MOLECULES
·
2020
·Vol. 25
·期 4
·897
·
IF 3.267
Qian-Chun Zhang,Guang-Ping Xia,Jun-Yi Liang,Xiao-Lan Zhang,Li Jiang,Yu-Guo Zheng,Xing-Yi Wang
In this study, a novel monolithic capillary column based on a NH2-MIL-53(Al) metal–organic framework (MOF) incorporated in poly (3-acrylamidophenylboronic acid/methacrylic acid-co-ethylene glycol dimethacrylate) (poly (AAPBA/MAA-co-EGDMA)) was prepared using an in situ polymerization method. The characteristics of the MOF-polymer monolithic column were investigated by scanning electron microscopy, Fourier-transform infrared spectroscopy, X-ray photoelectron spectroscopy, X-ray diffractometry, Brunauer-Emmett-Teller analysis, and thermogravimetric analysis. The prepared MOF-polymer monolithic column showed good permeability, high extraction efficiency, chemical stability, and good reproducibility. The MOF-polymer monolithic column was used for in-tube solid-phase microextraction (SPME) to efficiently adsorb trace sulfonamides from food samples. A novel method combining MOF-polymer-monolithic-column-based SPME with ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) was successfully developed. The linear range was from 0.015 to 25.0 µg/L, with low limits of detection of 1.3–4.7 ng/L and relative standard deviations (RSDs) of < 6.1%. Eight trace sulfonamides in fish and chicken samples were determined, with recoveries of the eight analytes ranging from 85.7% to 113% and acceptable RSDs of < 7.3%. These results demonstrate that the novel MOF-polymer-monolithic-column-based SPME coupled with UHPLC-MS/MS is a highly sensitive, practical, and convenient method for monitoring trace sulfonamides in food samples previously extracted with an adequate solvent.Keywords:monolithic capillary column;metal-organic framework;sulfonamides;solid-phase microextraction;ultra-high performance liquid chromatography-tandem mass spectrometry
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FOOD CHEMISTRY
·
2025
·
IF 9.8
Hongbo Li,Hao Wang,Meiyi Cao,Xing Tong,Shuo Wang,Mingfei Pan
The fluoroquinolone-enrofloxacin (ENR) residue in animal-derived foods poses a significant threat to human health, thereby necessitating developing precise, efficient, and user-friendly detection methods. This study developed a dual-mode fluorescence-colorimetric immunosensing platform using the composite of bimetallic nanoparticles integrated with metal-organic frameworks (Au/Pt NPs@NH 2 -MIL-53(Al)). The Au/Pt NPs with biocompatibility and peroxidase-like activity were modified onto fluorescent NH 2 -MIL-53(Al) and conjugated with Ab 2 to construct signal probes. The platform enables dual-mode quantitative analysis through the competitive binding of ENR and ENR-BSA conjugate to signal probes. It demonstrated a wider linear range (0.08–180 ng/mL) and high sensitivity [LOD: 0.068 ng/mL (fluorescence), 0.066 ng/mL (colorimetric), and 0.074 ng/mL (smartphone-assisted color recognition)]. In real sample analyses, the recoveries ranged from 86.7 % to 106.7 %, with satisfactory stability (RSD ≤ 4.4 %, n = 3). The dual-signal mode facilitates results self-calibration, enhancing reliability, while smartphone-assisted color recognition enables on-site, convenient screening, offering great potential for ENR detection in complex food matrices.
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MICROCHIMICA ACTA
·
2021
·Vol. 188
·期 2
·1-9
·
IF 5.833
Senosy Ibrahim Abdelhai,Zhang Xin-Zhong,Lu Zhi-Heng,Guan Xiao-Yu,Yang Zhong-Hua,Li Jian-Hong,Guo Hao-Ming,Abdelrahman Talat Mahmoud,Mmby Mohamed,Gbiliy Asmaa
Fe 3 O 4 @MIL-100 (Fe)/PEI are used for the first time as an adsorbent material for the extraction of pesticide residues (epoxiconazole, flusilazole, tebuconazole, and triadimefon) from food matrices. The adsorbent proposed (Fe 3 O 4 @MIL-100(Fe)/PEI) was characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), transmission electron microscopy (TEM), field emission scanning electron microscopy (FE-SEM), thermogravimetric (TG) analysis, and vibrating sample magnetometer (VSM) techniques to evaluate the properties of the sorbent. Then, the Fe 3 O 4 @MIL-100 (Fe)/PEI was employed for the quantification of the four triazole fungicides in fruits and vegetables (apple, orange, tomato, cabbage, and cucumber) using HPLC-UV for separation and detection. During the extraction process, the main parameters such as amount of adsorbent, extraction time, pH value, ionic strength, eluting solvent, and eluting volume were optimized. Under the optimum conditions, good linearity of this method was observed for all analytes, with correlation coefficients ( R 2 ) ≥ 0.9908. The limits of detection (LODs) ranged from 0.021–3.04 μg kg −1 . The extraction recoveries of the four triazole fungicides varied from 73.9 to 109.4% with relative standard deviations (RSD) in the range 0.5 to 6.2%. Compared with other MOFs, the modification of Fe 3 O 4 @MIL-100 (Fe) with PEI shows high efficient adsorption due to the combined benefits of MIL-100 (Fe) and PEI. The material is easily synthesized, has good stability, and is of low cost.
Graphical abstract
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ACS Applied Materials & Interfaces
·
2026
·
IF 7.8
Xiaopeng Zhang,Lin Chen,Longzhu Li,Xiaoming Yan,Junjiang Bao,Ning Zhang,Gaohong He
The introduction of guest metal molecules into metal–organic frameworks (MOFs) is an outstanding method to prepare dual-atom catalysts (DACs) with good oxygen reduction reaction (ORR) activity. However, most of the MOF-derived dual-atom catalysts reported to date exhibit a microporous structure and, therefore, suffer from the underutilization of active sites and poor mass transfer. This study employed NH2-MIL-101 as a precursor to form defect-bearing mesoporous Fe-NC via one-step pyrolysis for adsorbing [Co(en)3]3+, followed by secondary pyrolysis to generate Fe–Co binuclear site catalysts. The mesopores of NH2-MIL-101 are beneficial to [Co(en)3]3+ introduction and can improve the mass transfer of the ORR. Furthermore, the elevated nitrogen content within the [Co(en)3]3+ complex facilitates the co-coordination of Fe and Co with nitrogen, thereby enhancing the formation of Fe–Co diatomic sites. As a result, the obtained FeCo-NC-40 catalyst showed excellent ORR performance with a half-wave potential of 0.915 V (vs RHE). In addition, the liquid-phase Zn–air battery employing FeCo-NC-40 as the cathode catalyst demonstrated a peak power density of 178.13 mW·cm–2 and achieved a discharge specific capacity of 806.13 mAh·g–1 at 10 mA·cm–2, and there was no significant decay in stability for 10 days of continuous cycling.
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MICROCHEMICAL JOURNAL
·
2026
·
IF 5.2
Xu Xu,Yumeng Liu,Jia Lv,Baocheng Ji,Junguang Li,Ke Li,Dianbo Zhao,Yanhong Bai
A modified QuEChERS method was developed in analysis of 52 veterinary drugs. • A novel MIL-101(Cr)–rGO@melamine sponge composite was fabricated. • The fast matrix purification could be achieved within several seconds. • Matrix cleanup was achieved through simple soaking and squeezing. • The method showed low matrix effects, good recoveries, and high precision. Herein, we report the fabrication of an elastic, quick, easy, cheap, effective, rugged, and safe adsorbent using a functionalized melamine sponge (MLS) and used it for the high-throughput analysis of 52 veterinary drugs in beef liver samples via ultraperformance liquid chromatography–tandem mass spectrometry. The as-prepared adsorbent was obtained by successive loading of Matérial Institut Lavoisier-101 (Chromium) [MIL-101(Cr)] and reduced graphene oxide (rGO) on melamine sponge skeletons. Excellent linearity with determination coefficients of ≥0.9942 was obtained across a range of 0.25–200 μg·kg −1 . Relatively low limits of detection (0.1–4.9 μg·kg −1 ) and limit of quantitation (LOQ; 0.3–16.2 μg·kg −1 ) were obtained. When fortified at three levels (1×, 5×, and 10× LOQ), spiked recoveries varied between 63.5% and 115.4%, with the intraday and interday relative standard deviations of ≤12.9%. Through direct infiltration and compression, efficient matrix purification was accomplished within seconds, yielding negligible matrix effects (from −18.4% to +19.1%). Thus, the MIL-101(Cr)–rGO@MLS adsorbent possesses high potential for fast, convenient, and efficient matrix purification in complex sample analysis. Download: Download high-res image (179KB) Download: Download full-size image
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JOURNAL OF SOLID STATE CHEMISTRY
·
2026
·
IF 3.2
Yuye Li,Tianao Liu,Tingting Du,Congzhi Hu,Youyong Pang,Yongping Liu,Botian Liu,Ling Li,Huidan Lu,Bin Huang
Dyes and antibiotics possess high stability and are resistant to microbial degradation, leading to their persistence in the natural environment. Photocatalysis is an effective and green degradation method. In this work, a novel Ag/AgCl/NH 2 -MIL-53(Fe) (AAF) heterojunction photocatalyst was prepared using a solvothermal method, precipitation method, and photochemical reduction method, which effectively promotes the separation of photogenerated charge carriers. The study shows that the composite consisting of 95 wt% Ag/AgCl/NH 2 -MIL-53(Fe) (AAF-95) can photocatalytically degrade 99.4% of RhB within 15 min and 82.4% of TC within 12 min, achieving higher photocatalytic degradation activity than the individual materials. The main active species involved in the degradation are h + and •O 2 - . Based on Mott-Schottky tests, radical trapping experiments, and UV-vis DRS, a possible photocatalytic degradation mechanism and the advantages are proposed: AAF-95 broadens the light absorption range, and the NH 2 -MIL-53(Fe) increases the specific surface area, thereby enhancing the catalytic reaction activity. The coupling between the heterojunction and the SPR effect promotes the separation of photogenerated charge carriers and lowers the catalytic reaction barrier. These are the reasons for the enhanced photocatalytic degradation capability of the composite.
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TALANTA
·
2026
·
IF 6.7
Xiao Liang,Haifeng Wei,Xiantao Zeng,Yan Zhang,Cheng Rui,Mingyue Shen,Fan Liu,Lan Guo,Yiqun Wan
Prepared dishes, one of the prominent modern foods, carry the risk of alternaria toxins (ATs) contamination. To address this concern, an efficient dispersed solid-phase extraction (d-SPE) method based on MIL-101(Fe) coupled with ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method was developed for the analysis of six ATs in prepared dishes. Characterization results confirmed that the synthesized MIL-101(Fe) possesses a high specific surface area and appropriate pore sizes distribution. Furthermore, computational simulations revealed that ATs could be efficiently absorbed and purified by MIL-101(Fe) via hydrogen bonding, π-π stacking, and Lewis acid-base interactions. Under optimized conditions, the method exhibited excellent linearity (R 2 ≥ 0.9990), and the limit of quantifications (LOQs) ranging from 0.07 to 0.37 μg/L, with recoveries in the range of 76.2%-108.3% and relative standard deviations (RSDs) below 9.8%. this study aims to bridge this gap by utilizing UHPLC-MS/MS to develop a robust method for the high-sensitivity and high-accuracy quantification of ATs in prepared dishes. Furthermore, the adsorption mechanism of MIL-101(Fe) for target toxins was elucidated by grand canonical Monte Carlo (GCMC) simulation and Density Functional Theory (DFT) calculation.
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OPTICAL MATERIALS
·
2022
·
IF 3.754
Yang Wang,Sheng Feng,Changchang Ma,Yun Zhou,Zhiwei Ye,Xiaojun Dai,Xun Cao
In this paper, a novel Mn-doped CdS@NH 2 -MIL-125(Ti) (MC@NT) photocatalytic composites was synthetized through hydrothermal method . Hydrogen desorption and tetracycline and oxytetracycline degradation were performed under visible light to test their photocatalytic activities . The composites were characterized by XRD , FTIR, SEM, TEM, XPS , UV–Vis diffuse reflectance spectroscopy (DRS), EPR , EIS, and transient photocurrent response. From the characterization consequence, it could be seen that Mn-doped CdS was tightly attached to the surface of tetragonal NT in the form of nanoparticles . The MC@NT composites exhibited more promising catalytic activity than pristine monomeric materials. The photocatalytic hydrogen evolution rate reached 3.61 mmol g −1 h −1 . Within 110 min, the degradation efficiencies of TC and OTC were 90% and 88%, respectively. The free radical trapping experiments proved that ·O 2 − and h + were decisive role for degrading pollutants in the degradation catalysis process. Radical trapping experiments and electron spin resonance (ESR) indicated that the Z-scheme heterojunction was formed between Mn-doped CdS and NT, leading to facilitate the migration and shift of photogenerated carriers and holes. Cycling experiments showed that the as-prepared composites have good stability and have good prospects for practical applications. We believe this work will offer new ideas on the future development of efficient heterojunction catalysts for light energy conversion and other applications.
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FOOD CHEMISTRY
·
2023
·
IF 8.8
Junxue Liu,Wenyan Ma,Yufei Wang,Qinfen Gu,Qinhe Pan,Siyu Zong,Minghao Qin,Jiyang Li
Monitoring of gallic acid (GA) in food and biothiols in humans is crucial for body health. Nanozyme-mediated colorimetric strategy for evaluating them has been widely applied nowadays, however, the inferior efficient and susceptible single-signal recognition limit its further application. Herein, a sensitive biosensor was first constructed for bimodal detection of GA and biothiols based on CDs@MIL-53(Fe)-NO 2 , prepared through a facile and time-saving microwave treatment. Benefiting from the excellent fluorescent and electron transfer properties of CDs, CDs@MIL-53(Fe)-NO 2 exhibited significant enhanced blue fluorescence and oxidase-like activity, which could oxide colorless 3,3′,5,5′-tetramethylbenzidine without H 2 O 2 , and the blue product could quench the fluorescence of composite. The dual-mode assay based on such bifunctional nanozyme showed an extremely sensitivity towards GA/ l -cysteine/homocysteine with the detection limit of 62/65/124 nM and 17/16/27 nM in colorimetric/fluorescent modes, respectively. The practicability in real samples and portability based on a smartphone of the analysis has been investigated with reliable results.
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TALANTA
·
2022
·
IF 6.556
Lin Li,Yingying Li,Sijia Zhang,Ting Wang,Xiaohong Hou
In this study, MIL-101(Cr)/cellulose aerogel/melamine sponge composite was fabricated through a simple soaking method. The composite was packed in the syringe barrel and used as the sorbent for microextraction in packed syringe. Coupled to UPLC-MS/MS, the proposed method was employed for the analysis of trace nitroimidazoles in water samples. The parameters affecting the extraction efficiency, including sorbent type, pH value of sample solution, sample solution volume and elution solvent were optimized. Under the optimal conditions, good linearity (r > 0.99 for five analytes), high sensitivity (limit of detection: 8.250–16.33 ng L −1 ), ideal precision (intra-day precision: 1.1%–5.3%, inter-day precision: 1.8%–6.7%) and satisfactory accuracy (recovery: 70.4%–96.7%) were achieved. The proposed method was proved to be efficient, easily operative and environmentally friendly.
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Nanoscale
·
2022
·Vol. 14
·期 18
·7055-7074
·
IF 8.307
Rutong Song,Jun Yao,Mei Yang,Zhongbin Ye,Zhuang Xie,Xiang Zeng
Water pollution control is one of the major challenges currently faced. With the development of photocatalytic technology, an increasing number of new and efficient catalysts have been developed, but most of the catalysts have limited light capture ability and catalytic degradation efficiency. Therefore, in this work, hydrogen peroxide was further introduced to establish a photo-Fenton system to improve the photocatalytic effect by constructing a Z-scheme, and the degradation ability of the catalyst was maximized. Moreover, we successfully adhered bismuth tungstate nanosheets onto the surface of a MIL-101(Fe) framework and changed the number of active sites with iron ions of different doping amounts. We found that the number of active sites in the photo-Fenton system does not increase linearly, but increases and decreases regularly, which is similar to the change in band structure after doping. In addition, the results of the radical scavenger experiment and electron paramagnetic resonance (EPR) revealed that both hydroxide radical (˙OH) and superoxide radical (˙O2−) participated in methylene blue (MB) degradation, of which ˙OH was the main active species for pollutant degradation. Based on high-performance liquid chromatography-mass spectrometry (HPLC-MS) analysis, the possible degradation pathways were proposed. We believed that this work will provide insights into the heterojunction photo-Fenton system.
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CHEMICAL ENGINEERING JOURNAL
·
2023
·
IF 15.1
Yarui Wang,Chengzhuo Yu,Sen Wang,Jin Xu,Fanglan Geng,Silong Wang,Jitao Lv,Lixia Zhao,Yawei Wang
Humic acids (HA) released during algal bloom poses a key challenge for efficient photocatalytic degradation of Microcystin-LR (MC-LR) due to their scavenging function on active species. Herein, MIL-101(Fe)/TiO 2 -P25 (M/P) was constructed to diminish the inhibitory effect of HA on the photocatalytic degradation of MC-LR. Results showed that MC-LR could be efficiently removed assigning to the photogenerated holes (h + ) and superoxide radical (O 2 •− ) oxidation under visible light irradiation, where the carboxy groups of D -glutamic acid (Glu) and methyl- D -aspartic acid (MeAsp), and Adda side chain related to MC-LR biotoxicity were selectively destroyed to achieve MC-LR detoxication. More importantly, HA exerted non-inhibitory effect on MC-LR removal by M/P. The counteracting mechanisms were studied. Firstly, the location of TiO 2 in the pore structure of MIL-101(Fe) could occupy the adsorption sites of HA, and decrease the HA adsorption on M/P. Furthermore, XPS analyses suggested the coordination of unsaturated Fe metal sites on the surface of M/P hybrids complexed with –OH and –COOH of HA, which could accelerate the electron transfer and reduce hole consumption. Thus, the inhibitory effect of HA was alleviated during photocatalytic MC-LR treatment. This work offers a possible way to remove MC-LR in an abundant HA matrix water system efficiently.
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