MICROCHEMICAL JOURNAL
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2024
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IF 4.9
Yanling Liu,Yuying Chen,Xiaping Zhu,Ping Zhao,Wei Ren
The magnetic solid phase extraction material (MnFe 2 O 4 @TiO 2 ) was prepared by coating TiO 2 on MnFe 2 O 4 through an in-situ formation method. The structure and properties of MnFe 2 O 4 @TiO 2 were characterized by X-ray diffractometer (XRD), scanning electron microscope (SEM), nitrogen adsorption–desorption experiment, and vibrating sample magnetometer (VSM). The conditions for magnetic solid phase extraction (MSPE) of quinolone antibiotics were optimized, and an MSPE-HPLC method was established to determine quinolone antibiotics in water samples. The optimal conditions for MSPE are MnFe 2 O 4 @TiO 2 amount of 15 mg, extraction time of 15 min, 5 mL of methanol solution with 20 % ammonia as eluent, and elution time of 1 min. Under the optimal conditions, 50 mL 0.1 mg/L mixed standard solutions of fleroxacin, ofloxacin, norfloxacin, ciprofloxacin, and enrofloxacin have achieved enrichment multiples of 67.8, 72.1, 59.6, 55.8, and 60.7, respectively. The linear range of five antibiotics determined by MSPE-HPLC is 0.004–1 mg/L with the relative standard deviations (RSDs) of 2.1 %–4.9 % and the limits of detection (LODs) of 0.0006–0.0020 mg/L. The method is applied to the determination of the five antibiotics in rice paddy water and fish pond water; the recoveries range from 78.9 to 105.8 %, and the RSDs (n = 5) are 3.6 %–8.7 %.
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ELECTROANALYSIS
·
2024
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IF 2.7
Jiaqi Fu,Jincheng Du,Ting Hou,Zhong Wang,Liyuan Sui,Jinlian Li,Yanli Zhao,Ximing Cui,Dongmei Wu
Electrochemistry with purines as indicators may be a promising new method for antibiotic activity testing. However, the traditional electrochemical detection method (S-LSV) requires a long accumulation time for purines and has low signal intensity. High-temperature treatment of bacterial samples may significantly enhance the signal intensity and speed of detection. However, this process may also impact the structure and metabolism of bacteria. Further research is necessary to determine how electrochemical signals respond to antibiotic antibacterial activity. In this paper, the electrochemical detection method based on heat-treated Escherichia coli ( E. coli , H-LSV) was used to investigate the effects of 11 antibiotics with four different antibacterial mechanisms on the electrochemical behavior of E. coli . The results showed that compared to the S-LSV, the electrochemical signal of E. coli detected by the H-LSV increased by 362%, and showed a strong linear relationship with bacterial counts up to 1.88×10 8 CFU/mL, with a detection limit of 1.15×10 6 CFU/mL. The electrochemical signal consistently correlated with changes in viable E. coli counts following treatment with the four different antibacterial mechanisms. HPLC analysis further confirmed that the changes in purine contents in bacteria after antibiotic treatment were consistent with the trends in electrochemical signals. The evaluation of antibiotic antibacterial ability by H-LSV showed good consistency with results from plate counting and turbidity methods, but was closer to the results of plate counting. The inhibition rates of antibiotics on E. coli detected by H-LSV and S-LSV also showed high consistency, indicating that short-term high-temperature treatment of E. coli did not affect the response of the bacterium to the inhibitory activity of antibiotics.
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ENVIRONMENTAL TECHNOLOGY
·
2025
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IF 2
Tao Zhao,Minghao Xu,Xuerui Yang,Jean-Marc Chovelon,Lei Zhou
High-valent metal species (HVMS) exhibited exceptional oxidative capabilities and selectivity in advanced oxidation processes (AOPs), making them promising oxidants for environmental remediation. However, their inherent instability has hindered kinetic assessments and limited further applications. This study developed a quantitative structure–activity relationship (QSAR) model for predicting the pseudo-first order rate constants (kobs) of high-valent copper species Cu(III) with typical emerging contaminants (ECs). The optimal model was logkobs = 0.002×PSA – 10.1465 × q(C-)X – 4.5896 × ELUMO – 2.0116. R2adj (0.822), Q2LOO (0.784), and Q2ext (0.951) shown the model’s robust and great predictive ability. Polar surface area (PSA), Hirshfeld charge on carbon atoms (q(C-)X), and the energy of the lowest unoccupied molecular orbital (ELUMO) synergistically controlled the reactivity of Cu(III). A larger PSA was conducive to the diffusion of ECs in aquatic environments. Additionally, Density functional theory (DFT) calculations revealed that a smaller q(C-)X could increase the nucleophilic sites of ECs, thereby enhancing the electrophilic reaction of Cu(III). And a lower ELUMO was beneficial for adjusting the energy gap (EGAP) to enhance the reactivity of ECs. This study filled the gap in the prediction of kobs for Cu(III) and provided a reliable reference for the selective treatment of different ECs by HVMS.
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JOURNAL OF CHROMATOGRAPHY A
·
2025
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IF 4
Wuxia Ge,Yumei Chen,Xinru Ding,Wentao Bi,David Da Yong Chen
Magnetic aromatic polyamide (MAPA) composites were synthesized using a green mechanochemical ball milling process and used for magnetic solid-phase extraction (MSPE) and detection of trace level fluoroquinolone antibiotics (FQs) from water samples. The formation of MAPAs was facilitated by deep eutectic systems (DESys) created from magnetic beads and organic monomers during ball milling. A comprehensive study was conducted to investigate the kinetics, thermodynamics, and mechanisms of MAPA adsorption of ciprofloxacin hydrochloride (CIP) and ofloxacin (OFL) from water. The maximum adsorption capacities for CIP and OFL were found to be 151.5 mg/g and 164.1 mg/g, respectively. Additionally, the recyclability and selective adsorption capabilities of MAPAs were evaluated. MAPAs were subsequently used for MSPE of CIP and OFL in water samples. Both UV–Vis spectrometry and HPLC methods can be used for analysis, the MSPE-HPLC method showed superior linearity for CIP (0.06–1500 μg/L) and OFL (1–1200 μg/L), with R² values of 0.9995 and 0.9999, and limit of detection (LOD) as low as 0.006 μg/L and 0.02 μg/L, respectively. Both analytical methods are highly effective and practical for use with real water samples. MAPA used for MSPE offer a promising green approach for detecting antibiotic contamination in aquatic ecosystems.
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SEPARATION AND PURIFICATION TECHNOLOGY
·
2024
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IF 8.1
Meiling Liu,Liping Wang,Qilong Fan,Ningning Xiao,Zhiwen Chen,Yingying Dong,Chuanliang Zhao,Yongxia Sun,Xing Xu,Wendong Wang
Nitrogen (N)-doping has been reported effective to reinforce catalysis in advanced oxidation processes (AOPs) due to the formation of N-related active sites. Although several documents have reported that transition metal-nitrogen (metal-N x ) sites could work as reactive centers, the catalytic mechanism was hardly elucidated. In this study, N-doped cobalt oxide (N-CoO x ) was initiatively prepared via calcination in ammonia atmosphere to construct cobalt-nitrogen (Co-N x ) sites. The emergence of Co-N x sites effectively improved peroxymonosulfate (PMS) activation efficiency (above 5.8 times), leading to higher pollutant decomposition rate (95.8 % at 30 min) and kinetics constant (above 4.1 times). N introduction changed main facets of material and elevated adsorption energy (E ads ) (from −1.81 eV to −3.71 eV) between catalyst and PMS. Co atoms at Co-N x sites could donate larger quantity of electrons (from 1.088 e to 1.583 e) to PMS, therefore, contributed to stretching and breaking O–O bonds of PMS molecules to form reactive species. As a result, both radical and electron transfer pathway (ETP) were enhanced in the oxidation processes. Ultimately, the catalytic membrane coated with N-CoO x maintained 100 % treatment towards continuous antibiotic wastewater at environmentally relevant concentration (μg/L), realizing purification as well as separation of catalyst. This work systematically elaborates the superiority of Co-N x sites and unravels the underlying mechanism to inspire further study to metal-N x tailored catalysis.
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SPECTROCHIMICA ACTA PART A-MOLECULAR AND BIOMOLECULAR SPECTROSCOPY
·
2024
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IF 4.3
Yuxin He,Hanting Wang,Yuting Yan,Xinhui Jiang,Hecun Zou,Zhengwei Zhang
Gefitinib, a highly significant antitumor drug, is now commonly employed in clinical settings as a first-line treatment for patients with advanced or metastatic non-small cell lung cancer, colon cancer, and breast cancer. Herein, a convenient, rapid, and accurate fluorescence method based on nitrogen-doped carbon dots (NCDs) was designed for ultrasensitive detection of gefitinib. The NCDs were easily synthesized through one-pot hydrothermal process using p -phenylenediamine and D-glutamic acid as the precursors. The sensing strategy relied on the fluorescence of NCDs at 345 nm, which was selectively reduced by gefitinib based on the inner filter effect (IFE). With a broad linear range of 0.025–30 μg/mL and a low limit of detection of 5.5 ng/mL, the probe was successfully applied to the detection of gefitinib in human serum samples, demonstrating strong practicality, affordability, and high accuracy. The proposed sensor is simple in design, fast in detection and cost-effective, and exhibits promising application in drug real-time analysis.
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ANALYTICAL BIOCHEMISTRY
·
2024
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IF 2.6
Keyang Lai,Jun Xu,Kai Luo,Min Xie,Yuan Chen,Fan Li,Yaomin Zhou,Lihui Gong,Yonghua Xiong,Weihua Lai
Chloramphenicol (CAP) is a once widely used antibiotic, which is able to cause great harm to human health, is banned in some countries or organizations such as China, USA and the European Union for animal breeding. Because CAP in pig hair degraded slower and had amount of residues, pig hair could be used as the target to detect CAP residues. In this study, a competitive lateral flow immunoassay (LFIA), whose label was aggregation induced emission fluorescent nanobeads (AIEFN), was firstly developed for the detection of CAP in pig hair samples. It exhibited a low limit of detection (0.001 μg/kg) and a broad linear range (0.0025–0.32 μg/kg). The recovery rate and coefficient variation with spiked pig hair samples were 88.50%–106.17 % and 1.01%–7.37 %, which indicated good accuracy of this assay. The result of AIEFN-LFIA for the detection of CAP in pig hair was consistent with that of liquid chromatography-mass spectrometry. This assay was rapid with the total detection duration of about 20 min. AIEFN-LFIA was able to be used for rapid, sensitive, accurate and convenient detection of CAP residues in pig hair samples.
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ENVIRONMENTAL POLLUTION
·
2024
·
IF 7.6
Yanzhuo Zhang,Rui He,Yutai Sun,Jing Zhao,Xiaozhuan Zhang,Jiqin Wang,Alexandr V. Bildyukevich
Microplastics (MPs) in sludge can affect the ability of biochar-activated peroxymonosulfate (PMS) to degrade antibiotics. In this work, biochar was prepared by mixing sludge and polystyrene (PS) through hydrothermal carbonization (HTC) and high-temperature pyrolysis processes . The resulting biochar was used to activate PMS to degrade ofloxacin (OFX), levofloxacin (LEV), and pefloxacin (PFX). The addition of PS significantly enhanced the ability of biochar/PMS to degrade antibiotics and the levels of environmentally persistent free radicals (EPFRs, 4.59 × 10 20 spin/g) due to the decomposition of PS. The addition of PS resulted in a slight decrease in the specific surface area of biochar (2–3 m 2 /g on average), but a significant increase in the concentration of EPFRs increased the removal efficiency. The activation of PMS by biochar is dominated by free radicals, accounting for about 70%, in which SO 4 •- and •OH contribute the most and O 2 •- the least. However, 1 O 2 contributes 15–20% to the degradation of antibiotics in non-free radical processes. Overall, the process of biochar/PMS degradation of antibiotics is mainly dominated by free radicals, and the effect of non-free radicals is not obvious. Both hydrochar and pyrocarbon samples showed good hydrophilicity, and this property should improve the ability of active sites on biochar to degrade antibiotics. In the HTC process, PS can decompose during hydrochar preparation, with a maximum reduction value of 40.09%. The three-dimension excitation emission matrix fluorescence spectroscopy (3D-EEM) and total organic carbon (TOC) results show that the protein content in sludge plays a major role in reducing PS, with little effect of polysaccharide and SiO 2 . There are six to seven degradation intermediates of quinolone antibiotics, which are eventually degraded into CO 2 , H 2 O, and inorganic substances. The regeneration experiment showed good reusability of hydrochar and pyrocarbon, further demonstrating the suitability of biochar for the degradation of antibiotics.
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Marine Life Science & Technology
·
2025
·
IF 5.3
Liu Chang,Li Guoqiang,Chen Yuan,Lin Hong,Cao Limin,Wang Kaiqiang,Wang Xiudan,Flajnik Martin F.,Sui Jianxin
In this study, we investigated the molecular recognition mechanisms of shark-derived single-domain antibodies (ssdAbs) targeting fluoroquinolones using an integrated approach that combines in silico homologous modeling, molecular dynamics simulations, molecular docking, and alanine scanning mutagenesis. Three ssdAbs—2E6, 1N9, and 1O17—specific to enrofloxacin, norfloxacin, and ofloxacin, respectively, were selected based on previous work. Through AlphaFold2 and GalaxyWEB, the protein structures of these ssdAbs were predicted and optimized, followed by molecular dynamics simulations to emulate realistic protein behavior in a solvent environment. Molecular docking, alanine scanning mutagenesis, and subsequent verifications identified 30N and 93W of 2E6; 30N, 89R, 98Y, and 99D of 1N9; 100W and 101R of 1O17, all located within the complementarity determining region 3 loop, as critical for antigen binding. These residues primarily interact with their targets through hydrogen bonds, salt bridges, π–π stackings, and cation–π interactions. This study revealed, for the first time, the binding mechanism of ssdAbs to fluoroquinolones from a theoretical perspective, emphasizing the importance of aromatic and polar residues in recognizing characteristic epitopes, such as the carboxyl group at the C3 position and the 1-piperazinyl group at the C7 position. Our findings provide valuable insights for the rational design and enhancement of ssdAbs for detecting small molecule hazards in aquaculture.
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COLLOIDS AND SURFACES A-PHYSICOCHEMICAL AND ENGINEERING ASPECTS
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2024
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IF 4.9
Guangli Li,Xuan Wan,Qian Zheng,Mengyu Yang,Yonghui Xia,Xiaoman Qi,Tianyu Wang,Zhi Wu
The overuse of gatifloxacin seriously pollutes the environment and cause potential harm to our health. Hence, it is imperative to develop a rapid and sensitive method for gatifloxacin determination. Herein, an efficient electrocatalyst was designed for the voltammetric determination of gatifloxacin based on carboxylated multiwalled carbon nanotubes warped ZnCo 2 O 4 nanoparticles (ZnCo 2 O 4 /MWCNT-COOH). The ZnCo 2 O 4 nanoparticles were synthesized by a green deep eutectic solvent-mediated ion-thermal route, and further composited with MWCNTs-COOH. The ZnCo 2 O 4 / MWCNT-COOH combined the catalytic activity of ZnCo 2 O 4 with the high electrical conductivity of MWCNT-COOH, aiming to improve the electrochemical sensing performance toward gatifloxacin. The synergistic interactions between ZnCo 2 O 4 and MWCNT-COOH endowed the ZnCo 2 O 4 /MWCNT-COOH with extraordinary catalytic activity for gatifloxacin oxidation . Consequently, the ZnCo 2 O 4 /MWCNT-COOH displayed a wide linear response range (0.01–10 μM) for detecting gatifloxacin, with a high sensitivity (29.64 μA μM −1 cm −2 ) and low detection limit (2.0 nM). The ZnCo 2 O 4 /MWCNT-COOH showed robust voltammetric responses against potential interfering species, and maintained highly stable responses for at least two weeks. Moreover, the ZnCo 2 O 4 /MWCNT-COOH/GCE was successfully used to detect gatifloxacin in water samples with satisfactory recoveries (97.22 − 104.5 %). Together with its low cost, environment friendly and rapid response, the ZnCo 2 O 4 /MWCNT-COOH shows promising prospects in trace detection of gatifloxacin.
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AQUA-Water Infrastructure Ecosystems and Society
·
2025
·Vol. 74
·期 2
·159-174
·
IF 2.3
Sun Yao,Duan Runbin,Li Yuzhen,Lu Xinyu,Gao Jiangqi,Zhu Bingzi
View large Download slide View large Download slide Close modal The adsorption and desorption kinetics of antibiotics on natural soils in various aqueous solutions are crucial for understanding their occurrence, transport, and bioavailability in the environment. This study investigated the adsorption and desorption kinetics of three fluoroquinolone carboxylic acids (FQCAs), namely ciprofloxacin, ofloxacin, and levofloxacin, on red clay soil using batch experiments conducted with pure water, treated wastewater effluent, lake water, river water, and stormwater runoff. The research identified pH, electrical conductivity (EC), and organic suspended solids (OSS) as primary water quality parameters that negatively impacted the adsorbed and desorbed masses of FQCAs at equilibrium. Higher pH, EC, and OSS significantly reduced the initial adsorption rates and adsorption efficiencies and promoted initial desorption and desorption efficiencies. FQCAs adsorption processes exhibited a rapid phase mainly governed by external mass transfer and a slower phase primarily limited by intra-particle diffusion, both influenced by boundary layer effects. The adsorption removal of FQCA's ranged from 65.82 to 98.33%, but desorption was only 1.35–3.09%. These findings highlight the potential of red clay soil as an effective and environmentally friendly adsorbent for mitigating FQCA pollution. Future research should focus on investigating FQCA degradation after adsorption in soil and their transport dynamics under diverse field conditions. Measured q e and average adsorption rate over the first 20 s showed strong negative correlations with pH (pH > 7), electrical conductivity, and organic suspended solids. The q e of ciprofloxacin, ofloxacin, and levofloxacin was higher in pure water (PW) and lower in treated wastewater and lake water. Both adsorption and desorption exhibited a fast phase and a slower phase. High adsorption capacities and low desorption were observed. Lower desorption was observed in PW.
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JOURNAL OF CONTAMINANT HYDROLOGY
·
2024
·
IF 3.5
Jiale Xu,Yuting Zhang,Shaoxin Zi,Xuanqi Zhang,Zhengtong Qian,Jin Liu
Tire wear particles (TWPs), as a prevalent form of microplastic pollution in aquatic environments, have been shown to adsorb antibiotics, potentially exacerbating their toxic effects. This study provides a comprehensive analysis of the adsorption of ofloxacin (OFL), ciprofloxacin (CIP), sulfadiazine (SDZ), and tetracycline (TC) on TWPs that have undergone various aging processes, including cyclic freeze-thaw and ozone aging. We observed a significant increase in the specific surface area (SBET) of TWPs after aging, from an initial 2.81 ± 0.29 to 6.63 ± 0.16 m 2 /g for ozone-aged TWPs. This enhancement in surface area and pore volume led to a respective 1.36-fold and 28-fold increase in adsorption capacity for OFL and CIP, highlighting the substantial impact of aging on TWPs' adsorptive properties. Conversely, the adsorption of SDZ and TC was reduced post-aging, suggesting a complex interaction between antibiotic physicochemical properties and TWPs' surface characteristics. The pseudo-second-order model, indicating chemisorption interactions, effectively described the adsorption kinetics, with the Freundlich isotherm model capturing the adsorption behavior more accurately than the Langmuir model. Our findings underscore the critical role of hydrophobic and electrostatic interactions in the adsorption process, particularly for SDZ and TC. This study's results offer crucial insights into the environmental implications of TWPs, emphasizing the need for further research on their role in the transport and fate of antibiotics in aquatic ecosystems.
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