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ANALYTICA CHIMICA ACTA · 2015 · IF 4.513

Extensible automated dispersive liquid–liquid microextraction

Songqing Li,Lu Hu,Ketao Chen,Haixiang Gao

In this study, a convenient and extensible automated ionic liquid-based in situ dispersive liquid–liquid microextraction (automated IL-based in situ DLLME) was developed. 1-Octyl-3-methylimidazolium bis[(trifluoromethane)sulfonyl]imide ([C 8 MIM]NTf 2 ) is formed through the reaction between [C 8 MIM]Cl and lithium bis[(trifluoromethane)sulfonyl]imide (LiNTf 2 ) to extract the analytes. Using a fully automatic SPE workstation, special SPE columns packed with nonwoven polypropylene (NWPP) fiber, and a modified operation program, the procedures of the IL-based in situ DLLME, including the collection of a water sample, injection of an ion exchange solvent, phase separation of the emulsified solution, elution of the retained extraction phase, and collection of the eluent into vials, can be performed automatically. The developed approach, coupled with high-performance liquid chromatography–diode array detection (HPLC–DAD), was successfully applied to the detection and concentration determination of benzoylurea (BU) insecticides in water samples. Parameters affecting the extraction performance were investigated and optimized. Under the optimized conditions, the proposed method achieved extraction recoveries of 80% to 89% for water samples. The limits of detection (LODs) of the method were in the range of 0.16–0.45   ng   mL −1 . The intra-column and inter-column relative standard deviations (RSDs) were <8.6%. Good linearity ( r   >   0.9986) was obtained over the calibration range from 2 to 500   ng   mL −1 . The proposed method opens a new avenue for automated DLLME that not only greatly expands the range of viable extractants, especially functional ILs but also enhances its application for various detection methods. Furthermore, multiple samples can be processed simultaneously, which accelerates the sample preparation and allows the examination of a large number of samples.

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JOURNAL OF THE BRAZILIAN CHEMICAL SOCIETY · 2024 · IF 1.3

Polyamidoamine Dendrimer Modified Silica Nanoparticles: A Promising Sorbent for Benzoylurea Insecticides Detection in Tea Infusions

Zhang Yanchao,Cui Xiaoyan,Lin Xiwen,Mi Yiduo,Yan Yumei,Liu Xiaoyang,Jiao Keren,Gao Haixiang,Lu Runhua,Zhou Wenfeng

This research aims to develop a precise and efficient dispersive solid-phase microextraction (DSPE) technique using third-generation polyamidoamine (PAMAM) dendrimer-grafted nanoparticles to quantify benzoylurea pesticides in green tea, black tea, and oolong tea infusions. The extraction efficiency is optimized through single-factor adjustments of key parameters, including adsorbent quantity (5-20 mg), adsorption duration (5-20 min), desorbent identity (methanol, acetonitrile), volume (100-600 μL), sodium chloride concentration (0-10%, m/v), and sample solution pH (3-8). The optimized method demonstrates linearity in the range of 2-500 μg L-1, with limits of detection (LODs) ranging from 0.6-1.5 μg L-1 and limits of quantification (LOQs) from 2.0 5.0 μg L-1. Recovery rates of 81.2-96.0% are achieved, with intra-day relative standard deviations (RSDs) of 1.4-2.8% and inter-day relative standard deviations of 2.0-3.9%, indicating high accuracy and repeatability. The successful application of detecting residues in commercial tea samples underscores the strong potential of the technique to determine benzoylurea analyte levels.

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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.

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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.

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SENSORS AND ACTUATORS B-CHEMICAL · 2025 · IF 7.7

Co-binding-based supramolecular sensor array for fluorescence recognition of chitin synthesis inhibitors

Yilin Zhan,Zhongyong Xu,Lei Wang,Mingle Li,Xiaoqiang Chen,Taisheng Wang,Na Zhang,Bin Liu

The extensive agricultural use of chitin synthesis inhibitors (CSIs) has garnered significant concern due to their environmental persistence and potential ecological risks. A persistent challenge in this context is the concurrent discrimination and quantitative detection of multiple CSI residues in complex matrices. To address this issue, we developed a fluorescent sensor array utilizing a supramolecular system for the identification and quantification of four common CSIs: buprofezin, chlorfluazuron, diflubenzuron, and flufenoxuron. This system exploits the co-binding of a fluorescent indicator and CSI within the hydrophobic cavity of albumin, inducing pattern-based ratiometric fluorescence responses. The generated unique fluorescence fingerprint profiles for each CSI enable differentiation through multivariate statistical analyses, including linear discriminant analysis (LDA) and hierarchical cluster analysis (HCA), yielding 100 % classification accuracy across both individual CSIs and their mixtures. Furthermore, quantitative detection is facilitated by a linear correlation between LDA feature scores and CSI concentrations. The practical utility of this platform was substantiated by successful discrimination of CSIs in real-world samples, including millet, soil, and aqueous environments, with performance maintained across diverse matrix compositions, offering a critical advancement in addressing the analytical challenges posed by these persistent pesticide residues.

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