and crystallization. HRMS and 1H and 13C NMR were used to characterize them. Solid-state characterization was performed through powder X-ray diffraction (PXRD), Fourier transform infrared spectroscopy (FT-IR), differential scanning calorimetry (DSC), and scanning electron microscopy (SEM) techniques. Further, powder dissolution profiles were performed in two media, antioxidant and cytotoxic activities were determined through 2,2-diphenyl-1-picrylhidrazyl (DPPH) and an MTT assay on gastric adenocarcinoma (AGS), colorectal adenocarcinoma (SW-620), and hepatocellular carcinoma (HepG2) cell lines. DMC and BDM were extracted from Curcuma longa cultivated in Costa Rica, using pressurized liquid extraction (PLE), then isolated and purified, combining column chromatography and crystallization techniques. The highly pure solids obtained were shown to be crystalline with an amorphous component. Although the PXRD pattern of BDM suggested a high amorphous component, the crystal exhibited a well-defined and faceted shape. Meanwhile, DMC crystallized in a botryoidal habit, and this constitutes the first report for this compound. On the other hand, BDM was slightly more soluble than DMC, which in turn showed an antioxidant IC50 value 28% higher than BDM (12.46 and 17.94 µg/mL, respectively). In respect to the cytotoxic effects, DMC showed a better IC50 value than BDM for both the SW-620 and AGS cell lines, while BDM exhibited a better IC50 value than DMC against the HepG2 cell line (64.7 μM). In terms of selectivity, BDM and DMC had the highest SI value for SW-620 cells compared to non-tumoral cells, while both compounds also displayed the best cytotoxic effect against these colon adenocarcinoma SW-620 cells, indicating BDM and DMC as potential chemotherapeutic drugs.

A Review: Subcritical Water Extraction of Organic Pollutants from Environmental Matrices.

Most organic pollutants are serious environmental concerns globally due to their resistance to biological, chemical, and photolytic degradation. The vast array of uses of organic compounds in daily life causes a massive annual release of these substances into the air, water, and soil. Typical examples of these substances include pesticides, polychlorinated biphenyls (PCBs), and polycyclic aromatic hydrocarbons (PAHs). Since they are persistent and hazardous in the environment, as well as bio-accumulative, sensitive and efficient extraction and detection techniques are required to estimate the level of pollution and assess the ecological consequences. A wide variety of extraction methods, including pressurized liquid extraction, microwave-assisted extraction, supercritical fluid extraction, and subcritical water extraction, have been recently used for the extraction of organic pollutants from the environment. However, subcritical water has proven to be the most effective approach for the extraction of a wide range of organic pollutants from the environment. In this review article, we provide a brief overview of the subcritical water extraction technique and its application to the extraction of PAHs, PCBs, pesticides, pharmaceuticals, and others form environmental matrices. Furthermore, we briefly discuss the influence of key extraction parameters, such as extraction time, pressure, and temperature, on extraction efficiency and recovery.

Pressurized liquid extraction and gas chromatography/mass spectrometry for determination of nitrated polycyclic aromatic hydrocarbons adsorbed on refractory diesel particles

A pressurized liquid extraction (PLE) technique was evaluated in this study and optimized using response surface methodology (RSM) for the determination of polycyclic aromatic hydrocarbons and their nitro derivatives from diesel particulate matter. A central composite design (CCD) was applied for the study of three parameters (temperature, nature of solvent and static time) and the optimal conditions were determined for a time of 9 min and a temperature of 145 °C and dichloromethane as extraction solvent. With the GC/MS analytical technique, the limits of detection (LOD) obtained range from 0.3 to 1.5 µg.L-1 for PAHs and from 4.6 to 8 µg.L-1 for nitrated PAHs. Also, this method allowed excellent recoveries of NPAH adsorbed on diesel soot particles (R ≥ 90%) using a mixture of solvents (1% acetic acid in pyridine). The PLE process developed in this research is quantitative and reproducible while using much less solvent than conventional extraction methods.