INTERNATIONAL JOURNAL OF BIOLOGICAL MACROMOLECULES
·
2026
·
IF 8.7
Li Shuofeng,Junmin Wang,Zhi Li,Qianqian Wang,Chun Wang,Qiuhua Wu
Herein, a novel chitosan-based magnetic bio-sorbent (M-Cs-BD@TBB) was synthesized through grafting chitosan with benzaldehyde (BD) and then crosslinking with 1,3,5-tris(bromomethyl)benzene (TBB) before modification with Fe 3 O 4 . Owing to the presence of multiple functional groups (-OH, -C=N, O , benzene ring), high porosity, and excellent wettability, M-Cs-BD@TBB demonstrated good adsorption performance for benzoylurea insecticides (BUs). Hydrogen bonding, π-π stacking, halogen bonding, and pore-filling were proved to be the potential adsorption mechanism. Moreover, the adsorption process of M-Cs-BD@TBB for BUs followed the Langmuir model and the pseudo-second-order kinetics model, indicating monolayer adsorption predominantly governed by chemical adsorption. Furthermore, M-Cs-BD@TBB exhibited remarkable utilization potentiality thanks to its outstanding preparation reproducibility, stability, and repeatability. Then, this reliable and innovative bio-sorbent coupled with high performance liquid-phase chromatography provided an attractive method for effectively trapping and detecting trace levels of BUs in food samples.
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CHEMICAL ENGINEERING JOURNAL
·
2025
·
IF 13.2
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 CHROMATOGRAPHY A
·
2022
·
IF 4.601
Huazi Wang,Tiantian Wang,MingXiu Hong,Ziyang Wang,Xiaoyan Jin,Hai Wu
This study describes the development of a fully manual method for on-site dispersive liquid-liquid microextraction based on the direct solidification of switchable-hydrophilicity salicylic acid (on-site DLLME-DSSA) coupled with high-performance liquid chromatography with an ultraviolet detector (HPLC-UVD) and its utilization for the detection of benzoylurea insecticides (BUs) in water and honey samples. Salicylic acid (SA), a switchable hydrophilic aromatic acid, was used as an extraction solvent. It can be converted into the hydrophobic/hydrophilic forms in pH-changeable solutions, facilitating facile and effective dispersion and phase separation. Moreover, the melting point of SA (significantly higher than room temperature) enables its direct solidification without an ice-water bath, facilitating its collection by filtration. The dispersion, separation, and collection of the extraction solvent were carried out entirely in a plastic syringe without requiring special apparatus or additional energy. Univariate and response surface analyses were used to optimize various parameters of the on-site DLLME-DSSA method. Under optimal conditions, the limits of determination (LODs) were 1.50 µg L −1 and 0.03–0.09 mg kg −1 in water and honey, respectively. The relative standard deviations (RSDs) for inter-day ( n = 5) and intra-day ( n = 5) precision were ≤8.4%, whereas the extraction recoveries and enrichment factors for the BUs ranged from 67.0 to 97.1% and 29 to 34, respectively. Furthermore, the proposed method was used for the on-site extraction and laboratory detection of BUs from real water and honey samples. Theoretical analyses indicated non-covalent interactions (such as hydrogen bonds, electrostatic interactions, van der Waals forces, and π-π interactions) to be the main driving force for extraction. This study introduces a switchable hydrophilic aromatic acid capable of direct solidification into on-site DLLME for the first time, opening new frontiers in the development of on-site sample pretreatment methods.
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JOURNAL OF CHROMATOGRAPHY A
·
2022
·
IF 4.601
Jia Chen,Xiaofei Han,Gafang Fu,Weiyang Tang,Kyung Ho Row,Hongdeng Qiu
In this work, magnetic nitrogen-doped porous carbon (Fe 3 O 4 @N-PC) was prepared via incomplete combustion coupled with solvothermal synthesis for extraction of four benzoylureas (BUs) insecticides. Among them, nitrogen-doped porous carbon was produced through incomplete combustion of filter paper loaded with mixture formed by Zn(NO 3 ) 2 ·6H 2 O and polyethyleneimine solution, and magnetic nanoparticles were further introduced by solvothermal method. Compared with magnetic porous carbon (Fe 3 O 4 @PC), the surface hydrophilicity of Fe 3 O 4 @N-PC was improved by virtue of the doping of nitrogen atoms, and the dispersion of Fe 3 O 4 was more uniform, which greatly exposed the adsorption site. The characterization of Fe 3 O 4 @N-PC were carried out by TEM, XRD, elemental analysis, XPS, BET and magnetic hysteresis curve. Besides, Fe 3 O 4 @N-PC was successfully used as magnetic solid-phase extraction (MSPE) adsorbent, which showed excellent enrichment factors and extraction recoveries toward polar BUs insecticides due to the polar surface and introduction of Lewis-basic nitrogen. The optimum amount of Fe 3 O 4 @N-PC adsorbent, extraction time, pH value, desorption solvent, desorption time and PEI concentration for BUs insecticides extraction were determined to be 3 mg, 10 min, 8, acetone/acetic acid (19:1, V/V), 6 min and 60 g L −1 , respectively. Under this experimental condition, the enrichment factors ranged from 182 to 192 with good intra- and inter-day relative standard deviations (RSDs). The calibration lines were linear over the concentration in the range of 1–800 μg L −1 , the limit of detection (LOD) and limit of quantification (LOQ) were 0.3 μg L −1 as well as 1 μg L −1 , respectively. The recoveries for spiked sample ranged from 90.7 to 107.3% in spiked Yellow River water with the RSDs less than 7.0%. The results showed that the established MSPE strategy based on Fe 3 O 4 @N-PC could be used for the detection of trace BUs in complex samples.
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ANALYTICA CHIMICA ACTA
·
2022
·
IF 6.911
Wei Xie,Yulong Ju,Jian Zhang,Yiwen Yang,Yanbo Zeng,Hailong Wang,Lei Li
A magnetic Fe 3 O 4 @SiO 2 @MIPIL fluorescent sensor for the determination of imidacloprid (IMD) with high sensitivity and specificity was prepared through surface molecular imprinting technology on the surface of Fe 3 O 4 @SiO 2 by using dialkenyl ionic liquid (C) as a fluorescent polymer monomer . The as-prepared sensor was characterized by thermogravimetric, FT-IR, SEM, TEM, and nitrogen adsorption-desorption analysis. Results showed that IMD rapidly quenched the fluorescence of the sensor within 1 min and had an excellent linear relationship to the fluorescent quenching intensity of the sensor within the range of 1–1000 nM (IMD). The LOD was 0.3 nM (S/N = 3). The sensor had a specific response to IMD and was used to detect IMD in actual spiked environmental water and food samples with satisfactory result.
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FOOD CHEMISTRY
·
2022
·
IF 9.231
Shuofeng Li,Weihua Liu,Qianqian Wang,Mingming Xu,Yangjuan An,Lin Hao,Chun Wang,Qiuhua Wu,Zhi Wang
A magnetic covalent organic framework (COF) was constructed with ethidium bromide (EB) and 1,3,5-triformylphloroglucinol as building blocks. The prepared magnetic COF (named as EB-COF@Fe 3 O 4 ) exhibited high adsorption ability for five benzoylurea insecticides (BUs). By combining EB-COF@Fe 3 O 4 based magnetic solid-phase extraction with high performance liquid-phase chromatographic detection, a novel method was developed for determination of five BUs in water and food samples. Under the optimized conditions, a good linearity was obtained to be 0.03–100.0 ng mL −1 for water and juice, 0.9–500 ng g −1 for tomato. The detection limits of the method were 0.01–0.09 ng mL −1 , 0.03–0.3 ng mL −1 and 0.3–2.0 ng g −1 for water, juice and tomato samples, respectively. Satisfactory method recoveries were achieved in the range of 80.0%-116.0% with the intra-day and inter-day relative standard deviations below 10%. Moreover, the EB-COF@Fe 3 O 4 can be reused at least 25 times. Therefore, the established method is sensitive and robust for determining BUs in real samples.
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JOURNAL OF CHROMATOGRAPHY A
·
2022
·
IF 4.601
Xiang Li,Xiaofeng Lu,Xiaojing Liang,Yong Guo,Licheng Wang,Shuai Wang
A novel mosaic structured core-shell composite, Silica@C/Ni (Sil@C/Ni), has been prepared by embedding Ni nanoparticles on the surface of silica microspheres via coordination and carbonization reduction, and was used as magnetic solid-phase extraction sorbents in combination with high performance liquid chromatography (HPLC) for the extraction and determination of four benzoylurea insecticides (BUs) in tea leaves. Based on the fact that hydrogen bonding and hydrophobic interactions exist between the material and BUs, allowing BUs on the surface of the material can achieve rapid mass transfer and improved sorption performance, satisfactory extraction recoveries have been achieved in practical sample applications. Under the optimized experimental conditions, the linear ranges were 0.5–200 µg L −1 for diflubenzuron and triflumuron, 1.0–200 µg L −1 for teflubenzuron and 0.8–200 µg L −1 for flufenoxuron with the correlation coefficients R 2 ≥ 0.9991. The method has limits of detection and limits of quantification of 0.2–0.4 µg L −1 and 0.5–1.0 µg L −1 , respectively. The intra-day and inter-day relative standard deviations were less than 5%. The actual sample recoveries were 76.63–95.26%. In addition, Sil@C/Ni was used repeatedly for 15 times and still showed a relatively satisfactory recovery of the four BUs. Therefore, Sil@C/Ni has a high stability and can be used as an ideal magnetic solid phase extraction sorbent for the trace enrichment of BUs in tea-leaf samples.
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FOOD CHEMISTRY
·
2022
·
IF 9.231
Min Li,Weihua Liu,Xufeng Meng,Shuofeng Li,Qianqian Wang,Yaxing Guo,Yuanyuan Wu,Lin Hao,Xiumin Yang,Zhi Wang,Chun Wang,Qiuhua Wu
In this work, a novel knitting aromatic polymer (KAP) was fabricated for the first time by knitting ferrocene with 1,3,5-tris(bromomethyl)-2,4,6-trimethylbenzene via Friedel-Crafts reaction, and then the KAP was magnetically functionalized with Fe 3 O 4 nanoparticles to produce a magnetic KAP (M-KAP). Combining M-KAP based magnetic solid-phase extraction with high performance liquid chromatography-ultraviolet detection, a simple and sensitive method was developed for simultaneous determination of six benzoylurea insecticides (BUs) in honey and apple juice samples. In the optimized conditions, a good linearity for the BUs existed in the range of 1.67–1000 ng g −1 for honey sample and 0.500–100.0 ng mL −1 for apple juice sample. The limits of detection were 0.500–1.50 ng g −1 and 0.150–0.400 ng mL −1 for honey and apple juice sample, respectively. Satisfactory recoveries were in the range of 85.5–105.5% with RSDs ≤ 8.3%. The developed method demonstrated an excellent practicability for sensitive analysis of the BUs.
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JOURNAL OF CHEMICAL AND ENGINEERING DATA
·
2021
·
IF 2.694
Guangyu Xu,Fanyuan Zhang,Zhenghui Li
As a common solvent, water cannot dissolve flufenoxuron in this study well; therefore, methanol was added to the water to form a liquid mixture of different compositions. At first, the ratio of methanol mass was 90%, and then, it decreased by 10% until the methanol content was 10%. According to the above method, n-propanol, propylene glycol, and N,N-dimethyl formamide were made into corresponding mixed solvents. Under a pressure of 101.2 kPa, the temperatures of flufenoxuron and the solvent were kept at 278.15 K. Based on the basic principle of the static gravimetric method, the amount of solute diffusion in the above four mixed solvents was obtained. Other conditions remained unchanged, the temperature was increased by 5 K, and the above steps were repeated until the temperature was 323.15 K. There were two variables in the experiment; the temperature changes to a higher level and more flufenoxuron can be detected in the solution. Regardless of the change in temperature variables, the larger the mass of the organic solvent, the more solutes in the solution. Three models were employed to calculate the solubility of flufenoxuron. The maximum results of relative average deviation and the root-mean-square deviation were 0.43% and 4.24 × 10–4.
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FOOD CHEMISTRY
·
2021
·
IF 7.514
Weihua Liu,Juntao Wang,Shuangju Song,Lin Hao,Jiajia Liu,Yangjuan An,Yaxing Guo,Qiuhua Wu,Chun Wang,Zhi Wang
A uniform spherical structure covalent organic framework (TAPA-BPDA-COF) was prepared by a facile method at room temperature with tris(4-aminophenyl)amine (TAPA) and 4,4′-biphenyldicarboxaldehyde (BPDA) as building blocks. Based on the solid phase extraction with the TAPA-BPDA-COF as the sorbent and high performance liquid chromatography-diode array detection, a sensitive analytical method was established for the determination of four neonicotinoid insecticides from water and honey samples. Under the optimum conditions, good linear response for the quantification of the analytes was achieved in the range of 0.3–50.0 ng mL −1 for water samples and in the range of 8.0–500.0 ng g −1 for honey samples. The method recoveries fell in the range of 80.0–121.9% with RSDs less than 7.6%. The limits of detection at the signal to noise ratio of 3 were measured to be in the range of 0.08–0.12 ng mL −1 for water samples and 2.6–3.3 ng g −1 for honey samples, depending on compounds.
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JOURNAL OF CHROMATOGRAPHY A
·
2020
·
IF 4.049
Jiaxuan Fan,Zikai Liu,Jing Li,Wenfeng Zhou,Haixiang Gao,Sanbing Zhang,Runhua Lu
It is necessary to establish a rapid, simple and environmentally friendly detection method for benzoylurea pesticides (BUs) in environmental water samples because of their toxicity in environmental circulation. Herein, a novel polyethylene glycol (PEG) modified magnetic covalent organic framework material based on the Schiff base reaction was prepared (PEG/Fe 3 O 4 @SNW-1). This material was used as a sorbent for enriching five BUs by magnetic solid phase extraction prior to detection via high-performance liquid chromatography. After the optimization of several parameters (such as the salinity, extraction time, amount of sorbent, desorption time, etc.) that influenced the recovery of the magnetic solid phase extraction process, the limits of detection (S/N = 3) were defined as less than 1.0 μg L −1 , and the limits of quantitation (S/N = 10) were calculated as being lower than 3.4 μg L −1 . A satisfactory linear range of 5–1000 μg L −1 was achieved. Finally, the proposed method was applied to analyze benzoylurea pesticides in three environmental water samples. These results indicated that the proposed method was feasible and demonstrated the potential application of the PEG/Fe 3 O 4 @SNW-1 material for detecting similar pesticide residues in environmental water samples.
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RSC Advances
·
2020
·Vol. 10
·期 48
·28664-28673
·
IF 3.119
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.
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