ULTRASONICS SONOCHEMISTRY
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2026
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IF 10.2
Huixin You,Haonan Shen,Hejie Han,Yongjing Liu,Hua Li
In this study, eighteen LCST-type temperature-responsive deep eutectic solvents (TRDESs) were developed for the ultrasound-assisted extraction of alkaloids from white pepper, using piperine (PIP) as the indicator. After optimization, the best conditions were identified as lidocaine/valeric acid (1:1) as the solvent, a solid‑to‑liquid ratio of 1:40 mg/mL, 75°C, and 30 min of ultrasound, achieving a PIP yield of 33.7502 mg/g. By utilizing the temperature‑responsive behavior of TRDES, PIP was separated solely by adjusting temperature and water content, without additional reagents, resulting in a crude extract containing 122.3 μg/mg of PIP. Subsequent analysis confirmed that the TRDES‑based ultrasound‑assisted extraction did not affect the antioxidant or anti‑diabetic (α‑glucosidase and α‑amylase inhibitory) activities of the extract. The TRDES system also showed good reusability, retaining over 85% of its initial extraction efficiency after five cycles. Density functional theory calculations revealed that ultrasound‑assisted extraction proceeds via hydrogen bonding between lidocaine/valeric acid and the five‑membered ring of PIP. With a high GAPI score of 82, this method offers a clearly greener and more sustainable alternative to conventional extraction techniques. This work integrates the novel green solvent TRDES with ultrasound‑assisted extraction, laying a key foundation for developing environmentally friendly processes in natural product preparation.
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JOURNAL OF CHROMATOGRAPHY A
·
2026
·
IF 4
Qiuyue Hu,Ruochen Qi,Xindi Feng,Dian Jin,Li Sun,Zuoxiang Zeng,Feng Liang,Zhongli Xiong,Zhen Liu
Deep eutectic solvents (DESs) have emerged as promising green alternatives to conventional organic solvents for the sustainable extraction of bioactive compounds from medicinal plants. In this study, a DES-based extraction system enhanced by ultrasound was employed to extract flavonoids from Scutellariae Radix (SR). A hybrid optimization strategy integrating Box-Behnken design (BBD), artificial neural network (ANN) modeling, and genetic algorithm (GA) was utilized to maximize the extraction efficiency. Under the optimized conditions, the predicted yield of flavonoids reached 194.58 mg/g, which was in close agreement the experimental value (194.03 mg/g). The purified DES extracts exhibited strong antioxidant activity. After five consecutive extraction cycles, the DES maintained its structure stability and retained a high extraction yield with only a 11.39% decrease. The characterization of the solid extraction residue indicated the microstructure of SR was disrupted by the DES, facilitating the release of flavonoids. In addition, mechanistic studies based on quantum chemical calculations revealed strong hydrogen bonding and orbital interactions between the DES and flavonoids as key contributors to the extraction process. These results demonstrate the potential of DESs as tunable and reusable media for the efficient extraction of natural products, supported by both experimental data and molecular-level insights.
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Food Chemistry-X
·
2025
·
IF 8.2
Yuxin Wang,Jin Liu,Suzhen Li,Jizhen Fu,Xiaowen Wang,Li Li,Xu Jing
The widespread use of triazole fungicides has raised concerns over residual. This study presents an automated, environmentally friendly, simple, and efficient method for detecting triazole fungicides in food samples, utilizing high-throughput liquid processing, dispersive liquid-liquid microextraction, and ultra-high-performance liquid chromatography-tandem mass spectrometry. The automated liquid handling workstation was employed to automate the whole sample pre-treatment process. Fatty acid, bio-based solvent, and saturated sodium chloride solution were used as the extractant, dispersant, and demulsifier, respectively. The whole operation process obviated the use of toxic reagents and eliminated the need for time-consuming centrifugation. The linear ranged from 0.01 to 1 μg L −1 with limits of detection and quantification of 0.003 μg L −1 and 0.01 μg L −1 , respectively. Ten triazole fungicides were successfully detected in food samples with recoveries of 70.1 %–105.7 %. The automation of dispersive liquid-liquid microextraction demonstrates huge potential for broad applicability within the field of food safety testing.
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Journal of Environmental Chemical Engineering
·
2025
·
IF 7.2
Dongting Huang,Huixin You,Lirong Chen,Yongjing Liu,Hua Li
This study extends the development of a Graphene oxide@Zirconium-based metal-organic framework@Deep eutectic solvents (GO@MOF-808@DESs) through hydrothermal self-assembly using zirconium chloride and 1,3,5-benzenetricarboxylic acid (H 3 BTC), subsequently functionalized with four carbon-tailored fatty acid-based deep eutectic solvents (DESs) via ultrasonic impregnation. Comprehensive characterization of GO@MOF-808@DES confirmed the successful surface modification via DES. A dispersive micro-solid phase extraction(D-μSPE) method was established employing GO@MOF-808@DESs as an adsorbent for efficient removal of residual entacapone (ETCP) and tolcapone (TCP) from water. Optimization of the D-μSPE method revealed optimal conditions at pH 9.0, with a sample volume of 40 mL, an adsorbent dosage of 20 mg, and an adsorption time of 60 min. Under these conditions, the method achieved a significant adsorption capacity of 86.50 ± 4.79 mg/g for ETCP and 126.21 ± 2.72 mg/g for TCP. Mechanistic investigation revealed chemically dominated adsorption kinetics through pseudo-second-order modeling and Langmuir isotherm fitting. Concurrently, density functional theory (DFT) studies demonstrated that the synergistic effect between carboxyl-mediated hydrogen bonding and hydrophobic interactions led to enhanced adsorption performance. The engineered GO@MOF-808@DESs based D-μSPE method demonstrated superior performance in removing ETCP and TCP from river water matrices, achieving 99.67 % and 99.24 %, respectively. Meanwhile, a sensitive and reliable method for trace-level monitoring of ETCP and TCP residues in environmental waters was successfully proposed, employing GO@MOF-808@DESs-based D-μSPE coupled with liquid chromatography-tandem mass spectrometry (LC-MS/MS). This study presents a robust strategy for fabricating high-performance GO@MOF-808@DESs composite materials, demonstrating significant potential for practical applications.
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MICROCHEMICAL JOURNAL
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2025
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IF 5.1
Pengge Wei,Jianxiang Liu,Jing Zhao,Longshan Zhao
Traditional maceration extraction methods for dioscin typically involve substantial consumption of organic solvents and long extraction times. The present study aimed to develop a green and sustainable extraction procedure for the extraction of Dioscin from Dioscorea nipponica Makino (DNM). A series of switchable natural deep eutectic solvent (SNADES) based on medium chain fatty acids were prepared to achieve high extraction efficiency of Dioscin from DNM. As a result, hexanoic acid and heptanoic acid were selected as the optimal solvents. The optimal extraction conditions were as follows: a molar ratio of 1:1, a liquid-solid ratio of 50 mL·g −1 , an ultrasonic duration of 50 min, and a polarity switch phosphoric acid dosage of 800 μL without additional salt. The SNADES-UALLME method established in this study minimizes the use of organic reagents and provides a new insight for development of green extraction methods for active ingredients from traditional Chinese medicine.
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JOURNAL OF FOOD COMPOSITION AND ANALYSIS
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2025
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IF 4.6
Yawen Zhang,Hongli Zhang,Jiangong Ma,Jing Zhao,Huajuan Yin,Xu Jing,Xiaowen Wang
With the advent of new-generation green extraction solvents, deep eutectic solvents (DESs) present significant prospects for the extraction of bioactive substances. In this study, saponins were extracted from oats using an ultrasonic-assisted method with green DESs, replacing conventional toxic organic solvents. Adding sodium chloride markedly reduced solubility, resulting in the separation of two phases from the extract: DES and water. The saponins were separated into the water phase, while the DES was reused in subsequent extractions, supporting extractant recycling and promoting sustainable development. Adding salt offers a more gentle, convenient, and cost-effective alternative to current phase separation methods, such as pH adjustment, temperature variation, and carbon dioxide or nitrogen gas application. Optimizing the extraction and recovery parameters yielded the highest oat saponin extraction efficiency at 18.73 mg g –1 , and the recovery was 86.4 %. When compared with ethanol extracts, DES extracts exhibited superior antioxidant activity. Lastly, the greenness of this extraction method was confirmed through three greenness evaluation programs of greenness. The extraction method based on emerging responsive solvents can be extended to other hydrophilic bioactive substances.
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Foods
·
2026
·Vol. 15
·期 17
·3002
·
IF 6
Min Li,Yulin Wang,Huajuan Yin,Xu Jing,Yunlong Li
Triazole fungicides (TFs) are widely used in cereal production due to their potent fungicidal activity and broad-spectrum efficacy. Nonetheless, residues of TFs in food products may pose risks to food safety and human health. Therefore, the development of efficient and environmentally friendly sample preparation methods is paramount for the reliable determination of TFs. Herein, a novel green solvent-based dispersive liquid–liquid microextraction method coupled with high-performance liquid chromatography (DLLME-HPLC) was developed for the determination of TFs in cereal samples. The prepared magnetic deep eutectic solvents (MDESs), composed of nonanoic acid and ferric hydroxide, served as green, magnetically responsive extraction solvents, enabling rapid magnetic separation without centrifugation. Four bio-based solvents (BBSs) were investigated as green dispersive solvents to facilitate the dispersion of MDESs and replace conventional toxic organic dispersants, thereby further enhancing the environmental sustainability of the extraction procedure. Owing to the combined effects of hydrophobic interactions, hydrogen-bonding networks, and magnetic responsiveness, the proposed method achieved efficient extraction and rapid phase separation while minimizing solvent consumption and operational complexity. The greenness of the method was evaluated using multiple green analytical chemistry metrics, confirming its low environmental impact, reduced waste generation, and improved operational safety compared with conventional DLLME procedures. Under optimized conditions, the method was successfully applied to determine TFs in rice, wheat, corn, buckwheat, and oat samples, achieving recoveries ranging from 75.0% to 101.9% and relative standard deviations of 1.6–4.8%. The developed DLLME method provides a rapid, sensitive, and environmentally friendly strategy for cereal pesticide residue analysis and expands the application of MDESs and BBSs in green sample preparation.
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INTERNATIONAL JOURNAL OF ENVIRONMENTAL ANALYTICAL CHEMISTRY
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2023
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IF 2.6
Xingle Guo,Xin Huang,Haijuan Jiang,Guisen Zhang,Liyan Jia,Xu Jing,Junxue Wu
A pre-treatment and analytical procedure for parathion-methyl (PM) in food samples was developed using cyclodextrin-based dispersive liquid-liquid microextraction (CD-DLLME) accompanied by a smartphone digital image colorimetry (SDIC). The extractant used was a green deep eutectic solvent synthesised from hexanoic acid and menthol. Cyclodextrin aqueous solutions were used as the green dispersion solvents to complete the dispersion and extraction process. Thus, a simple, fast, and environmentally friendly pre-treatment method was proposed. PM that was hydrolysed to a yellow product under an alkaline environment, and the colour intensity could be obtained using a smartphone for analysis. PM showed linearity ranging from 0.0020 to 1.0000 mg L−1, with limits of quantification and detection of 0.0020 and 0.0006 mg L−1. This method has been successfully applied in water, juice, tea, and vinegar, with recoveries ranging from 80.4 to 105.7% and relative standard deviation between 1.3 and 3.6%. This method can determine the concentration of PM in different food samples.
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FOOD CHEMISTRY
·
2023
·
IF 8.8
Jing Zhang,Jiaxi Deng,Jia Zheng,Yi Ma,Huibo Luo,Xiaogang Luo,Changjun Hou,Danqun Huo
An acid-sensitive carbon dot fluorescence sensing array was investigated for the differentiated recognition of distilled spirits. Due to the electrostatic interactions between CDs and organic acids, organic acids affect the protonation and fluorescence properties of CDs, which in turn modify the CDs triple fluorescence emission. The regular linear variation of the fluorescence sensor was found under acidic conditions (3.0 < pH < 6.2). A comprehensive study of acids with selectivity, different concentrations (0.1 mM, 1 mM, 10 mM, 40 mM), different types (8 species) and mixed acids (formic acid and acetic acid), and good quantification capability for acetic acid (0.01–1 mM). Demonstrating good recognition ability of the sensor array for complex analyte. On this basis, the fluorescence sensor array was applied to the classification and recognition of liquors. LDA has realized the identification of 16 kinds of Baijiu and 21 kinds of distilled liquors with an accuracy of 100%.
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Food Chemistry-X
·
2023
·
IF 6.1
Min Wang,Luyao Zhao,Yu Niu,Shu Qin,Lixin Zhang,Liyan Jia,Xu Jing
In this study, a magnetic deep eutectic solvent coupled with dispersive liquid–liquid microextraction using high-performance liquid chromatography (MDES-DLLME-HPLC) was developed to detect strobilurin fungicides. The green hydrophobic MDES synthesized by methyltrioctylammonium chloride, ferric chloride, and heptanoic acid was used as an extraction solvent, which was dispersed by vortex and separated by an external magnetic field. The use of toxic solvents was avoided, and the separation time was reduced. The best experimental results were obtained through single factor and response surface optimization. The method had a good linear relationship with R 2 > 0.996. The limit of detection (LOD) ranged from 0.001 to 0.002 mg L −1 . The extraction recoveries were 81.9–108.9%. The proposed method was rapid and green, and it has been successfully applied to detection of strobilurin fungicides in water, juice, and vinegar.
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JOURNAL OF CHROMATOGRAPHY A
·
2022
·
IF 4.601
Yao Wang,Li Yang,Rong-rong Xing,Run-qin Wang,Xuan Chen,Shuang Hu
A homogeneous liquid-liquid microextraction (HLLME) was established based on a switchable deep eutectic solvent (DES) for the preconcentration and determination of six flavonoids with different polarity in “Scutellariae Radix” combined with high performance liquid chromatography (HPLC). A switchable DES composed of N,N-dimethylethanolamine (DMEA) and heptanoic acid was used as an extraction solvent in the HLLME method, which was miscible thoroughly with the aqueous sample phase initially, and then underwent rapid phase transition induced by the addition of an inorganic acid. After the extraction, the upper hydrophobic layer was recovered for HPLC analysis. Different experimental parameters were optimized, and the optimal extraction conditions were as follows: the switchable DES extraction phase, 90 µL of DMEA-heptanoic acid (1:1 mole ratio); phase-switching trigger, 100 µL of 5 mol/L HCl; 10% (w/v) of salt concentration in sample phase; extraction time, 0.3 min. Furthermore, the structures of the switchable DES and the upper hydrophobic layer were characterized by Fourier transform infrared spectroscopy, proton nuclear magnetic resonance spectroscopy and differential scanning calorimetry to illustrate the phase-switching mechanism of the extraction phase during the extraction process. Under the optimized conditions, the enrichment factors for six target analytes were between 0.4 and 104. The calibration curves were linear (r≥0.9866) in the range of 0.033–8.65 mg/L for scutellarin, 0.022–5.77 mg/L for baicalin, 0.0033–0.865 mg/L for scutellarein and wogonoside, and 0.0022–0.577 mg/L for baicalein and wogonin, respectively. Low detection limits (≤8.0 × 10 −3 mg/L) and quantification limits (≤2.4 × 10 −2 mg/L) as well as good precisions (relative standard deviations lower than 9.2%) and acceptable accuracies (spiked recoveries 89.3–114.4%) were also obtained. The proposed method is a simple, fast, and eco-friendly sample pretreatment method.
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Foods
·
2022
·Vol. 11
·期 24
·3997
·
IF 5.561
Youyou Yang,Jing Li,Jiangtao Xing,Weihai Xing,Chaohua Tang,Zhenghua Rao,Junmin Zhang
Volatile compounds play vital roles in food sensory attributes and food quality. An analysis of volatile compounds could illustrate the sensory attributes at the microscale level. Here, untargeted profiling approaches for volatiles in five most-consumed meat species were established using headspace SPME-GC/high resolution Orbitrap MS. An extended high-resolution database of meat volatile compounds was established to enhance the qualification accuracy. Using sulfur-containing compounds, aldehydes, and ketones as the research model, the parameters including fiber coating types, extraction temperature, extraction time, and desorbing time were optimized. Principle component analysis, volcano analysis and partial least squares discriminant analysis were applied to run the classification and the selection of discriminant markers between meat varieties, respectively. Different varieties could be largely distinguished according to the volatiles’ profiles. 1-Octen-3-ol, 1-octen-3-one, 2-pentyl furan and some other furans degraded from n-6 fatty acids would contribute to distinguishing duck meat from other categories, while methyl esters mainly from oleic acid as well as dimethyl sulfoxide and carbon disulfide possibly produced from the sulfur-containing amino acids contributed to the discrimination of beef. Therefore, volatiles’ profiling not only could interpret the aroma style in meat but also could be another promising method for meat differentiation and authentication.Keywords:differentiation;GC-HRMS;SPME;statistical analysis;untargeted profiling;volatiles
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