JOURNAL OF CHROMATOGRAPHY A
·
2023
·
IF 4.1
Yuanyuan Fu,Zhentao Li,Changjun Hu,Qiaoyan Li,Zilin Chen
A new kind of covalent organic framework (COF) was first utilized as an stationary phase for open-tubular electrochromatography (OT-CEC) by in situ synthesis immobilized method at room temperature. On the basis of our previous work, 4,4′,4″-(1,3,5-Triazine-2,4,6-triyl)trianiline (TZ) and 2,5-bis(2-propyn-1-yloxy)-1,4-benzenedicarboxaldehyde (BPTA) were employed as building blocks for the synthesis of COF TZ-BPTA. The coated capillary and COF TZ-BPTA were characterized by scanning electron microscopy (SEM). Then, Fourier transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), and X-ray diffraction (XRD) were also applied to characterize COF TZ-BPTA and the modified column. In SEM, it can be seen that COF TZ-BPTA was the spherical shape and the modified capillary was covered with globular particles equably. The COF TZ-BPTA coated column exhibited good separation resolution and efficiency towards two antiepileptic drugs and other kinds of small organic molecules involving alkylbenzene, sulfonamides, polycyclic aromatic hydrocarbon (PAH), parabens, amino acids and herbicides. The maximum column efficiency was over 2.8 × 10 5 plates·m −1 . In addition, the precisions (RSDs) of the retention times for the alkylbenzenes of intra-day runs (n = 3), inter-day runs (n = 3) and column-to-column runs (n = 3) were all less than 1.70% and separation performance was without obvious change within 100 times run. In addition, the real sample was tested on COF TZ-BPTA coated column. Hence, COF TZ-BPTA showed great potential in the separation domain.
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SEPARATION AND PURIFICATION TECHNOLOGY
·
2022
·
IF 9.136
Chunyan Hu,Jianyi Li,Juncheng Ke,Jianjun Liang,Qiuliang Liu,Qiliang Wang,Wentao Huang
Double template magnetic molecularly imprinted polymers (CBZ/OXC-MIPs) with specific recognition for carbamazepine (CBZ) and oxcarbazepine (OXC) were prepared using surface molecular imprinting and magnetic response imprinting techniques. Itaconic acid (IA) was selected as functional monomer by annealing simulation algorithm. The preparation of CBZ/OXC-MIPs was optimized from the ratio of template molecules to functional monomer, the dosages of crosslinker and solvent, and the ratio of CBZ to OXC. Characterization analysis showed that the imprinted polymer was successfully prepared with magnetic properties , and had a porous structure with pore sizes mainly distributed between 1 nm and 2 nm. Adsorption experiments suggested that the adsorption process of CBZ/OXC-MIPs was well fitted with the Freundlich model, and there were high and low affinity adsorption sites in CBZ/OXC-MIPs. The adsorption reached the optimal equilibrium at about 30 min, which conformed to the pseudo-second-order kinetic model. CBZ/OXC-MIPs showed a specific recognition in competitive adsorption, and the adsorption capacity decreased by 3.39 % after 10 cycles of regeneration. Molecular simulation and characterization demonstrated that the selective adsorption mainly depended on van der Waals forces, hydrogen bond, and electrostatic interaction.
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CHEMICAL ENGINEERING JOURNAL
·
2021
·
IF 13.273
Cong Pan,Libin Fu,Fenna Lide,Yaobin Ding,Chengjun Wang,Jia Huang,Shaobin Wang
Reduction of bromate (BrO 3 − ) by various technologies has been extensively investigated, while the fate of oxygen and bromine atoms in BrO 3 − in these processes has been largely ignored. In this study, reduction of BrO 3 − by Fe(II) ions was investigated under various conditions via electron spin resonance (ESR), laser flash photolysis (LFP), probe of phenol and quenching experiments. It was found that reduction of BrO 3 − by Fe(II) ions produced HO•, O 2 • − and reactive bromine species (eg., Br• and Br 2 • − ). HO• and O 2 • − were generated from release of one/two oxygen atoms in BrO 3 − and its reduction intermediates (BrO 2 − and BrO − ) at one time, while Br• and Br 2 • − were generated from activation of hypobromous acid by Fe(II) and reactions of HO• with formed Br − . Due to the formation of these reactive species, the tested ten organic pollutants with diverse structures can be efficiently degraded, which including carbamazepine (CBZ), ibuprofen, phenol, benzoic acid, paracetamol, bisphenol a, 4-chlorophenol, oxcarbazepine, diclofenac and sulfamethoxazole. CBZ degradation intermediates by BrO 3 − /Fe(II) system were specially identified by liquid chromatography (LC)-mass spectrometry (MS), and three pathways of hydroxylation/nitrosylation, ring contraction-amine cleavage and bromination for CBZ degradation were proposed accordingly. This study might shed new fundamental insights to bromate reduction and its implication for transformation of co-existed organic pollutants.
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WATER RESEARCH
·
2019
·
IF 7.913
Qin He,Jian-Jun Liang,Li-Xi Chen,Shu-Li Chen,Huai-Li Zheng,Hong-Xia Liu,Hui-Jie Zhang
Carbamazepine (CBZ) is a typical pharmaceutical residue commonly found in aqueous environments, but its removal through activated carbon or advanced oxidation processes is often disrupted by co-existing organic matter. An imprinting system which consisted of the target pollutant CBZ (template molecule) and 10 different kinds of functional monomers was constructed via molecular simulation to screen for appropriate monomers , thereby addressing CBZ removal disruptions. An annealing method simulation was used to search for stable, low-energy conformations of the template-monomer interaction system to calculate the binding energy of these different monomers with CBZ. The order of binding affinity calculated was: 4-vinylbenzoic acid > itaconic acid > methacrylic acid, which was consistent with the experimental observations. The adsorption capacity of the molecular imprinted polymer (MIP) prepared using 4-vinylbenzoic acid reached 28.40 mg/g, and the imprinting factor reached 2.72. The simulation and measurement of the ultraviolet spectrum of the imprinting system showed that a new interaction system was formed between the template and monomers, and that multiple binding conformations between them took place when specific recognition occurred. Energy calculation and hydrogen bond analysis revealed that the van der Waals force , including the π-π conjugate and electrostatic forces including hydrogen bonding, played an important role during selective adsorption, which was confirmed by infrared spectroscopy analysis.
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WATER RESEARCH
·
2018
·
IF 7.051
Tongcai Liu,Kai Yin,Chengbin Liu,Jinming Luo,John Crittenden,Weiqiu Zhang,Shenglian Luo,Qunying He,Yongxiu Deng,Hui Liu,Danyu Zhang
Oxcarbazepine (OXC) is ubiquitous in the aqueous environment. And due to its ecotoxicological effects and potential risks to human, an effective way to eliminate OXC from aqueous environment has aroused public concerns in recent years. Radical-based reactions have been shown to be an efficient way for OXC destruction, but the reactions of OXC with reactive oxygen species (ROS) and carbonate radical (CO 3 •− ) are still unclear. In this study, we focused the degradation of OXC and ROS, CO 3 •− generation mechanism, and their roles in OXC degradation via UV and UV/H 2 O 2 . The triplet state of oxcarbazepine ( 3 OXC ∗ ) was found to play an important role in OXC degradation via UV. And hydroxyl radicals ( • OH) and singlet oxygen ( 1 O 2 ) were found to be the dominant ROS in OXC degradation. Superoxide radical (O 2 •− ) did not react with OXC directly, but it may react with intermediate byproducts. Generation of CO 3 •− played a positive role on OXC degradation for both UV and UV/H 2 O 2 . In addition to • OH, 3 OXC* also contribute to CO 3 •− production. The second-order rate constants of OXC with • OH and CO 3 •− were 1.7 × 10 10 M −1 s −1 and 8.6 × 10 7 M −1 s −1 , respectively. Potential OXC degradation mechanisms by • OH were proposed and included hydroxylation, α-ketol rearrangement, and benzylic acid rearrangement. Compared with non-selective • OH, the reactions involving CO 3 •− are mainly electron transfer and hydrogen abstraction. And the acute toxicity of OXC was lower after UV/H 2 O 2 and UV/H 2 O 2 /HCO 3 − treatments, which was confirmed by luminescent bacterial assay ( Vibrio fischeri bacterium).
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ENVIRONMENTAL SCIENCE AND POLLUTION RESEARCH
·
2015
·Vol. 23
·期 3
·2848-2855
·
IF 2.828
Bu Lingjun,Zhou Shiqing,Shi Zhou,Deng Lin,Li Guangchao,Yi Qihang,Gao Naiyun
The degradation kinetics and mechanism of the antiepileptic drug oxcarbazepine (OXC) by UV-activated persulfate oxidation were investigated in this study. Results showed that UV/persulfate (UV/PS) process appeared to be more effective in degrading OXC than UV or PS alone. The OXC degradation exhibited a pseudo-first order kinetics pattern and the degradation rate constants ( k
obs ) were affected by initial OXC concentration, PS dosage, initial pH, and humic acid concentration to different degrees. It was found that low initial OXC concentration, high persulfate dosage, and initial pH enhanced the OXC degradation. Additionally, the presence of humic acid in the solution could greatly inhibit the degradation of OXC. Moreover, hydroxyl radical (OH•) and sulfate radical (SO 4
− ••) were identified to be responsible for OXC degradation and SO 4
− • made the predominant contribution in this study. Finally, major intermediate products were identified and a preliminary degradation pathway was proposed. Results demonstrated that UV/PS system is a potential technology to control the water pollution caused by emerging contaminants such as OXC.
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TALANTA
·
2012
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IF 3.794
Shuchao Wu,Wei Xu,Qamar Subhani,Bingcheng Yang,Deying Chen,Yan Zhu,Lanjuan Li
This paper describes the determination of carbamazepine (CBZ) in human plasma using ion chromatography combined with online electrochemical derivatization and fluorescence detection. Separation of CBZ with anion exchange column was demonstrated to be feasible using either basic (10 mM NaOH) or acidic (0.1 M H 3 PO 4 ) reagent with a small amount of acetonitrile (ACN) added as eluent . Electrochemical derivatization of CBZ into a strongly fluorescent product, which could be carried out only under the acidic condition, was investigated via the previously reported electrolytic cell (EC), as well as two modes of acidification . The linear range of CBZ for human plasma was between 10–2000 μg L −1 under the optimized experimental conditions. The limit of detection (LOD, S/N=3) was 1.3 μg L −1 and the relative standard deviation (RSD, n =7) was 2.6%. Better sensitivity and selectivity of the present method were demonstrated in comparison with ion chromatography with ultraviolet detection (IC-UV). The spiked recoveries of CBZ in 2 human plasma samples were 78.5 and 114%, respectively.
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Journal of Environmental Chemical Engineering
·
2025
·
IF 7.2
Jilong Wang,Qi Xiang,Ye Han,Zeyu Ma,Wei Cheng,Jie Sun,Shaobin Wang
To overcome the limitations of traditional Electro-Fenton (EF) in natural waters, such as low conductivity and metal ion leaching, we developed a novel metal-free EF system incorporating solid polymer electrolytes (EF-SPE). Nitrogen-doped carbon cathodes, optimized via calcination (e.g., 800 °C), enabled efficient in-situ H 2 O 2 electro-generation and activation for carbamazepine (CBZ) degradation. This EF-SPE system achieved a CBZ degradation half-life of 10 min (k = 0.052 min −1 ), operated effectively across a broad pH range (3–9), and exhibited low specific energy consumption for mineralization (6.73 kWh·m −3 ). Experimental and computational studies reveal that graphitic N and pyridinic N were the primary active sites for the electro-generation of H 2 O 2 and its activation to •OH, respectively. The system demonstrated universal efficacy for various pharmaceuticals and personal care products in different natural waters, showcasing its potential for sustainable water purification.
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JOURNAL OF SEPARATION SCIENCE
·
2025
·Vol. 48
·期 4
·e70151
·
IF 2.8
Yu-Fei Zhang,Zheng Yu,Zhao Zhao,Le-Qing Xu,Xun-Yi Wu,Chun-Lai Ma
Monotherapy or combination therapy with anti-seizure medications (ASMs) remains the cornerstone of epilepsy treatment. Therapeutic drug monitoring is important for individualized ASM treatment and for optimizing outcomes in patients with epilepsy. Therefore, the simultaneous and accurate quantification of ASMs is necessary and helpful for clinical use. In this study, a new method was developed to simultaneously quantify carbamazepine, lacosamide, lamotrigine, levetiracetam, oxcarbazepine, perampanel, sodium valproate, topiramate, and an active metabolite of oxcarbazepine, 10, 11-dihydro-10-hydroxycarbamazepine, in human plasma by high-performance liquid chromatography-tandem mass spectrometry using the positive/negative ion-switching ionization mode. The method was assessed for accuracy, precision, linearity, recovery, and matrix effects according to the criteria of the U.S. Food and Drug Administration Bioanalytical Method Validation Guidelines for Industry for Bioanalytical Methods. The lower limit of quantification was determined to be 0.001–25 µg/mL for each analyte. The intra- and inter-day precision values had <14.6% coefficients of variation, and the accuracy ranged from 85.3% to 113% at the three levels of quality control. In addition, this method was successfully applied to therapeutic drug monitoring of ASMs in patients with epilepsy. This method allows for simple preparation, accurate quantification, and the determination of different ASMs without requiring analytical method switching, making it particularly suitable for therapeutic drug monitoring in busy clinical and hospital laboratory settings.
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