Search Results (593)

Alkyl-substituted pyridines are ubiquitous structural motifs found in natural products, pharmaceuticals, agrochemicals, and functional organic materials. However, their direct synthesis remains challenging because of the electron-deficient nature of the pyridine ring and the harsh conditions typically required for conventional carbonyl-to-alkane reduction. Herein, we report a mild and environmentally benign Pd/C–H₂ catalytic system that enables one-pot oxidative aromatization–deoxygenation of dihydropyridinedione derivatives to afford alkyl-substituted pyridines. The transformation proceeds efficiently at room temperature under atmospheric hydrogen pressure using ethanol as a green solvent, delivering the desired products in up to 91% isolated yield. The protocol exhibits broad substrate scope, high chemoselectivity, operational simplicity, and excellent catalyst recyclability. Mechanistic studies, including hydrogen-free control experiments and intermediate isolation, support a sequential Pd-mediated pathway involving oxidative aromatization, stepwise hydrogen-transfer reduction, and final deoxygenation, with water as the sole stoichiometric by-product. This method provides a sustainable and scalable alternative to classical harsh or reagent-intensive deoxygenation strategies for the synthesis of alkyl-substituted pyridines. Full article

Background: The development of greener synthetic routes to active pharmaceutical ingredients (APIs) is a key challenge in sustainable chemistry. Methods: In this work, we explored the use of deep eutectic solvents (DESs) in the multi-step synthesis of a fluoroquinolone following the Grohe method. Results: Several steps of the synthetic sequence were successfully carried out using DESs, achieving moderate to good yields, while operating under mild reaction conditions and reducing purification requirements. Overall, the use of DESs led to an overall yield of up to 43%. A comprehensive greenness assessment, combining EcoScale scoring and the GSK and CHEM21 solvent selection guides, confirmed the superior sustainability profile of DESs, reflecting their lower toxicity, biodegradability, and reduced energy demands. Conclusions: These findings establish DESs as promising, eco-friendly alternatives to volatile and hazardous organic solvents for the synthesis of quinolone derivatives, offering a valuable step toward more sustainable pharmaceutical manufacturing. Full article

An innovative dispersive liquid–liquid microextraction technique utilizing a solid dispersion was established for the quantification of triazine herbicides in environmental water samples. Naturally derived monoterpenoids were utilized as eco-friendly extraction solvents, markedly decreasing the reliance on harmful extraction solvents. A small amount of Pop Rocks candy served as a solid dispersant; the rapid release of carbon dioxide promoted the generation of fine monoterpenoid droplets, effectively replacing conventional hazardous liquid dispersants. The solidification technique of floating organic droplets facilitated the effective phase separation of monoterpenoids from aqueous samples, thereby obviating the need for centrifugation. Triazine herbicides exhibited good linearity within the concentration range of 0.008–0.8 mg/L with correlation coefficients above 0.99 and detection limits of 0.002 mg/L. The proposed method was effectively implemented on surface and groundwater samples, attaining recoveries between 86.4% and 98.0%. Molecular docking analysis suggests a spontaneous binding between the monoterpenoid and triazine herbicides. A comprehensive green assessment utilizing two evaluation tools confirmed the excellent environmental performance of the method. This technique offers superior greenness and simplicity compared with conventional techniques, demonstrating strong potential for application in the environmental analysis of pesticide residues. Full article

The rapid expansion of China’s photovoltaic (PV) industry has led to a significant increase in decommissioned PV modules. To address the high energy consumption and environmental impact of traditional recycling techniques, this study proposes a novel method that integrates DMPU solvent recycling with pyrolysis for recovering PV cell sheets. DMPU, an organic solvent with low volatility, non-toxicity, and excellent recyclability, was used in this study. The effects of temperature and treatment duration on the structural integrity of silicon cell sheets were systematically evaluated, establishing optimal parameters: immersion in DMPU at 200 °C for 60 min, followed by pyrolysis at 480 °C for 60 min. A case study was conducted on a small-scale recycling facility with a daily processing capacity of 200 standard PV panels, encompassing system boundaries such as transportation, pretreatment, and pyrolysis. The recycling process consumed 2.14 × 10⁹ kJ of energy annually, reducing CO₂ emissions by 9357.2 tons. Compared to conventional methods such as pyrolysis, mechanical dismantling, and chemical dissolution, the proposed approach employing a green, recyclable solvent markedly reduces energy consumption and carbon emissions, offering notable environmental benefits. Full article

This study demonstrates a sustainable, integrated pathway for valorizing carrot processing by-products through solvent-free lycopene recovery. The approach combines optimized infrared dehydration with ultrasound-assisted extraction using edible oils. Drying kinetics were modeled at multiple temperatures, with the Midilli model providing the best fit (R² > 0.99), enabling accurate prediction of moisture content removal while preserving bioactive compounds. Optimization via Box–Behnken design identified efficient extraction conditions (49.7–60 °C, 10 mL/g, 60 min), achieving lycopene equivalent (LE) yields of 3.07 to 5.00 mg/kg oil. Sunflower and blended oils showed comparable performance under maximum sonication power (240 W), with strong agreement between predicted and experimental yields. The process generated two valuable outputs: a functional lycopene-enriched oil and an exhausted carrot powder co-product, the latter retaining its crude fiber content despite other compositional changes. This research presents a scalable, green methodology that aligns with circular economy principles, transforming agro-industrial waste into functional food ingredients without organic solvents. Thus, the developed approach establishes a transferable model for the sustainable valorization of carotenoid-rich residues, contributing directly to greener food production systems. By providing a practical technological framework to convert waste into wealth, this work supports the fundamental transition toward a circular bioeconomy. Full article

In the present study, ten type-V natural deep eutectic solvents (NADESs) were synthesized and comprehensively characterized, based on urea as a hydrogen-bond acceptor and three different groups of donors—glycerol, organic carboxylic acids, and carbohydrates. Their physicochemical parameters, spectral characteristics (FTIR), surface tension, and solvatochromic properties were determined using Nile Red, betaine 30, and Kamlet–Taft parameters. The densities of the systems (1.243–1.361 g/cm³) and the high values of molar refraction and polarizability indicate the formation of highly organized hydrogen-bonded networks, with the incorporated carboxyl and hydroxyl groups enhancing the structural compactness of the NADES. Surface tension varied significantly (46.9–80.3 mN/m), defining systems with low, medium, and high polarity. Solvatochromic analysis revealed high E_NR, E_T(30), and E_T^N values, positioning all NADES as highly polar media, comparable or close to water, but with distinguishable H-bond donating/accepting ability depending on the third component. The normalized Kamlet–Taft parameters show that the NADES cover a broad solvent spectrum—from highly H-bond accepting to strongly H-bond donating or dipolar systems—highlighting the potential for fine-tuning the solvent according to target applications. The obtained results highlight the applicability of these NADESs as green, tunable media for the extraction and solvation of bioactive compounds. Full article

Extracts from the stem bark of Stryphnodendron adstringens (barbatimão) exhibit relevant medicinal properties, such as anti-inflammatory, antioxidant, antimicrobial, and wound-healing activities, which reinforce their potential for developing herbal medicines. The $550 billion plant bioactive market (by 2030) demands safer, green-chemistry-aligned extraction methods for responsible industrial scaling. In this study, dry extracts obtained from the stem bark of S. adstringens were obtained by ultrasound-assisted maceration in one- and two-step extraction systems. Parameters such as yield, solvent evaporation time, cost, acute toxicity, epigallocatechin gallate (EGCG) concentration, cell viability, antioxidant potential, and anti-inflammatory activity were evaluated. High-EGCG two-step organic extracts were industrially difficult, needing more raw material and toxic solvents. In contrast, the single-step extracts showed a better balance between yield, cost, safety, and biological efficacy. All extracts showed cell viability above 70% at safe concentrations and significantly reduced the production of inflammatory cytokines. Thus, the results confirm that optimizing single-step extraction, with lower environmental impact solvents, enables producing safe and effective polyphenol-rich extracts, consolidating water as the main candidate for industrial-scale phytotherapeutic formulations of barbatimão, in line with its traditional use in infusions. Full article

Metal-organic frameworks (MOFs) offer high porosity for water remediation but face challenges in handling as powders. We address these limitations by physically immobilizing Fe–BTC MOF within calcium-crosslinked low-methoxyl pectin matrices (PE–Ca–MOF). Solvent-cast films and freeze-dried foams were fabricated using water-based and polyvinylpyrrolidone (PVP)-assisted Fe–BTC dispersions, preserving MOF and pectin structures confirmed by FT–IR. PVP improved Fe–BTC dispersion and reduced particle size, enhancing distribution and plasticizing the matrix proved by DSC. Incorporation of water-dispersed Fe–BTC increased the equilibrium adsorption capacity but reduced the initial adsorption rate, while the PVP-assisted foam further enhanced uptake in comparative batch tests through its more open porous structure. At pH 7, PE–Ca–5%MOF films showed high adsorption capacities and removal efficiencies for paraquat (35.5 mg/g, 70.6%) and tetracycline (14.5 mg/g, 46.8%), while maintaining Zn²⁺ uptake compared to calcium-pectin films without MOF. Adsorption followed pseudo-first-order kinetics and Langmuir isotherms. Green regeneration with acetic acid enabled >80% capacity retention over five adsorption–desorption cycles. Foam architectures increased porosity and active-site accessibility (SEM), improving performance even at lower MOF loadings. Overall, controlling MOF dispersion and composite morphology enables efficient, reusable, and environmentally friendly bio-based adsorbents for water purification. Full article

The growing concern over plastic pollution and the widespread presence of micro- and nanoplastics has renewed interest in polyhydroxybutyrate (PHB) as a biodegradable alternative; however, its industrial deployment remains constrained by costly recovery operations with a high environmental burden. This study examines how PHB biosynthesis and intracellular organization, physicochemical properties, and the characteristics of the producing microorganism influence the performance of conventional recovery routes, including extraction with organic solvents, alkaline/oxidative chemical digestion, and enzymatic–physical schemes coupled with mechanical disruption. Based on this foundation, quantitative data are analyzed for PHB content in bacteria, mixed microbial cultures, cyanobacteria, and microalgae, along with extraction yields, polymer purity, and solvent recyclability in processes employing chlorine-free solvents, green solvents, and hydrophobic natural deep eutectic solvents (NaDESs) formulated with terpenes and organic acids. The analysis integrates mechanistic perspectives on NaDES–cell and NaDES–PHB interactions with solvent design criteria, biorefinery configurations, and preliminary evidence from technoeconomic and life cycle assessments. The findings identify NaDES as an up-and-coming platform capable of reconciling biopolymer quality with the principles of green chemistry while delineating critical gaps in recovery efficiency, viscosity management, solvent recycling, and pilot-scale validation. Full article

Two amide-preformed aromatic diamine monomers, N,N-bis(4-(3-aminobenzamido)phenyl)-N’,N’-bis(4-methoxyphenyl)-1,4-phenylenediamine (m-6) and N,N-bis(4-(4-aminobenzamido)phenyl)-N’,N’-bis(4-methoxyphenyl)-1,4-phenylenediamine (p-6), were synthesized and utilized to prepare two series of electroactive poly(amide-imide)s (PAIs) through a two-step polycondensation reaction with commercially available aromatic tetracarboxylic dianhydrides. The obtained polymers exhibited solubility in various polar organic solvents, and most of them could form transparent, flexible films via solution casting. Thermal analysis indicated glass transition temperatures (T_g) ranging from 250 °C to 277 °C, as measured by DSC, with no significant weight loss observed before 400 °C in TGA tests. Cyclic voltammograms (CV) of the polymer films on ITO-coated glass substrates revealed two reversible oxidation redox pairs between 0.67 and 1.04 V vs. Ag/AgCl in an electrolyte-containing acetonitrile solution. The PAI films showed stable redox activity with high optical contrast both in the visible and near-infrared regions, transitioning from colorless in the neutral state to green and blue in the oxidized states. Furthermore, the polymer films retained good electrochemical and electrochromic stability even after more than 100 cyclic switching operations. The PAIs displayed outstanding electrochromic performance, including high optical contrast (up to 95%), rapid response times (below 4.6 s for coloring and 5.7 s for bleaching), high coloration efficiency (up to 240 cm²/C), and low decay in optical contrast (less than 5% after 100 switching cycles for most PAIs). Full article

A magnetic deep eutectic solvent-based single-drop microextraction technique coupled with high-performance liquid chromatography (MDES-SDME-HPLC) was established for the determination of five triazine herbicides in environmental water samples. MDES, used as the extraction solvent, was composed of heptanoic acid, methyltrioctylammonium chloride, and iron chloride. This pretreatment method requires only 50 μL of MDES, thereby avoiding the use of large volumes of toxic organic solvents. The MDES containing the target triazine herbicides was rapidly separated from the aqueous matrix by applying an external magnetic force, thus eliminating the need for centrifugation or additional reagents to achieve phase separation. The method demonstrated a linear range of 0.2–20 μg L⁻¹, with a limit of detection of 0.06 μg L⁻¹. Recoveries obtained from different environmental water matrices ranged from 75.5% to 102.4%. The greenness of the method was confirmed using five independent green analytical assessment tools. This approach represents a green and efficient analytical technique for detecting triazine herbicides in environmental water samples. Full article

Deep eutectic solvents (DESs) have attracted significant attention as eco-friendly and sustainable alternatives to conventional, often toxic, organic solvents. They are easy to synthesize, and their tunable physicochemical properties enable their application in microextraction techniques for a wide range of analytes. However, some DESs may exhibit thermal instability, and their high viscosity or solubility can influence the extraction efficiency. Despite these limitations, in recent years, DESs have been successfully used in multiple roles in solid-phase microextraction (SPME). They may be used to functionalize or modify sorbent materials, thereby forming composite sorbents with enhanced performance. Moreover, DESs can be combined with polymers to produce hybrid materials with improved extraction capabilities. Additionally, DESs can act as porogens within SPME sorbents, increasing sorption capacity and, consequently, extraction efficiency. They can also serve as green desorption solvents, replacing traditional volatile organic solvents during the recovery of analytes from sorbent materials. This review synthesizes current knowledge on the implementation of DESs in SPME techniques, critically evaluating their primary advantages and inherent limitations. The novelty of this review lies in the assessment of DES-based SPME through the metrics of greenness and sustainable chemistry. Furthermore, the review identifies research perspectives and priorities to advance DES-based SPME, including: the integration of predictive modeling (COSMO-RS, machine learning) to elucidate DES-analytes interactions; the adoption of 3D printing for the precision fabrication of DES-based sorbents; the standardization of DES-based SPME performance; and the exploration of natural DESs for in vivo SPME in biomedical applications. Full article

Electrospinning of poly(lactic acid) (PLA) commonly relies on toxic organic solvents, which limit its sustainability and biomedical applicability. In this work, a green electrospinning process was developed using dimethyl carbonate (DMC), a biodegradable and low-toxicity solvent, combined with acetone as a volatile co-solvent to promote efficient jet solidification. Three commercial PLA grades were evaluated for solubility and spinnability, and PLA 4043D was identified as the most suitable for DMC and acetone systems. The electrospinning parameters, including solvent ratio, flow rate, and applied voltage, were systematically optimized to achieve stable jet formation and uniform fiber morphology. Under optimized conditions, the process produced continuous, bead-free nanofibers with a mean diameter of ~1 µm and uniform nanoscale surface porosity resulting from differential solvent evaporation. The resulting fibers were characterized in terms of morphology, structure, thermal behavior, and mechanical performance, confirming increased amorphous content, high porosity (about 78%), and tensile strength of ~3 MPa for the selected electrospinning condition. This study demonstrates that DMC-based solvent systems enable a sustainable and potentially biocompatible route, considering the lower toxicity of the solvents employed, offering a green alternative to conventional toxic processes for the fabrication of medical scaffolds. Full article

Mini-LC systems, including Cap-LC, Nano-LC and Chip-LC, offer a sustainable alternative to conventional LC methods thanks to their reduced solvent consumption, enhanced separation efficiency and environmentally friendly operation. Integrating micro-scale sample preparation techniques, such as µ-SPE, IT-SPME, LPME and QuEChERS, with Mini-LC significantly improving analytical sensitivity and selectivity. Mini-LC coupled with mass spectrometry has demonstrated excellent performance in the detection of trace levels of pesticides, pharmaceuticals, veterinary drug residues, perfluoroalkyl substances (PFASs), and mycotoxins. Despite current challenges relating to matrix effects, instrument stability and method standardization, Mini-LC represents a promising analytical platform for the cost-effective, high-sensitivity, green monitoring of contaminants in food safety and environmental analysis. This review summarizes recent advances in the application of Mini-LC techniques for analyzing emerging organic contaminants (EOCs) in food and environmental samples. This paper also provides a critical review of this topic, covering works published in the last four years (early 2022–mid 2025). Additionally, it discusses the use of these techniques in combination with mass spectrometry (e.g., low-resolution MS or high-resolution MS) for the detection of EOCs in food and environmental samples. Full article

Exploring green organic solvents is a global demand. Most of the currently used solvents pose some concerns regarding environmental sustainability and occupational health risks. In this work, propylene glycol was employed for the first time as a green solvent for mobile phase preparation in the reversed phase chromatographic separation of a mixture of two antioxidants, glutathione and ascorbic acid. The slight viscosity of propylene glycol was manipulated by using water as a co-fluidizing agent to facilitate pumping. Method optimization was performed using factorial design experimental Expert 13^® Software (Minneapolis, MN, USA) to achieve the maximum resolution and the minimum run time. The reported method was properly validated according to the International Conference on Harmonization criteria at the linearity range of 1–500 µg/mL, with acceptable accuracy and precision for both drugs. The method was effectively applied for the quantification of both drugs in their commercial pharmaceutical formulation. The proposed method was assessed for environmental and operator safety by means of global tools like AGREE and MoGAPI and has proved high degrees of greenness. Propylene glycol has several benign properties, such as low volatility, less toxicity, compatibility with UV detectors and very low flammability, that will soon assemble it as a promising alternative for the conventionally used solvents. Full article