Search Results (2,341)

Sample preparation is frequently a time-consuming process and can be a major bottleneck in many analytical techniques that involve some form of modification to a sample so that it can be analyzed without interference or to increase its sensitivity. As part of the movement towards “green analytical chemistry”, the reduction in organic solvent usage and toxicity via alternative solvents compared to those traditionally used in analytical chemistry has gained increasing interest. Although ionic liquids were thought to have limitations, deep eutectic solvents (DESs) are being looked at as alternatives to traditional organic solvents in analytical chemistry because of their ability to produce a “tunable” set of physico-chemical properties that enable the selective and efficient extraction of a wide variety of analytes from a very diverse array of matrices. Although deep eutectic solvents have attracted increasing attention in analytical extraction applications, a systematic comparison of their performance across various extraction techniques is still lacking. This review fills this gap by offering a comprehensive and integrated evaluation of DES-based extraction approaches, emphasizing the interdependence between solvent characteristics, extraction efficiency, selectivity, and sustainability. The insights presented herein are intended to support the rational selection of appropriate DES-based extraction strategies for diverse analytical purposes. Moreover, these findings are expected to contribute to the advancement of greener, more efficient sample preparation methodologies within the field of green analytical chemistry. In this review article, we describe several analytical chemistry techniques that utilize DESs, such as dispersive liquid–liquid microextraction, solid-phase extraction, ultrasound-assisted extraction, etc., and explain the basic principles and mechanisms behind each technique. Additionally, comparative evaluations are provided to identify the relative advantages and disadvantages of the techniques mentioned above in terms of extraction efficiency and selectivity, and speculation regarding future trends and challenges in DES-based extraction systems will also be included. By integrating recent advances and comparative performance assessments, this review serves as a reference for researchers and industry practitioners, fostering innovation and promoting the wider adoption of sustainable extraction technologies. Full article

An analytical method was established for the rapid determination of 45 pigments and preservatives in edible ink by ultra-high performance liquid chromatography coupled with triple quadrupole tandem mass spectrometry (UHPLC-MS/MS), which provides technical support for the composition analysis and industrial development of edible ink. The samples were easily extracted with 75% aqueous methanol solution and purified with a Captiva EMR-Lipid HF solid-phase extraction cartridge. After filtration through a polytetrafluoroethylene (PTFE) membrane, the analytes were determined by UHPLC-MS/MS under multiple reaction monitoring (MRM) mode in both positive and negative ion modes. Poroshell 120 AQ-C18 was selected as the analytical column, and valve switching timing control was adopted during the gradient elution process. The external standard method was used for quantitative analysis. In the established method, the 45 pigments and preservatives exhibited good linear relationships within the mass concentration range of 0.0002–200.0 μg/mL. The limits of detection (LOD) and limits of quantification (LOQ) were 0.0004–8.00 mg/kg and 0.001–20.00 mg/kg, respectively. Using 25% aqueous glycerol solution as the blank matrix, the recoveries of analytes at different spiked levels met the detection requirements. The established method is simple and rapid, and can be applied to the qualitative and quantitative detection of typical pigments and preservatives in edible ink. Full article

Soybean residue, a major by-product of soy milk and tofu processing, is a large-yield and nutrient-rich substrate, but it is currently experiencing low utilization rates. In this study, a prodigiosin-producing strain, Serratia marcescens BD2025, was isolated from naturally fermented soybean residue. Subsequently, prodigiosin was produced by solid-state fermentation of soybean residue, and the fermentation conditions were further optimized by a Box–Behnken (BBD) model involving the soybean residue-to-water ratio, inoculum size, and temperature. Under the optimized conditions of a soybean residue-to-water ratio of 1:4.28, an inoculum size of 5.2%, and cultivation at 27.5 °C for 48 h, the prodigiosin yield reached 19.05 mg/g. High-performance liquid chromatography analysis showed that the major pigment peak had a retention time comparable to that of a prodigiosin standard, with an estimated purity of 96% based on peak area normalization. The results show that prodigiosin remains relatively stable at below 40 °C, in acidic conditions, and in darkness. The extracted prodigiosin inhibited both Escherichia coli and Staphylococcus aureus, with stronger activity against S. aureus. The scavenging ability of DPPH radical was dose-dependent, with the scavenging activity of 93.13% at 5 mg/mL. These findings indicate that soybean residue can serve as a solid-state fermentation substrate for prodigiosin production and provide a basis for the value-added utilization of soybean-processing residues. Full article

The sustainable valorization of spontaneous flora biomass for the recovery of high value-added phytochemicals represents a key opportunity within the circular bioeconomy, yet it remains constrained by the environmental limitations of conventional extraction solvents and the lack of data-driven optimization frameworks. In this study, Natural Deep Eutectic Solvents (NADES) composed of betaine and 1,3-propanediol were designed and applied as bio-based extraction media for the recovery of bioactive metabolites from Artemisia annua L. spontaneous biomass in the context of green extraction and sustainable resource utilization. Two liquid–solid extraction techniques, namely vortex-assisted extraction and ultrasound-assisted extraction, were evaluated. The influence of key process parameters, including the eutectic component molar ratio, water content, solid-to-liquid (S/L) ratio, extraction temperature, and extraction time, was systematically investigated. Results demonstrated that extraction efficiency was strongly dependent on both solvent composition and process conditions, with distinct optimum parameters for different phytochemical classes. Maximum total polyphenol content (52.08 mg GAE/mL) was achieved via ultrasound-assisted extraction at 20 °C for 15 min, using a 1:3 NADES ratio with 40% water dilution and S/L = 1:5, while the highest flavonoid yield (17.34 mg QE/mL) was obtained by vortex-assisted extraction for 45 min using a 1:6 NADES ratio under the same dilution and S/L conditions. To identify extraction conditions associated with improved process efficiency, a hybrid modeling approach combining deep neural networks with the Success-History-based Adaptive Differential Evolution (SHADE) algorithm was employed, enabling high-accuracy prediction of extraction performance across a broad parameter space. The proposed framework demonstrates the feasibility of integrating green solvent design with machine learning-driven process modeling for the efficient valorization of underutilized plant biomass, contributing to the development of resource-efficient, sustainable extraction protocols, consistent with principles of process intensification and resource-efficient extraction strategies. Full article

This study explores an innovative approach based on deep eutectic solvent (DES)-synergistic ultrasonic-assisted extraction (UAE) of anthocyanins from blueberry pomace (BP). Choline chloride–lactic acid (ChCl-LA, 1:2) was identified as the most efficient DES and provided the highest anthocyanin recovery. The optimal conditions for ChCl-LA-synergistic UAE (ChCl-LA-UAE) were obtained as follows: ultrasonic power of 270 W, extraction time of 30 min, liquid-to-solid ratio of 35:1, and water content in ChCl-LA of 40%, achieving a total anthocyanin content (TAC) of 3.5168 mg/g, with R² = 0.9860. This value was significantly higher than those obtained with 70% ethanol (3.1962 mg/g) and pure water (1.9137 mg/g). SEM images revealed that ChCl-LA-UAE disrupted the surface structure of the samples, thereby promoting anthocyanin release. COSMO-RS simulations confirmed that ChCl-LA significantly enhanced the interaction between the solvent and the representative anthocyanin (cyanidin-3-O-glucoside, C3G), resulting in higher extraction efficiency. In vitro antioxidant assays further demonstrated that the synergistic system exhibited stronger antioxidant activity. Overall, ultrasonic-synergistic DES extraction could be an eco-friendly method for recovering high-value compounds from blueberry and its byproducts. Full article

Radix Paeoniae Alba, the dried root of Paeonia lactiflora Pall., contains characteristic monoterpene glycosides, but efficient recovery of these polar constituents remains challenging. This study developed an ionic liquid-assisted sequential ultrasound–microwave extraction method and evaluated paeoniflorin, oxypaeoniflorin and albiflorin by HPLC as multi-marker responses. Among the ionic liquids tested, 1-propyl-3-methylimidazolium dihydrogen phosphate showed the best extraction response. Box–Behnken response surface optimization gave practical extraction conditions of a solid-to-liquid ratio of 1:26 g/mL, ionic liquid concentration of 0.12 mol/L and ultrasound time of 22 min. Under these conditions, paeoniflorin and total marker glycosides reached 29.12 and 34.98 mg/g dry material, respectively, representing increases of 32.4% and 34.5% compared with conventional reflux extraction. UPLC-QTOF-MS profiling provided complementary chemical profile information for the optimized extract and tentatively annotated Paeonia-related monoterpene glycoside derivatives, galloylated glucose derivatives and polyphenolic constituents. Electrostatic potential, SAPT and non-covalent interaction analyses, supported by ¹H NMR chemical shift perturbation, suggested possible hydrogen bonding, electrostatic and dispersion interactions between paeoniflorin and the selected ionic liquid. These results support the optimized process as an efficient extraction approach and provide molecular interaction insights into ionic liquid-assisted recovery of monoterpene glycosides. Full article

Maternal exposure to polycyclic aromatic hydrocarbons (PAHs) during pregnancy has been associated with adverse obstetric and perinatal outcomes, including miscarriage, low birth weight, intrauterine growth restriction, and spontaneous abortion. Exposure occurs through multiple pathways, including dietary intake and inhalation, which ultimately determine the final body burden. PAHs may reach relevant levels in the blood, representing the initial step in their internal distribution to the placenta, umbilical cord, and breast milk, thereby compromising maternal–fetal health. In this exploratory study, maternal blood samples were collected from pregnant women residing in different regions of Antioquia, Colombia. Serum was isolated from whole blood, subsequently extracted using freezing-assisted liquid–liquid extraction, purified by solid-phase extraction, and analyzed by GC–MS. Method performance showed PAH recoveries between 60 and 120%, limits of detection (LOD) ranging from 0.5 to 3.3 ng·mL⁻¹, and limits of quantification (LOQ) ranging from 1.4 to 9.9 ng·mL⁻¹. Airborne PAH concentrations were measured using a photoelectric aerosol sensor, and higher levels were observed in municipalities intersected by major highways, indicating a strong vehicular contribution, with an average concentration of 72.6 ± 39.2 ng·m⁻³. Low and medium-molecular weight PAHs were detected in serum samples at an average concentration of 43.8 ± 8.8 ng·g⁻¹ of lipid (mean of ∑ individual congeners). In contrast, a high-molecular-weight PAH, benzo[a]pyrene (BaP), was detected in one participant. Pyrene (PYR) and fluoranthene (FLU) were the predominant congeners, suggesting combustion-related sources, primarily vehicular emissions. Serum PAH levels showed a correlation with the frequency of consumption of canned fish and meat, but not with short-term airborne PAH measurements. These exploratory findings suggest that dietary intake is a primary pathway of bioaccumulation during acute exposure and plays a key role in determining the parental PAHs burden during pregnancy in polluted environments. However, additional data on parent PAHs and their metabolites are needed to provide a more comprehensive assessment of cumulative exposure arising from dietary sources and chronic inhalation of airborne PAHs. Full article

Purple carrot peels are an abundant agro-industrial by-product rich in phytochemicals and have potential applications such as natural colorants and antioxidants. In the context of increasing interest in the valorization of vegetable processing residues, the recovery of bioactive compounds from such materials has become an important scientific and industrial objective. This study aimed to optimize the parameters of a solvent extraction process to maximize total anthocyanin content (TAC), total polyphenol content (TPC), and antioxidant activity (AA) from purple carrot peels. A Central Composite Design, combined with response surface methodology, was used to evaluate the effects of temperature, extraction time, ethanol concentration, and pH across 30 experimental runs. The optimal extraction conditions were identified as pH 4, an ethanol concentration of 50%, a temperature of 80 °C, and an extraction time of 35.88 min. Under the optimized extraction conditions, the experimental values obtained for TAC, TPC, and AA were 2.10 mg C3G/g D.W., 20.60 mg GAE/g D.W, and 19.02 mMol Trolox/g D.W, respectively, which were in close agreement with the predicted values of 2.10 mg C3G/g D.W., 20.30 mg GAE/g D.W, and 19.05 mMol Trolox/g D.W. The good agreement between predicted and experimental values confirmed the adequacy and predictive capability of the developed response surface models. A total of 32 phenolic compounds were characterized by UHPLC–MS/MS, with shikimic acid identified as the dominant compound, highlighting the chemical diversity and abundance of bioactive phenolics in purple carrot peels. The results demonstrate that optimization of extraction parameters significantly enhances the efficiency of conventional solid–liquid extraction, enabling the effective recovery of antioxidant compounds. The proposed approach supports the sustainable valorization of purple carrot by-products as cost-effective sources of natural pigments for food industry applications. Full article

Phosphogypsum (PG) was used as a calcium source for preparing calcium carbonate (CaCO₃) through NH₄Cl leaching followed by high-pressure carbonation. The effects of NH₄Cl concentration, liquid-to-solid mass ratio, temperature, and leaching time on Ca²⁺ extraction were investigated, and the effects of CO₂ pressure, carbonation time, and NH₃·H₂O dosage on Ca²⁺ conversion were evaluated. The optimal conditions were an NH₄Cl concentration of 1.5 mol/L, a liquid-to-solid mass ratio of 60:1, a leaching temperature of 25 °C, a leaching time of 60 min, a CO₂ pressure of 1 MPa, a carbonation time of 10 min, and 12 vol% NH₃·H₂O addition. Under these conditions, the Ca²⁺ leaching rate and conversion rate reached 81.25% and 97.36%, respectively. The product obtained without organic additives was mainly spherical vaterite with partial particle agglomeration. Based on the optimized process, aspartic acid, glutamic acid, ethanol, and glycerol were introduced to regulate CaCO₃ crystallization. Appropriate additive dosages further improved Ca²⁺ conversion, promoted calcite as the dominant polymorph, and produced well-dispersed spherical CaCO₃ particles. Among the tested additives, glutamic acid and glycerol showed the strongest effects on crystal morphology regulation. Full article

To exploit medicinal and edible plant resources, this study investigated the extraction, structural characterization, and in vitro digestion of Elaeagnus angustifolia polysaccharide (EAP). Despite the nutritional value of this polysaccharide, its digestive properties remain unclear. Ultrasound-assisted extraction was optimized via response surface methodology. Crude EAP was purified by AB-8 macroporous resin purification and decolorization, followed by deproteinization and dialysis. The purified product (91.07% total sugar; 2.37% protein) was characterized by ultraviolet (UV) spectroscopy, Fourier-transform infrared (FT-IR) spectroscopy, high-performance liquid chromatography (HPLC), and gel permeation chromatography (GPC), and its digestion profile was assessed using a three-stage in vitro model (INFOGEST 2.0). Under optimal conditions, the crude polysaccharide yield (based on ethanol-precipitated solid; 87.83% total sugar) reached 2.44 ± 0.01%. EAP was identified as a pyranose-type polysaccharide, with glucose, mannose, and galactose as the predominant monosaccharides (relative molar proportions, 0.470:0.199:0.081, normalized to the total detected monosaccharides), with a weight-average molecular weight of 1.739 × 10⁵ g·mol⁻¹. In vitro digestion revealed negligible digestibility in the oral phase (0%), and low digestibility in the gastric (0.55%) and intestinal (2.76%) phases, with a cumulative digestibility of 3.30%. This marked resistance to gastrointestinal digestion indicates EAP is a partially digestible polysaccharide with potential prebiotic properties. The demonstrated resistance to gastrointestinal breakdown provides a theoretical basis for the high-value utilization of EAP in functional foods as a potential fermentable substrate for gut microbiota modulation. Full article

In the Czochralski process of silicon single-crystal growth, the V/G value at the solid–liquid interface is a key parameter affecting intrinsic crystal defects. However, online V/G detection remains difficult because the temperature gradient G cannot be directly measured, while multi-condition distribution shifts and limited labeled data reduce the robustness of data-driven models. To address these issues, this paper proposes DWC-ISBiGNN, an adaptive multi-condition invariant feature extraction method based on the Invariant-Specific Bidirectional Graph Neural Network. The proposed method introduces dynamic sample graph construction with stage-aware global nodes to capture non-stationary process correlations, source-domain credibility weighting to suppress negative transfer, and a semi-supervised training framework combining stage-conditional alignment with teacher–student regression consistency to exploit unlabeled target-domain data. Experiments on industrial data from a 12-inch silicon single-crystal production line show that DWC-ISBiGNN achieves an RMSE of 0.0041, an MAE of 0.00285, and an $R^2$ of 0.9549. Compared with the original IS-BiGNN, the RMSE is reduced by 32.6%, and $R^2$ is increased by 5.43 percentage points. The results demonstrate that the proposed method provides an effective soft-sensing approach for V/G prediction under multiple operating conditions. Full article

This study investigated the effect of brief mechanical homogenization using a household blender on the properties of nopal mucilage and its performance in removing potentially toxic elements (PTEs), specifically Pb, Ni, As, Cd, and Zn, from a real cyanidation barren solution. An aqueous extract from Opuntia ficus-indica cladodes was homogenized for 0, 30, or 60 s before spray drying, yielding powders designated as CA, CB, and CC. The powders and water-reconstituted dispersions were characterized and evaluated in coagulation–flocculation assays. Homogenization reduced water activity and average hydrodynamic diameter and significantly modified the ζ potential, although the effects were not proportional to processing time. At 10% w·v⁻¹, the reconstituted mucilages showed frequency-dependent viscoelastic behavior consistent with a transient gel-like organization. All treatments removed more than 98% of Pb, Ni, and As at doses of 200–800 mg·L⁻¹. Cd removal was more variable and significantly affected by mucilage type, whereas Zn showed lower, non-monotonic removal. ESEM–EDS detected PTE-bearing inorganic domains within the recovered flocs, corroborating transfer from the liquid to the solid phase. Overall, mechanical homogenization modified the colloidal, supramolecular, and gel-related properties of spray-dried nopal mucilage, which showed potential as a multifunctional hydrocolloid for treating chemically complex cyanidation process streams. Full article

Oca (Oxalis tuberosa) skin is considered an agroindustrial waste byproduct, which currently holds no economic value. Nevertheless, this waste is a natural source of antioxidant compounds, which can be recovered through the use of sustainable technologies. Thus, this study aims to evaluate and compare the efficacy of 15% ethanol combined with two extraction techniques like solid–liquid extraction (SLE) and pressurized liquid extraction (PLE) for the recovery of antioxidant compounds from five oca skin cultivars. Regardless of the oca cultivar, the use of PLE was more efficient for obtaining extracts rich in polyphenol with high antioxidant capacity compared to the SLE process. Under PLE conditions, Pachatusan and Yawar cultivars presented the highest value of total polyphenols and antioxidant capacity. In comparison, the QuesWe and Pachatusan cultivars presented the lowest values. Polyphenol profile analysis showed that the PLE process effectively disrupted the cell wall matrix, resulting in a greater release of monomers (gallic acid, catechin, and epicatechin) and procyanidin B2 compared to the SLE process, while procyanidin A2 was more efficiently recovered under SLE, particularly in the Pachatusan cultivar. Principal component analysis (PCA) confirmed cultivar-dependent polyphenolic patterns, explaining 81.7% and 84.8% of total variance for SLE and PLE, respectively, with PLE generating more pronounced differentiation among cultivars driven by catechin, epicatechin, and gallic acid. The integration of PLE technology with the Oca skin framework facilitates the standardized production of extracts rich in antioxidants. Future research should concentrate on evaluating the stability of these specific dimers within food matrices, as well as their bioavailability in human clinical models. Full article

An ultrasound-assisted extraction method combined with response surface methodology was applied to optimize the extraction of phenolic compounds and evaluate the antioxidant capacity of Ferula communis inflorescence. Response surface methodology with a central composite design was used to optimize the process. As independent variables, ethanol concentration (40–80% v/v), solvent-to-sample ratio (10–40 mL/g), and extraction time (14–30 min) were assessed. A solid-to-liquid ratio of 19 mL/g, a 60% ethanol concentration, and a 23 min extraction duration were the ideal extraction parameters. The extraction yield, total phenolic content (TPC), total flavonoid content (TFC), and DPPH radical scavenging capacity (IC₅₀) were predicted to be 18.91%, 34.93 mg GAE/g, 18.03 mg QE/g, and 0.58 mg/mL, respectively, under these optimized conditions. The efficacy of the central composite design in optimizing polyphenol extraction from F. communis was validated by experimental results that closely matched the predicted values. Eleven phenolic compounds were identified by HPLC-DAD, with pyrogallol and kaempferol being the most prevalent components. These results suggest that F. communis may represent a promising source of bioactive compounds with potential antioxidant applications. Full article

Background/Objectives: Semaglutide, a long-acting glucagon-like peptide-1 (GLP-1) analog for type 2 diabetes and obesity, requires sensitive and high-throughput bioanalytical methods to support pharmacokinetic studies. However, previously reported liquid chromatography–tandem mass spectrometry (LC–MS/MS) assays have been limited by lengthy run times (~18 min) and suboptimal sensitivity. This study aimed to develop and validate a rapid, sensitive LC–MS/MS method for quantifying semaglutide in plasma. Methods: Plasma samples (50 μL) were prepared by acetone-mediated protein precipitation followed by solid-phase extraction. Chromatographic separation was performed on a Cadenza CD-C18 MF column within 9 min, using positive electrospray ionization in multiple reaction monitoring mode with the transitions m/z 1029.4 → 110.1 for semaglutide and m/z 938.9 → 109.9 for liraglutide (internal standard). Validation followed the U.S. Food and Drug Administration (FDA) bioanalytical guidelines. Results: The assay showed a lower limit of quantification of 1 ng/mL with linearity across 1–500 ng/mL (R² = 0.9999), with sharp peak shape and no carryover. Intra- and inter-day accuracies were 95.69–103.76% and 94.93–100.08%, with precision ≤4.50% and ≤5.88%. Recovery (93.05–107.95%) and matrix effects (96.34–104.12%) were consistent across quality control levels, and the analyte was stable under all tested conditions. The method was successfully applied to a pharmacokinetic study in Sprague–Dawley rats following subcutaneous administration of 50 μg semaglutide. Conclusions: The validated method offers shorter analysis time, improved sensitivity, and reduced sample volume compared with previously reported assays, supporting its application in preclinical pharmacokinetic studies of semaglutide and related GLP-1 analogs. Full article