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JOURNAL OF FLUORESCENCE · 2024 ·Vol. 35 ·期 4 ·1927-1936 · IF 2.6

ZnS:Mn Quantum Dots Coated with a Silica Molecularly Imprinted Polymer for Trace Teflubenzuron Detection in Vegetable Samples

Feng Tian,Chen Zhenkun,Cheng Xiaomin

A novel nanocomposite fluorescent probe consisting of quantum dots and a silica molecularly imprinted polymer (MIPs-capped ZnS:Mn QDs) was synthesized and applied for the rapid detection of teflubenzuron (TBZ) based on the fluorescence quenching of a composite probe via TBZ. The fluorescence quenching efficiency of MIP@SiO2@ZnS:Mn QDs displayed a linear relationship over the concentration range of 0–26.24 μmol/L with a correlation coefficient of 0.9857 and the limit of detection was 2.4 μg/L. The selectivity test showed that the nanocomposite had good selectively rebind TBZ with higher imprinting factor of 3.06 compared with four structurally similar compounds. In addition, the probe was successfully applied to the detection of TBZ in vegetable samples with a recovery of 90.3~97.1% and with a relative standard deviation below 3.2%. This developed method has the advantages of simple preparation, fast response and low toxicity for trace TBZ detection.

研究领域: 分析化学 · 纳米技术 · 环境科学 · 食品安全 · 材料科学
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CHEMICAL ENGINEERING JOURNAL · 2025 · IF 13.2

Ionic liquids accelerate the crystallization of a magnetic fluorine-functionalized 3D covalent organic framework for efficient capture of trace benzoylurea insecticides in juices and beverages

Zekun Liu,Lu Liu,Yan Dong,Yan Li,Chong Zhang,Xiao-Li Wang,Lingxi Zhao,Hai-Long Jiang,Yong-Ning Wu,Xiangfeng Chen,Feng Li,Ru-Song Zhao

The fabrication of functionalized three-dimensional covalent organic frameworks (3D COFs) involves intricate and demanding synthetic procedures, which has significantly restricted their broad applications. However, ionic liquids (ILs) have demonstrated the capability to facilitate COF crystallization, shorten reaction durations, and achieve functional modification of COFs. Furthermore, the excessive utilization of benzoylurea insecticides (BUs) in agricultural products is substantially hazardous to ecological systems and human health. Herein, we proposed for the first time a mixed ILs-mediated Schiff base polymerization strategy. It enabled one-step synthesis of a highly crystalline NH₂-Fe₃O₄@F-3D COF at room-temperature conditions, specifically designed for the detection of BUs in complex food matrixes. NH₂-Fe₃O₄@F-3D COF contained a distinctive and well-connected porous structure as well as a high specific surface area (361.4 m 2 /g). It also contained abundant exposed -F groups and a small quantity of -COOH functionalized groups, which were introduced by the 2,3,5,6-tetrafluorobenzaldehyde monomer and ILs. NH₂-Fe₃O₄@F-3D COF exhibited a favorable affinity toward BUs via fluorine‑fluorine affinity and hydrogen bonding interaction. The approach manifested a wide linear scope (25–10,000 ng/L) and possessed low detection thresholds (0.42–2.93 ng/L) regarding the nine analytes being examined. Its effectiveness was further assessed by employing it for detecting BUs in juices and beverages, thus corroborating its adequacy in quantifying trace amounts of BUs in complex food matrixes. The devised high-performance polymerization and functionalization strategy, specifically engineered to fabricate 3D COFs, exhibits extraordinary potential utility in the identification and quantification of contaminants present within practical samples.

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JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY · 2024 · IF 5.7

Unraveling Key Amino Acid Residues Crucial for PxGSTs1 Conferring Benzoylurea Insecticide Resistance in Plutella xylostella

Yifan Li,Ruichi Li,Hainan Shao,Zhuoda Liu,Xueyi Gao,Zhen Tian,Yalin Zhang,Jiyuan Liu

The widespread use of benzoylurea insecticides (BUs) has led to significant resistance issues in various agricultural pests. Previous studies have demonstrated that the overexpression of sigma glutathione S-transferase 1 (PxGSTs1) can confer resistance to novaluron in Plutella xylostella; however, the underlying molecular mechanism remains unclear. This study investigates the role of glutathione S-transferase PxGSTs1 in mediating resistance to BUs in P. xylostella. Using a combination of RNA interference and transgenic Drosophila models, we demonstrated that the overexpression of PxGSTs1 significantly contributes to the resistance against BUs. Functional assays revealed that PxGSTs1 binds to these insecticides with varying affinities. Structural analysis through homology modeling and molecular docking identified the importance of hydrogen bonding and pi–pi stacking in resistance mechanisms. Site-directed mutagenesis confirmed the critical role of Ser65 and Tyr97 in these interactions. Our findings provide a molecular basis for the development of novel BUs and inform strategies for managing BU resistance in P. xylostella.

研究领域: 昆虫学 · 分子生物学 · 害虫管理
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FOOD CHEMISTRY · 2024 · IF 8.5

Construction of magnetic recoverable porous electron-rich organic frameworks for efficiently enrichment of phenylurea herbicides from water and milk samples prior to HPLC detection

Hua Wang,Lin Hao,Yaxing Guo,Chun Wang,Qiuhua Wu,Zhi Wang

Porous electron-rich organic frameworks have attracted an increased attention in the adsorption and removal of pollutants due to their abundant electron-rich nitrogen atoms, which can effectively interact with positively charged substance. In this study, a porous electron-rich organic framework (Car-POF) and positively charged amino-functionalized magnetic nanoparticles (Fe 3 O 4 -NH 2 ) were used to construct a magnetic electron-rich Fe 3 O 4 -NH 2 @Car-POF for the enrichment of some phenylurea herbicides from water and milk samples prior to high performance liquid chromatographic detection. The adsorption capacity of Fe 3 O 4 -NH 2 @Car-POF for the phenylureas ranged from 14.93 to 28.83 mg g −1 . The LODs were observed in the range of 0.05–0.20 ng mL −1 and 0.5–1.5 ng mL −1 , and LOQs in the range of 0.17–0.66 ng mL −1 and 1.7–5.0 ng mL −1 for water and milk samples with RSD less than 9.0. The adsorption studies with cationic and anionic dyes revealed that Fe 3 O 4 -NH 2 @Car-POF is favorable for the adsorption of positively charged compounds.

研究领域: 环境科学 · 分析化学
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ANALYTICAL CHEMISTRY · 2024 · IF 6.7

Design and Synthesis of Fluorine-Containing Embedded Carbon Dots Stationary Phase for Separation of Versatile Analytes

Zhihua Song,Wenpu Wu,Lei Sui,Xinyan Han,Hui Xu,Gangqiang Yang,Peng Zhang,Na Zhou,Lingxin Chen,Jinhua Li

Thus far, numerous new stationary phases have been developed. A fluorine-containing embedded carbon dots (F3-CDs-SiO2) stationary phase was first designed and synthesized. The resulting F3-CDs-SiO2 stationary phase was characterized carefully by scanning electron microscopy, transmission electron microscopy, elemental analysis, X-ray photoelectron spectroscopy, and Brunauer–Emmett–Teller experiment. The F3-CDs-SiO2 stationary phase was slurry packed into the HPLC column (150 × 2.1 mm) for evaluation. Furthermore, the F3-CDs-SiO2 column was successfully used for separation of pesticides, nucleosides, sulfonamides, alkaloids, and alkylbenzenes. The retention mechanism (including hydrophobic interaction, F–F, hydrogen bond interaction, ion-exchange, dipole–dipole interaction, electrostatic interaction, etc.) was investigated carefully. Meanwhile, the F3-SiO2 stationary phase was synthesized and used to evaluate the role of CDs. Furthermore, various commercial stationary phases (including amino-SiO2, diol-SiO2, C18-SiO2, and PFP-SiO2) were used for comparison. Moreover, the F3-CDs-SiO2 column possessed good repeatability, reproducibility, and stability in separation of versatile analytes.

研究领域: 分析化学 · 材料科学 · 化学工程
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JOURNAL OF SEPARATION SCIENCE · 2024 ·Vol. 47 ·期 11 ·2300730 · IF 2.8

Alien species water hyacinth realizes waste into treasure: The preparation of biomass sorbent to determine benzoylurea insecticides in tea products

Hongmei Liu,Baogui Ye,Zhongwei Zhao,Mengyun Liu,Fangbin Fan,Caihong Tao

A fast and effective analytical method with biomass solid-phase microextraction sorbent combined with a high-performance liquid chromatography-ultraviolet detector was proposed for the determination of benzoylurea (BU) insecticides in tea products. The novel sorbent was prepared by activating and then carbonizing water hyacinth with a fast growth rate and low application value as raw material and showed a high specific surface area and multiple interactions with analytes, such as electrostatic action, hydrogen bonding, and π-π conjugation. After optimizing the three most important extraction parameters (pH [X 1 ], sample loading rate [X 2 ], and solution volume [X 3 ]) by Box-Behnken design, the as-established analytical method showed good extraction performance: excellent recovery (80.13%–106.66%) and wide linear range (1–400 µg/L) with a determination coefficient of 0.9992–0.9999, a low limit of detection of 0.02–0.1 µg/L and the satisfactory practical application results in tea products. All these indicate that the water hyacinth-derived material has the potential as a solid-phase extraction sorbent for the detection and removal of BU insecticides from tea products, and at the same time, it can also achieve the effect of rational use of biological resources, maintaining ecological balance, turning waste into treasure, and achieving industrial production.

研究领域: 环境科学 · 分析化学 · 植物学
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MICROCHEMICAL JOURNAL · 2024 · IF 4.9

Room temperature in situ growth of fluorinated covalent organic framework on electrospun nanofibers for efficient detection of benzoylurea insecticide residue in water samples

Xuan Su,Jingjing Hui,Yusong Zhou,Wen-Bo Cheng,Xiwen He,Langxing Chen,Yukui Zhang

The accurate detection of benzoylurea insecticides (BUs) residues is vital for the environment and human health. In this work, a room-temperature synthesis strategy was developed to fabricate the covalent organic framework (COF)–polyacrylonitrile (PAN) nanofibers composite by an electrospinning technique. The COF was functionalized on PAN nanofibers via in situ polymerization of 1,3,5-tris(4-aminophenyl)triazine (TAPT) and 2,3,5,6-tetrafluoroterephthaldehyde (TFTA). The obtained TAPT-TFTA@PAN nanofibers showed a porous structure, high surface area, good crystallinity and excellent extraction efficiency to BUs. A sensitive method combining dispersive solid-phase extraction (DSPE) using TAPT-TFTA@PAN nanofibers as an adsorbent with liquid chromatography–ultraviolet detector was developed for trace analysis of four BUs in environment water samples. This method achieved a wide linear range of 0.5–200 ng·mL −1 for triflumuron and hexaflumuron, and of 0.5–150 ng·mL −1 for teflubenzuron and fluazuron. The limits of detection (S/N = 3) for four BUs ranged from 0.11 to 0.42 ng·mL −1 . The accuracy of the proposed method was validated by measuring trace BUs in the spiked water samples with recoveries in the range of 98.3 %∼125.3 %. The results demonstrated that the TAPT-TFTA@PAN nanofibers have great potential as an extractant for effective enrichment of benzoylurea insecticide from complex water samples.

研究领域: 环境科学 · 分析化学
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JOURNAL OF CHROMATOGRAPHY A · 2025 · IF 4

UiO-66 with missing cluster defects for high-efficient extraction and enrichment of benzoylurea insecticides

Xuejing Lou,Yingge Hao,Huina Zhou,Zhen Song,Youmei Wang,Minghua Lu

The creation of defects in crystalline structures can tune metal-organic frameworks (MOFs) properties, such as improving their adsorptive and catalytic performance with producing more porosity and active sites. In this work, the bimetallic UiO-66 containing Zn and Zr was prepared. And then UiO-66 with missing cluster defects (UiO-66-1/3) were obtained by acid washing to remove the Zn nodes. UiO-66-1/3 was used as sorbent of dispersive solid-phase extraction (dSPE) to extract and enrich (BUs). Combination with high-performance liquid chromatography-diode array detector (HPLC-DAD) was developed to detect trace BUs in soil samples. Adsorption equilibrium can be reached in 3 min. The method possesses high enrichment factor (202-325), low detection limit (0.005-0.04 ng·mL -1 ), and wide linear range (0.02-200 ng·mL -1 ). In addition, the recovery rate of UiO-66-1/3 as an adsorbent was still higher than 95% after reused for 16 times. This work provides a new material for the enrichment and detection of benzoylurea insecticides in the environment.

研究领域: 环境科学 · 分析化学
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ANALYST · 2024 · IF 3.6

Molecularly imprinted polymer-coated silica microbeads for high-performance liquid chromatography

Wenpu Wu,Cuichi Yu,Lei Sui,Hui Xu,Jinhua Li,Na Zhou,Lingxin Chen,Zhihua Song

Molecularly imprinted polymer (MIP)-based chromatographic separation materials, owing to their advantages of unique selectivity, low cost, suitable reproducibility, and acceptable stability, have attracted a great deal of research in different fields. In this investigation, a new type of MIP-coated silica (MIP/SiO2) separation material was developed using sulfamethoxazole as a template; the specific recognition ability of MIP and appropriate physicochemical properties (abundant Si-OH, suitable pore structure, good stability, etc.) of SiO2 microbeads were combined. The MIP/SiO2 separation materials were characterized carefully. Then, various compounds (such as sulfonamides, ginsenosides, nucleosides, and several pesticides) were used to comprehensively evaluate the chromatographic performances of the MIP/SiO2 column. Furthermore, the chromatographic performances of the MIP/SiO2 column were compared with those of other separation materials (such as non-imprinted polymer-coated silica, C18/SiO2, and bare silica) packed columns. The resolution value of all measured compounds was more than 1.51. The column efficiencies of 13 510 plates per meter (N m−1) for sulfamethoxazole, 11 600 N m−1 for ginsenoside Rd, and 10 510 N m−1 for 2′-deoxyadenosine were obtained. The acceptable results verified that the MIP/SiO2 column can be applied to separate highly polar drugs such as sulfonamides, ginsenosides, nucleosides, and pesticides.

CAS / MDL: 83121-18-0 64628-44-0
研究领域: 分析化学 · 材料科学 · 药学
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Polymer-Plastics Technology and Materials · 2024 · IF 2.6

Magnetic nanoparticles coated with a molecularly imprinted polymer via manganese-doped ZnS:Mn quantum dots for the determination of Triflumuron

Zhenkun Chen,Tian Feng,Xiaomin Cheng

A novel multifunctional silica magnetic molecularly imprinted polymer (MQDs-MIPs) nanoparticle probe was synthesized for the rapid detection of triflumuron (TFM). The fluorescence probe consists of magnetite (Fe3O4) as a core and is wrapped with a molecularly imprinted polymer doped with Mn-doped ZnS quantum dots (QDs). Under optimal detection condition, the fluorescence quenching efficiency of MIP@Fe3O4@ZnS:Mn QDs displayed a linear relationship over the concentration range of 0–27.88 μmol/L with a correlation coefficient of 0.9947. Four structurally similar compounds were selected for selectivity testing and the nanocomposite showed good selectivity with a higher imprint factor of 2.52. This developed method has the advantages of simple preparation, fast response and low toxicity for trace TFM detection.

研究领域: 分析化学 · 环境科学 · 材料科学
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FOOD CHEMISTRY · 2021 · IF 7.514

Room-temperature synthesis of magnetic covalent organic frameworks for analyzing trace benzoylurea insecticide residue in tea beverages

Junhong Xin,Yiran Zhou,Xia Wang,Guiju Xu,Meng Xie,Lu Liu,Rusong Zhao,Yongning Wu,Minglin Wang

A novel magnetic covalent organic framework (NH 2 –Fe 3 O 4 @COF) was prepared using a simple room-temperature synthesis in this study. These magnetic particles exhibited high adsorption performance with short adsorption time (10 min) for six benzoylurea insecticides (BUs) as magnetic solid-phase extraction (MSPE) adsorbents. Quantum chemistry calculation demonstrated that adsorption mechanism was primarily attributed to strong halogen bonds between electronegative O atoms of COF and electropositive F atoms of BUs as well as potential hydrophobic effect. Wide linearities (10–1000 ng·L −1 ) and low limits of detection (0.06–1.65 ng·L −1 ) for six analytes were obtained via liquid chromatography–tandem mass spectrometry. Applicability of the proposed method was further evaluated by analyzing four kinds of original tea beverages. Recoveries of six BUs in spiked samples ranged from 80.1% to 108.4%.

研究领域: 分析化学 · 食品科学 · 环境科学
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RSC Advances · 2020 ·Vol. 10 ·期 48 ·28664-28673 · IF 3.119

Study on the adsorption mechanism of benzoylurea insecticides onto modified hyperbranched polysilicon materials

Chaoran Liu,Xiaodong Huang,Zilin Meng,Heng Qian,Xinya Liu,Runhua Lu,Wenfeng Zhou,Haixiang Gao,Donghui Xu

Several hyperbranched polysilicon (HBPS) materials with different end group modifications were designed and synthesized and the structures were characterized. The modified HBPS polymers were applied to the adsorption of benzoylurea insecticides (BUs). The binding mode and binding energy between the HBPS and BUs were quantified and the results of an adsorption kinetics study and an adsorption thermodynamics experiment were verified by calculation and mutual verification. The adsorption mechanism of BUs onto HBPS was also discussed. The theoretical results show that the most effective way to combine the adsorbent and BUs is via hydrogen bonding when the end group is an amino group. Moreover, the most effective combination when the end group is β-cyclodextrin is the interaction of the BUs with the interior of the cavity to form a host–guest coating. The theoretical results of other end group-modified HBPS materials were also obtained and verified by adsorption experiments. In this work, an experimental method for obtaining the binding mode by theoretical calculations and then verifying it according to adsorption experiments was established.

研究领域: 农药科学 · 材料科学 · 环境科学
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