MICROCHEMICAL JOURNAL
·
2025
·
IF 5.1
Kaige Zhang,Yanrong Chen,Jing Wang,Rong Guo,Guifen Zhu
A novel supramolecular deep eutectic solvent based ferrofluid for vortex-assisted liquid-liquid microextraction (SUPRADES-FF-VA-LLME) method was developed firstly for extraction of Alkylphenols (APs) from water and beverage samples. In this method, the SUPRADES composed of hydroxyethyl-β-cyclodextrin, thymol and caprylic acid was firstly designed, synthesized and then used as carrier liquid for ferrofluid. The influencing parameters were screened by a plackett-burman design and optimized by a central composite design. Under optimal conditions, the linear range of 4-heptylphenol, 4-octylphenol and 4-nonylphenol was 0.3–400, 0.2–400 and 5–400 μg L −1 , respectively, with R 2 ≥ 0.9990. And the limit of detection and the quantification of this method were 0.05–1.5 μg L −1 and 0.2–5 μg L −1 , respectively. Both intra-day and inter-day precision ( n = 5) were ≤2.1 %, and the enrichment factor were 22–24. After microextraction, phase separation was quickly completed with the help of an external magnet, without the need of centrifugation equipment, greatly simplifying the operation steps and shortening the extraction time (∼2 min). Additionally, due to the introduction of hydroxyethyl-β-cyclodextrin, the encapsulation effect between its hydrophobic cavity and APs significantly enhances its molecular recognition ability, the method modification resulting in 19–29 % increase in extraction efficiency. Extraction mechanism was also studied by density functional theory. Combined with high performance liquid chromatography-fluorescence, this method was used for determination of APs in environmental water and beverages with spiked recovery of 98.4–102.4 %. The SUPRADES-FF-VA-LLME provides a new technique for the selective separation of pollutants, which is expected to be widely used in the field of food analysis and environmental monitoring.
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SPECTROCHIMICA ACTA PART A-MOLECULAR AND BIOMOLECULAR SPECTROSCOPY
·
2026
·
IF 4.8
Zhima Yangcuo,Xiaodan Zheng,Yajuan Zhang,Xin Yang,Xinyi Zheng,Hang Zhu,Wenhui Chen,Qihong Cai
Under alkaline conditions with sodium hydroxide (NaOH), both 1-naphthol (1-NAP) and 2-naphthol (2-NAP) transitioned from their molecular forms to ionic forms, resulting in redshifts of their fluorescence spectra. Thus, not only the interference of 2-NAP raman peak was eliminated, but the fluorescence intensity of two naphthols was also enhanced, thereby improving the selectivity and sensitivity of their analysis. Due to their structural similarity, the conventional fluorescence spectra of 1-NAP and 2-NAP overlapped and interfered with each other, precluding their simultaneous measurement without prior separation. In this study, the wavelength difference (Δλ) = 140 nm was selected for synchronous fluorescence spectrometry (SFS) scanning to simplify the spectra. However, the interference of 2-NAP on 1-NAP remained significant. So, the second-order derivative technique combined with SFS was adopted. The method that eliminated the severe interference between 1-NAP and 2-NAP and wastewater background by utilizing spectral parameters. Finally, a new second-order derivative SFS for simultaneous determination of 1-NAP and 2-NAP was first established. The detection limits were 0.0850 ng·mL −1 for 1-NAP and 0.1066 ng·mL −1 for 2-NAP, with linear ranges of 0.5–80 ng·mL −1 and 0.5–50 ng·mL −1 , respectively. Recoveries of two naphthols in wastewater were 87.53%–93.50% (1-NAP) and 89.85%–104.00% (2-NAP). The new SFS established in this research has been successfully applied to the analysis and detection of 1-NAP and 2-NAP residues in wastewater, achieving satisfactory results. It is expected to become a new routine detection method for 1-NAP and 2-NAP.
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JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY
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2026
·
IF 6.2
Yao Wang,Junhua Qiu,Chengwei Wang,Ruiyu Yang,Fuyou Guo,Tian Li,Shili Li,Lei Yang,Wei Ding
Plant-derived terpenoids are essential secondary metabolites exhibiting broad-spectrum antibacterial properties. However, the bioactivities of terpenoids against Ralstonia solanacearum remain unexplored. Herein, the bioactivities of 30 terpenoids against R. solanacearum were assessed, and trans-anethole (TAN) was identified as a potent antibacterial agent with a minimum inhibitory concentration and minimum bactericidal concentration of 50 and 75 mg/L, respectively. TAN was low-toxic to silkworms, earthworms, seeds, and E. coli. Furthermore, TAN (>25 mg/L) significantly impeded the R. solanacearum growth, blocked ATP and exopolysaccharide (EPS) synthesis, caused DNA damage and cell rupture, and affected swimming motility and biofilm formation, and suppressed expressions of related genes. Compared with thiodiazole copper, and ethylicin, 100 mg/L TAN had a significantly greater control efficiency in both greenhouse and field tests. Importantly, TAN enhanced the abundance of the beneficial bacteria Bacillus and Sphingomonas. These findings highlight TAN as a potential bacterial wilt control agent.
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Insects
·
2026
·Vol. 17
·期 1
·69
·
IF 2.9
Huiyin Hu,Huanqian Yao,Shuyin He,Xinyi Xie,Cuiting Liu,Veeran Sethuraman,Jingjing Zhang,Benshui Shu
Simple SummaryThe fall armyworm,Spodoptera frugiperda, is an economically important pest that has caused extensive damage to many crops all around the world over the past decade. Due to the advantages of being bioactive, biodegradable, and ecologically safe, thymol, one of the principal ingredients identified in essential oils, has exhibited its potential in pest control. However, the effects and toxicological mechanisms of thymol onS. frugiperdaare still unclear. In this study, we evaluated the bioactivity of thymol on the larvae ofS. frugiperda. RNA-Seq was performed to explain the preliminary toxicological mechanisms of thymol on larvae by the identification and functional enrichment analyses of differentially expressed genes (DEGs). Overall, our findings indicate that thymol also exhibits the potential for the control ofS. frugiperda.The global migratory pest,Spodoptera frugiperda, has garnered widespread attention due to the serious damage it inflicts on agricultural productivity, particularly in maize. Thymol is a phytochemical that exhibits functional diversification in plant defense, encompassing antibacterial activities and insect pest management. However, the impact of thymol onS. frugiperdais still undetermined. This study examined the growth inhibition and mortality induction inS. frugiperdalarvae after thymol exposure. The detrimental effects of 2.0 and 4.0 mg/g thymol treatments on the growth and development ofS. frugiperdawere also examined. RNA-Seq was used to investigate the probable toxicological mechanism of thymol onS. frugiperda, resulting in the identification of 1754 and 1022 DEGs impacted by 2.0 and 4.0 mg/g thymol treatments, respectively. The DEGs associated with chitin metabolism and cuticle synthesis, hormone biosynthesis, and protein and fat digestion were subjected to additional analysis. Our findings demonstrate the efficacy of thymol in controllingS. frugiperdaand lay the groundwork for understanding the molecular toxicological mechanisms of thymol on larvae.
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JOURNAL OF SEPARATION SCIENCE
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2026
·Vol. 49
·期 8
·e70493
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IF 3.6
Ying Shao,Xiaoyan Jiang,Mengtao Jin,Xuerong Yang,Zuguang Li,Jinsong Liu
Fluorinated liquid crystal monomers (FLCMs) are widely used in various electronic materials owing to their outstanding optoelectronic properties. However, their persistence, bioaccumulation, and toxicity, such as endocrine disruption, in the environment have rendered them emerging contaminants of significant concern. Switchable natural deep eutectic solvents (SNADESs) are prepared from natural compounds and their metabolites. These solvents possess the characteristics of green solvents while overcoming many limitations of conventional organic solvents, and have thus been widely adopted in the analysis and detection of environmental pollutants. In this study, a pH-SNADES was utilized as the extraction medium. Combined with ultrasound-assisted homogeneous liquid-liquid microextraction, a method for the extraction of FLCMs from environmental water samples was established, and the target analytes were qualitatively and quantitatively determined by gas chromatography-mass spectrometry. The results demonstrated that five of these compounds exhibited excellent linearity in the range of 0.5-500 ng mL −1 , while the other two (4-(3,4-difluorophenyl)-4'-pentyl-1,1'-bi(cyclohexyl) and 3,4,5-trifluoro-4'-(4-pentylcyclohexyl)biphenyl) showed linearity in the range of 1-500 ng mL −1 , with limits of detection ranging from 0.001 to 0.167 ng mL −1 and limits of quantification ranging from 0.003 to 0.556 ng mL −1 . Applied to real water samples, the method yielded spiked recoveries of 80.79%-125.42%, relative standard deviations of 0.09%-5.14%, and enrichment factors of 8-26, with its greenness and applicability further validated by three greenness assessment tools. The proposed method is efficient, environmentally friendly, and features mild reaction conditions and simple operation, providing technical support for the detection of FLCMs in environmental water samples.
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FOOD CHEMISTRY
·
2026
·
IF 10.4
Yujiao Cheng,Tianpeng Xiao,Jiying Zhang,Guowei Hu,Tiangang Lei,Guohua Li,Kelin Du,Qin Long,Yongrui He,Jun Wang,Min Zhang,Linhua Huang
Volatiles in orange juices from three new bud mutation varieties of Longleaf orange were investigated by gas chromatography–mass spectrometry (GC–MS) and multidimensional GC–MS/olfactory (MDGC-MS/O) combined with aroma extract dilution analysis (AEDA). The 103 volatiles (34 odorants) were identified, with concentration increasing as Xiaxiangmicheng (XXMC)>Changyexiangcheng (CYXC)>Zhongganmicheng (ZGMC). The XXMC had the highest number of odorants (31), followed by CYXC (28) and ZGMC (25). C10-hydrocarbons and -alcohols ( d -limonene, linalool, and geraniol), as well as C6-alcohol ((E)-3-hexen-1-ol), exhibited high flavor dilution (FD) values (≥64) and contributed to the fatty, citrusy, floral, and grassy odors in juice. Higher odor activity values of esters conferred stronger fruity note in XXMC, while the lower ester-to-aldehyde ratio in ZGMC failed to mask the undesirable odors from volatile sulfur compounds. Four potential flavor markers were screened to distinguish the three bud mutation varieties.These provide a theoretical basis for citrus variety evaluation and flavor improvement.
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DESALINATION
·
2026
·
IF 9.9
Ping Keung Wong,Lok Wan Ng,Wei Han,Matthew Y. Lui
Natural deep eutectic solvents are used as novel media for extractive desalination. • Achieves among the lowest salinity and dissolved organics for similar process. • Solvent components create synergic effects to enhance water yield. Extractive desalination is a low-cost, membrane-free process for desalination that can be applied in the presence of low-grade heat sources, such as industrial waste heat and solar thermal energy. However, the solvents previously proposed for extractive desalination of water for human usage are relatively toxic and unsustainable, causing health and environmental concerns. Thus, the use of greener, but still effective, extractants is critical to the viability of this process. In this study, the use of natural deep eutectic solvents (NADESs) for extractive desalination of simulated brackish water, seawater and brine was investigated. Menthol/decanoic acid NADESs demonstrated the most effective desalination performance, producing freshwater with relatively low salinity (140–700 ppm from seawater) compared to other extractants. Moreover, the quantity of these food-based solvents discharged into the water phase was relatively low (around or less than 120 ppm). Consequently, the produced freshwater generally meets international standards and regulations, which is not commonly reported for extracts produced by this process. The presence of menthol enhanced water yields by over threefold, achieved by breaking the strong dimeric hydrogen bonds in decanoic acid molecules that hinder water absorption, and by extending the hydrogen-bond lifetimes between extractant and water. Moreover, the water yield improved with decreasing salinity of the water source, making brackish water and seawater particularly attractive for this process.
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JOURNAL OF CHROMATOGRAPHY A
·
2026
·
IF 4
Mengting Fu,Huimin Zhang,Mengting Cui,Jinling Bai,Zhiyu Liu,Zhixin Ouyang,Liyun Kong
A green HDES-based TA-DLLME was developed for PAEs analysis in beverages. • Optimized method achieved high preconcentration factors and low detection limits. • COSMO-RS and DFT studies revealed strong hydrogen-bonding interactions. • Sample analysis detected PAEs in beverages meeting national food safety standards. The quantification of phthalic acid esters (PAEs) in food and beverages is crucial for assessing human exposure levels. In this study, an environmentally benign microextraction methodology was developed utilizing a thymol-butyric acid deep eutectic solvent (DES) for the sensitive determination of six PAEs in beverage samples. Through systematic optimization, the temperature-assisted dispersive liquid-liquid microextraction (TA-DLLME) protocol achieved high enrichment factors (82.01–112.39) and extraction recoveries (66.94%-91.75%). Low detection limits (1.14–4.85 μg/L) were achieved, when coupled with HPLC-PDA analysis. The validated method was successfully applied to commercial beverages, with PAEs detected in 78.6% of samples at concentrations ranging from 4.04 to 47.1 μg/L. Mechanistic investigations through COSMO-RS and DFT calculations revealed that strong hydrogen-bonding interactions between the DES components and PAEs (ΔE = -17.29 to -26.28 kcal/mol) are the primary driver of the high extraction efficiency. With the advantages of low solvent consumption (≤200 μL) and rapid processing (<15 min), this approach provides a sustainable and practical alternative for routine monitoring of PAEs in liquid food products. Download: Download high-res image (136KB) Download: Download full-size image
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DENTAL MATERIALS
·
2026
·
IF 6.3
Changyu Shao,Tong Shi,Dayu Wang,Chang Liu,Zhenhang Tang,Yuanyu Zhou,Haihua Pan,Zhijian Xie,Ruikang Tang,Zhuo Chen
Chondroitin sulfate mediates the amorphous calcium phosphate ordered assembly. • Chondroitin sulfate directs the oriented crystallization of the hydroxyapatite. • Biomimetic restores the enamel hierarchical structure and mechanical properties. • Hydrogel mineralization system demonstrates significant efficacy for enamel repair. Objectives This study aims to develop a biomimetic mineralization strategy using chondroitin sulfate (CS) to reconstruct the intricate hierarchical structure of enamel and restore its mechanical properties. Methods Demineralized enamel was remineralized in a CS-containing artificial saliva (AS). The crystallization of hydroxyapatite (HAP) in AS was investigated using transmission electron microscopy (TEM) and atomic force microscopy (AFM)-infrared spectroscopy. Enamel repair efficacy was systematically evaluated via scanning electron microscopy (SEM) and AFM to characterize the microstructure and repair thickness, while nanoindentation was employed to quantify the mechanical properties. In addition, acid resistance was evaluated using a 50 mM HCl solution. Furthermore, an AS-hydrogel mineralization system was developed to evaluate its efficacy in restoring demineralized enamel under biologically relevant conditions. Results The results demonstrate that CS-modified ACP successfully assembles into chain-like precursors via anisotropic forces, which simultaneously regulate the oriented crystallization of HAP. This strategy resulted in a newly formed mineralized layer that effectively reconstructs the hierarchical architecture and recovers mechanical properties, including hardness, elastic modulus, and coefficient of friction, to near-native levels. In addition, the repaired enamel exhibits an acid resistance level comparable to that of native enamel. Significance This study establishes a new, mechanism-driven strategy for enamel remineralisation that is mediated by CS, and a corresponding hydrogel mineralization system, which can be translated into practice, offering a promising approach to future clinical enamel restoration. Download: Download high-res image (411KB) Download: Download full-size image
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
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2026
·
IF 2.5
Pu Zhang,Shuang Feng,Yuru Feng,Jingqiong Lu,Zhiwang Han,Maurizio Quinto,Tao Sun,Xu Jing
Several novel hydrophobic natural deep eutectic solvents were developed. • A vortex-assisted liquid–liquid microextraction method was established. • The simple and efficient method was successfully applied to various urine samples. • The enhanced greenness was confirmed using AGREEprep, AGREE, and GAPI. A novel, facile, and environmentally friendly analytical method was developed based on vortex-assisted liquid-liquid microextraction and high-performance liquid chromatography with diode-array detection for detecting pyrethroid pesticides (PPs) in urine. Natural deep eutectic solvents (NADESs) were prepared using plant essential oil-derived monoterpenoids (thymol, carvacrol, and menthol) combined with aromatic primary alcohols (benzyl alcohol, phenethyl alcohol, and phenylpropyl alcohol) as hydrogen bond donors and acceptors. These solvents served as environmentally benign extraction media, thereby avoiding the use of conventional volatile, toxic organic solvents. NADESs are naturally derived, easy to prepare, biodegradable, and environmentally friendly solvents. Hydrophobic and π-π interactions between the NADESs and PPs may contribute to enhancing the affinity of PPs toward the NADESs phase. Vortex technology, accelerating mass transfer between the sample and extractant phases, enables fast extraction of PPs. Under optimized conditions, the method achieved a low detection limit (0.002 mg L −1 ), satisfactory precision with relative standard deviations (0.3%–2.4%), and acceptable recovery (80.7%–86.2%). The method demonstrated excellent performance in urine analysis and was feasible as a facile and green strategy for monitoring the content of PPs in biological matrices and assessing exposure risk.
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JOURNAL OF CHROMATOGRAPHY A
·
2026
·
IF 4
Shuo Xie,Mengting Fu,Yike Han,Wanning Li,Penghui Li,Liyun Kong
An in situ DES-LLME/HPLC method was developed for neonicotinoids determination. • COSMO-RS was used to screen hydrogen bond donor for the in situ extraction. • Neonicotinoids content in wastewater and tea infusion was successfully detected. • This method offered a highly efficient, reproducible, and sustainable alternative. Accurate quantification of neonicotinoids (NEOs) in complex water and tea infusion samples is crucial for environmental risk assessment and human exposure evaluation. However, traditional sample pretreatment methods are often time-consuming, labor-intensive, and rely heavily on large volumes of toxic organic solvents. In this study, an innovative in situ deep eutectic solvent (DES)-based liquid-liquid microextraction (LLME) method was developed for the preconcentration of NEOs. Conductor-like Screening Model for Real Solvents (COSMO-RS) was employed to screen suitable hydrogen bond donors as extractants. The extraction mechanism relies on stable hydrogen bonding interactions between the target analytes (acting as hydrogen bond acceptors) and the hydrogen bond donor, hexyl 4-hydroxybenzoate. The optimized LLME procedure employs 10 mL aqueous sample, 150 mg hexyl 4-hydroxybenzoate, and 120 s vortex mixing. Compared with conventional extraction method, this approach significantly reduces sample volume to 10 mL, eliminates volatile organic solvents, simplifies the workflow, and completes sample preparation in < 20 min. In combination with high-performance liquid chromatography (HPLC), the proposed method enables sensitive simultaneous determination of six NEOs, with limits of detection (LODs) ranging from 0.390 to 3.165 μg/L, recoveries of 81.61–123.04%, and relative standard deviations precision of 2.32–16.13%. The developed in situ DES-LLME method, combined with HPLC, provides a rapid, sensitive, and practical approach for monitoring NEOs in aqueous environments, showing considerable potential for applications in environmental surveillance and human exposure assessment. Download: Download high-res image (231KB) Download: Download full-size image
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MICROCHEMICAL JOURNAL
·
2026
·
IF 5.2
Fenfen Zeng,Fuhui Luo,Yangting Ou,Wanting Liang,Xu Ren,Fengxiang Zhang,Hanqing Pang,Wei Shi
The simultaneous extraction of bioactive compounds with differing polarities from plant matrices remains a significant challenge. This study was conducted to overcome the drawbacks of traditional extraction methods for the precious medicinal herb Hedyotis diffusa (HD), such as their low extraction efficiency, incapacity to completely utilize HD, and instability of active ingredients. To this end, a biphasic DES with ultrasound assistance was developed for the simultaneous extraction of high-value iridoids and triterpenes from HD. Following a thorough screening process that encompassed 56 two-phase combinations, the choline chloride-acetic acid (ChCl-Aa)/L-menthol-n-octanoic acid (Men-Oa) system was identified as the optimal formulation. Through the implementation of polarity regulation and response surface methodology, this optimal biphasic DES attained extraction yields of 15.65 ± 0.19 mg/g for five target compounds under mild conditions (41.65 °C, 30.71 min, liquid-solid ratio 15.73 mL/g, hydrophilic-to-hydrophobic phase volume ratio 0.77), which is a 2–3-fold improvement over traditional extraction methods. Characterization results indicated that the DES facilitated target release primarily by forming hydrogen-bond networks, which not only enhanced solubilization but also contributed to the disruption of cell wall. This disruptive effect was further augmented by the biphasic interface generated under ultrasonication, leading to significantly improved extraction efficiency. This strategy establishes a green and efficient approach for the valorization of plant resources.
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