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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TALANTA
·
2023
·
IF 6.1
Mengyao Mu,Shiping Zhu,Yanmei Gao,Ning Zhang,Youmei Wang,Minghua Lu
Due to widespread application of benzoylurea insecticides (BUs) and its persistence in environment, the effective capture of benzoylurea insecticides residues in environment is an important issue of environmental safety monitoring. To obtain excellent adsorption performance, creating defective structure in metal-organic frameworks (MOFs) can be employed as the method for adjusting its properties. Zirconium(Ⅳ)-based MOF termed as UiO-66-30% was constructed with 2-aminoterephthalic acid (NH 2 -BDC) and terephthalic acid (H 2 BDC) as building blocks. After calcination and removal of thermal-sensitive ligand (NH 2 -BDC), hierarchically porous UiO-66-30% (HP-UiO-66-30%) with multistage pore structure and good stability was obtained. The unique structure of HP-UiO-66-30% endowed it to achieve instantaneous equilibrium (within 2 min) when it was used as a dispersed solid phase extraction (d-SPE) adsorbent to extract BUs from environmental samples, greatly reducing the operation time. A wide linear range (0.05–200 ng mL −1 ), good linearity (R 2 ≥ 0.9980), low detection limits (0.01–0.03 ng mL −1 ) and quantification limits (0.05–0.1 ng mL −1 ) were obtained for BUs. In addition, the HP-UiO-66-30% material possessed the good reusability and the adsorption capacity did not change significantly over 16 adsorption-desorption cycles. Finally, the established dispersed solid phase extraction-high performance liquid chromatography-diode array detector (d-SPE-HPLC-DAD) method was successfully applied to determination of BUs residues in environmental soil samples. The results demonstrated that HP-UiO-66-30% was an excellent sorbent for extraction BUs from environmental samples.
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ANALYTICA CHIMICA ACTA
·
2023
·
IF 6.2
Xiang Li,Xiaofeng Lu,Xiaojing Liang,Zhimin Yang,Shuai Wang,Yong Guo
Background Large accumulations of pesticide residues in the environment eventually enter the human body with food. Based on magnetic solid-phase extraction (MSPE) technology , it is possible to achieve efficient extraction of trace pesticide residues in foodstuffs, and the construction of MSPE adsorbents with excellent magnetic properties and many active sites is still one of the main research topics. Based on this, we developed a new strategy for the preparation of "MOF-on-MOF" composites, which were carbonized and used as adsorbents for the extraction of pesticide residues in cereals. Results A novel corn cob core-shell composite Fe 2 O 3 @C@ZIF-8 was created by embedding ZIF-8 onto the surface of Fe 2 O 3 @C derived from MIL-88A(Fe), and used for the extraction of benzoylurea insecticides(BUs) from cereals. The adsorption behaviour between Fe 2 O 3 @C@ZIF-8 and BUs was investigated by static and kinetic experiments and the adsorption mechanism was elaborated. For the trace analysis of BUs, a magnetic solid-phase extraction combined with high performance liquid chromatography-ultraviolet detector (HPLC-UV) approach was also developed. Under the optimized experimental conditions, the limits of detection and quantification were 0.015–0.03 μg L −1 and 0.05–0.1 μg L −1 , and the relative standard deviations for the intra-day and inter-day ranges were 1.82%–2.13 % and 3.85%–4.59 %, respectively. The spiked recoveries of the four cereals ranged from 82.72% to 104.45 %. After 10 cycles of use of Fe 2 O 3 @C@ZIF-8, the recoveries of BUs ranged from 77.90% to 96.74 %. Significance The analytical method based on Fe 2 O 3 @C@ZIF-8 as adsorbent has a low limit of detection, a wide linear range and is highly applicable to the analysis of real samples. In addition, the strategy developed in this study for the preparation of thermoplastic polymer-assisted "MOF-on-MOF" composites has promising applications.
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FOOD CHEMISTRY
·
2023
·
IF 8.8
Xian-Xian Ji,Yu-Long Liu,Xin-Yue Chang,Rui-Long Li,Fei Ye,Liu Yang,Ying Fu
Diflubenzuron is widely used as a benzoylurea insecticide, and its impact on human health should not be underestimated. Therefore, the detection of its residues in food and the environment is crucial. In this paper, octahedral Cu-BTB was fabricated using a simple hydrothermal method. It served as a precursor for synthesizing Cu/Cu 2 O/CuO@C with a core–shell structure through annealing, creating an electrochemical sensor for the detection of diflubenzuron. The response of Cu/Cu 2 O/CuO@C/GCE , expressed as Δ I / I 0 exhibited a linear correlation with the logarithm of the diflubenzuron concentration ranging from 1.0 × 10 −4 to 1.0 × 10 −12 mol·L −1 . The limit of detection (LOD) was determined to be 130 fM using differential pulse voltammetry (DPV). The electrochemical sensor demonstrated excellent stability, reproducibility, and anti-interference properties. Moreover, Cu/Cu 2 O/CuO@C/GCE was successfully employed to quantitatively determine diflubenzuron in actual food samples (tomato and cucumber) and environmental samples (Songhua River water, tap water, and local soil) with good recoveries. Finally, the possible mechanism of Cu/Cu 2 O/CuO@C/GCE for monitoring diflubenzuron was thoroughly investigated.
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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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JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY
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2022
·
IF 5.895
Lijuan Zang,Yutao Ren,Man He,Beibei Chen,Bin Hu
A fluorinated covalent organic framework (COF), named F-COF, was fabricated via simple room-temperature synthesis. With the characteristics of rich fluorine atoms, hydrophobicity, and large conjugated structure, F-COF was evaluated for the extraction of five benzoylurea insecticides (BUs) containing fluorine atoms, benzene ring, and urea bridge. Specifically, F-COF-coated stir bars were prepared by physical adhesion and exhibited higher extraction recovery (73–93 versus 40–85%) toward BUs than commercial stir bars in a shorter extraction time (50 min versus 24 h). The adsorption behavior of BUs on F-COF was explored, and it was assumed that the halogen bond (O–F), hydrophobic interaction, electrostatic interaction, and π–π stacking contributed to the adsorption. On the basis of it, a method combining stir bar sorptive extraction with liquid chromatography–ultraviolet detector was developed for trace analysis of five BUs. Under the optimal conditions, the limits of detection for BUs were found to be 0.301–0.672 μg/L, with the linear range of 1.0/2.0–500 μg/L and relative standard deviations of <8.0% (c = 5 μg/L and n = 7). The accuracy of the proposed method was validated by the recovery test, and the recoveries of target BUs in spiked pear juice and pear beverage were 82.0–113 and 84.0–112%, respectively.
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Analytical Methods
·
2022
·Vol. 14
·期 33
·3153-3159
·
IF 3.532
Ling Mei,Tiantian Si,Shuai Wang,Jie Zhu,Hao Tang,Xiaojing Liang
The TiO2@MOF-919(Fe–Cu) solid-phase extraction material was prepared by growing MOF-919(Fe–Cu) in situ on three-dimensional radial TiO2 microspheres by a simple solvothermal method. This combination drew on both the resources of good single dispersion and extraction rate, which made it a better extraction material. It was accompanied with high-performance liquid chromatography (SPE–HPLC) for the separation and determination of four benzoylurea pesticides (triflumuron, chlorbenzuron, teflubenzuron and diflubenzuron) in afforestation irrigation water and juice samples (grape, peach and apple juices). Under the optimal conditions, the linearity of the method ranged from 1 to 400 μg L−1 with a correlation coefficient (R2) ≥ 0.9994, while the detection limit was in the range of 0.40–0.56 μg L−1 for the four pesticides. The adopted material showed good reusability and can be used no less than 10 times. The intra-day and inter-day precision were in the range of 1.78–3.24% and 4.06–5.08%, respectively. The proposed method was then successfully applied for the detection of benzoylurea pesticides in the spiked samples with good recoveries (72.3–108.4%) and good precision (5.15%) due to π–π and hydrophobic interactions between the analytes and adsorbent. The results show that the composite had the potential to be used as a SPE adsorbent for the enrichment and extraction of benzene ring structures containing imide groups in actual 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
·
2022
·
IF 3.119
Guangyu Xu,Fanyuan Zhang,Zhenghui Li
The equilibrium solubility of teflubenzuron in solvent mixtures of methanol (1) + water (2), ethanol (1) + water (2), propylene glycol (1, PG) + water (2), and N,N-dimethylformamide (1, DMF) + water (2) was determined experimentally by an isothermal dissolution equilibrium method within the temperature ranging from 278.15 to 323.15 K under an atmospheric pressure of 101.1 kPa. The solubility of teflubenzuron increased monotonously with the increase in mass fraction of methanol, ethanol, PG, and DMF and temperature. At the same temperature and mass fraction of methanol (ethanol, PG, and DMF), the mole fraction solubility of teflubenzuron is greater in DMF + water than in the other three solvent mixtures. Besides, the solubility of teflubenzuron was correlated with three models. The obtained average relative deviation (RAD) is lower than 0.41% for correlative studies. It is noteworthy that the solubility data presented in this work contributes to expansion of the physicochemical information about the solubility of drugs in binary solvent mixtures and also allows the thermodynamic analysis of the respective dissolution.
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MICROCHEMICAL JOURNAL
·
2023
·
IF 4.8
Juntao Wang,Jiajia Liu,Weihua Liu,Ziwang Liu,Qiuhua Wu,Zhi Wang,Hongyuan Yan
A novel magnetic hyper crosslinked polymer (BTA-MHCP) was prepared by one-pot reaction of benzotriazole, 1,3,5-triphenylbenzene and phenyl-functionalized Fe 3 O 4 @SiO 2 . The BTA-MHCP was then investigated as the adsorbent for the rapid magnetic solid-phase extraction (MSPE) of the 5-nitroimidazoles (5-NDZs) including dimetridazole, metronidazole, secnidazole, ronidazole and ornidazole. The adsorbent showed good adsorption properties for the 5-NDZs. The key factors that affect the MSPE such as extraction time, the amount of sorbent, and the type of eluent and its volume were optimized. Under the optimal conditions, the linear response ranges for the established method were 0.15–100.0 ng mL −1 and 3.9–100.0 ng g −1 for drinking water and fish samples, respectively, with the coefficients of determination ( r 2 ) of 0.9981 to 0.9998. The limits of detection (S/N = 3) for the analytes were 0.02–0.05 ng mL −1 and 0.7–1.3 ng g −1 , and the method recoveries ranged from 92.0% to 101.0% and from 89.9% to 104.0% for drinking water and fish samples, respectively.
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JOURNAL OF CHROMATOGRAPHY A
·
2023
·
IF 4.1
Mingcai Ma,Xiaofeng Lu,Licheng Wang,Yong Guo,Hui Ding,Shuai Wang,Xiaojing Liang
Hydrophobization and stability is crucial for the practical application of most metal-organic frameworks (MOFs) in extraction technique. In this study, a stable core-shell MOF@COF composite (NH 2 -MIL-101(Fe)@TAPB-FPBA-COF) was successfully prepared by Schiff base reaction and applied to solid-phase extraction (SPE) of hydrophobic flavonoids. Notably, the TAPB-FPBA-COF shell acts as a hydrophobic "shield", which not only improves the hydrophobicity and stability of hydrophilic NH 2 -MIL-101(Fe), but also makes the extraction efficiency of flavonoids from MOF@COF composite significantly higher than that of pure NH 2 -MIL-101(Fe) and TAPB-FPBA-COF. In addition, a sensitive analytical method with excellent linearities (0.1–500 ng mL −1 , R 2 ≥ 0.9967), low limits of detection (0.02–0.04 ng mL −1 for water; 0.04–0.07 ng mL −1 for grape juice; 0.06–0.08 ng mL −1 for honey), good repeatability (intra-day/inter-day precision are 1.86–5.37%/1.82–7.79%, respectively) and only 5 mg of adsorbent per cartridge was established by optimizing the SPE process combined with high performance liquid chromatography with ultraviolet-visible detector (HPLC-UV). Meanwhile, selectivity study and comparative experiments with the commercial C18 adsorbent showed that the MOF@COF adsorbent exhibited satisfactory extraction efficiency for flavonoids due to multiple interactions such as hydrogen bonding, hydrophobic, and π-π interactions. Finally, the good recoveries in grape juice (84.5–102.5%) and honey (87.5–104.6%) samples further validated the applicability of the proposed method in complex samples.
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MICROCHIMICA ACTA
·
2023
·Vol. 190
·期 11
·1-11
·
IF 5.7
Li Dan,Gao Yanmei,Mu Mengyao,Zhu Shiping,Zhang Ning,Lu Minghua
Ionic liquid (IL)-modified UiO-66-NH 2 composite was prepared and used as sorbent of dispersed solid-phase extraction (dSPE) for extracting trace benzoylurea insecticides (BUs) from complex environmental matrices. The IL in framework endowed the prepared material had electropositive characteristics, which can produce interaction with electron rich guest molecules, such as BUs. The high thermal and chemical stability of UiO-66-NH 2 /IL enabled it to be reused for 16 times without significant reduction in adsorption performance. Due to the multiple forces including π-π, hydrogen bonding, and fluorine-fluorine interaction, UiO-66-NH 2 /IL showed good adsorption performance, short adsorption time (20 s) and rapid desorption ability (60 s) for BUs. Under the optimal conditions, the method exhibited wide linear range (0.02–500 ng mL -1 ) with correlation coefficient ( R 2 ) not worse than 0.9928, high enrichment factor (252–300), and low detection limit (0.005–0.4 ng mL -1 ). The dispersed solid phase extraction coupling with high-performance liquid chromatography-diode array detector (dSPE-HPLC-DAD) was successfully used to detection of BUs in real environmental samples and satisfactory recoveries were obtained (80.5%±2.4–118%±3.2). The results indicated that UiO-66-NH 2 /IL composite can be a potential sorbent for the preconcentration of trace insecticides in environmental samples. Graphical abstract
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危险品化学品经营许可证（带存储）