MICROCHEMICAL JOURNAL
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2025
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IF 5.1
Xi-Meng Li,Bei-Ni Chen,Zheng-Quan Nie,Jian-Mei Yang,Jun-Nan He,Tong Yang,Jun-Hui Zhang,Jin-Xin Yang,Lei Zhang,Yan Zhao,Yue Sun,Jin Zhang
The precise determination of enantiomeric purity for mandelic acid ( D/L -MA), a chiral drug precursor, is crucial for the synthesis efficiency and efficacy of related chiral pharmaceuticals. High-performance liquid chromatography (HPLC) currently serves as a mainstream method for enantiomeric purity analysis, yet it suffers from some limitations, such as complicated sample pretreatment, long analysis cycles, and dependency on specialized equipment and operators. In this study, an electrochemical detection platform based on L -cysteine-stabilized gold nanoprobes was constructed, enabling effective analysis of MA enantiomer ratios. The sensor showed good selectivity for MA over its analogs. It also exhibited favorable enantioselectivity for D/L -MA, with a selectivity coefficient ( K D − MA / L − MA ) of 4.3. The limit of detection (LOD) for D -MA was determined to be 0.023 μM. Furthermore, this method showed good quantitative precision for real enantiomer mixtures at different ratio; the relative error is less than 5.4 % compared to reference measurements by HPLC. Density functional theory (DFT) calculations further reveal that the binding energy difference between L -MA and D -MA with the sensing interface reaches 34.9 kcal/mol (−7.3 kcal/mol vs. −42.2 kcal/mol). This stereospecific interaction regulates interfacial electron transfer kinetics to achieve enantiomeric discrimination. This study provides an electrochemical strategy integrating experimental and theoretical analyses for the purity assessment of chiral drug precursors, demonstrating the application potential in chiral drug synthesis and pharmaceutical quality control.
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COLLOIDS AND SURFACES B-BIOINTERFACES
·
2026
·
IF 5.9
Zhichao Ma,Yiran Wang,Yanxin Qin,Qikun Yin,Ming Wei,Wenbo Lu
The development of a quantitative electrochemical method for H 2 O 2 detection is crucial as it enables the real-time assessment of both bleaching agent residues in food and oxidative stress in cancer cells. The single-atom Co catalyst Co SAs@ZIF-NC was prepared using a bimetallic ZIF-8-67 precursor via a template-confined synthesis strategy. Successful synthesis was confirmed through comprehensive characterization of its structure and morphology using X-ray diffraction, scanning electron microscopy, transmission electron microscopy, X-ray photoelectron spectroscopy, Brunauer-Emmett-Teller method, and X-ray absorption near edge structure. The as-synthesized Co SAs@ZIF-NC was immobilized on the surface of a pencil-lead graphite electrode, enabling the electrochemical detection of H 2 O 2 . The H 2 O 2 sensor showed excellent analytical performance for H 2 O 2 detection, with a linear range of 1–2000 μM, a detection limit of 0.21 μM, and a sensitivity of 2395.54 μA·mM -1 ·cm -2 (S/N=3), alongside reliable selectivity, stability, and reproducibility. It was successfully applied to determine H 2 O 2 residues in food and monitor extracellular H 2 O 2 levels in A549 cells. Therefore, this paper proposes a novel material design strategy for single-atom catalysts for electrochemical H 2 O 2 sensing.
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高影响因子
ELECTROANALYSIS
·
2026
·Vol. 38
·期 7
·e70190
·
IF 2.6
Hao Liang,Xuening Jin,Hebing Pei,Zunli Mo
The enantioselective recognition of biomolecules such as amino acids has significant value in medicine, life sciences, agriculture, and other fields. In this study, a novel electrochemical chiral sensor, CS@Cu-β-CD/GCE, was successfully prepared by self-assembling Cu 2+ modified β-cyclodextrin (β-CD) with chitosan (CS) and coating it onto a glassy carbon electrode (GCE). This method effectively addresses the agglomeration issues associated with CS while significantly enhancing the conductive properties of the material and increasing the number of chiral recognition sites. Experimental testing and structural analysis revealed that differentiated hydrogen bonding provides the driving force for molecular binding, while the confinement of the Cu-β-CD cavity and steric hindrance enable structure selection. At optimized testing conditions (30 s incubation, 25°C, pH = 6.0, 5.0 mM), it exhibited the peak current ratio (I D /I L ) of up to 2.25 for phenylalanine (Phe) isomers, outperforming most previously reported electrochemical sensors. Meanwhile, the CS@Cu-β-CD/GCE exhibits excellent stability (98.6% signal retention after 16 days of storage at 5°C), high enantiomeric selectivity for Phe, and good resistance to interference, can be developed for distinguishing racemic phenylalanine. This strategy provides a simple and efficient approach for electrochemical chiral identification of Phe enantiomers and holds wide-ranging application prospects in chiral sensing and drug analysis.
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CHEMICAL ENGINEERING JOURNAL
·
2026
·
IF 12.5
Pengyu Hu,Longwen Lei,Chenglong Fu,Yi Wang,Haiming Li,Xing Wang,Zhiwei Wang,Lan Yao,Yanzhu Guo
Lignin-based CDs with fluorescence and oxidase-like activity were designed firstly • Synergistic engineering of rich graphitic N and large sp 2 domains narrows bandgap • Relationship of structure and visible light-driven oxidase-like activity was revealed • A ratiometric colorimetric/fluorescent system for nitrite detection was constructed Renewable lignin-derived carbon dots with oxidase activity are potential sustainable alternatives for natural enzymes, but their weak visible-light absorption fundamentally inhibits triggering their oxidase-like activity. Herein, we successfully engineered N-doped lignin carbon dots (LCD MA ) with superior visible-light harvesting capacity via enlarging their conjugated sp 2 domain size and graphitic N content. Owing to the synergistic effect of these structures, the bandgap of LCD MA was narrowed to 3.241 eV, which efficiently extended its visible absorption range to 500 nm, and red-shifted its fluorescent light to green region. The superior visible absorption endowed LCD MA with outstanding oxidase-like activity via boosting the generation of photogenerated electrons, which drove the reduction of O 2 to • O 2 − . The LCD MA exhibited a rapid catalytic rate (V max = 21.64 × 10 −5 mM s −1 ) and strong affinity (K m = 0.70 mM) for 3,3′,5,5′-tetramethylbenzidine. Owing to the catalytic activity and green fluorescence of LCD MA , we constructed a ratio-metric colorimetric and fluorescence dual-mode solution system for nitrite detection in the linear range of 2–250 μM, whose detection limits were as low as 0.85 μM and 1.60 μM, respectively. Furthermore, we engineered an all-in-one portable sensing platform by encapsulating LCD MA and TMB into hydrogel for visual and quantitative detection of nitrite through smartphone with a detection limit of 8.95 μM. This study not only provided an effective strategy for rationally engineering sustainable carbon dots with oxidase-like activity from renewable biomass, but also delivered a practical and effective analytical tool for food safety monitoring. Download: Download high-res image (370KB) Download: Download full-size image
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SEPARATION AND PURIFICATION TECHNOLOGY
·
2025
·
IF 9
Jianjun Wang,Xueqing Liu,Dongning Li,Jiao Liu,Zhichun Shi,Yu Zang,Toshiki Aoki
The uranium extraction is of great importance for the development of the nuclear energy industry. In this study, a series of porous organic polymers were explored via crosslinking the amino acids and tetraphenyl-porphyrin by Friedel-Crafts alkylation reaction (HCP-TPP-AAs). The obtained polymer was loaded on carbon cloth to prepare the polymer electrode and was applied for the electrosorption of uranyl ions in an aqueous solution. The experimental parameters such as external voltage, pH value, adsorption time, and initial uranium concentration have also been systematically investigated to evaluate their influences on the adsorption performance. Owing to the abundant active sites such as the TPP unit, amino and carboxyl groups in the polymer skeleton, the HCP-TPP-AAs electrodes displayed an excellent uranium adsorption capacity and selectivity. Under the driving force of the electrode, the maximum U(VI) adsorption capacity reached up to 754.5 mg/g, which was six times higher than that of the static adsorption. Furthermore, the uranium removal efficiency by HCP-TPP-AAs electrodes was 81 % in the coexistence of competing metal ions and it can still maintain 85 % of its original adsorption capacity after seven cycles. The XPS analysis and DFT calculations indicate that the TPP unit, COOH and NH 2 groups in the polymer network display a strong inner sphere complexation with the uranyl ion. This strategy overcomes the long-standing drawbacks of conventional uranium extraction (e.g., low adsorption capacity, poor selectivity, and slow kinetics), offering innovative materials and technical solutions for the efficient capture of U(VI) from seawater and wastewater.
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RSC Advances
·
2022
·Vol. 12
·期 16
·9637-9644
·
IF 4.036
Jian Zhang,Lingling Liang,Yanqing Miao,Yang Yang,Xin Bao,Chunye Liu
A hydroxypropyl-β-cyclodextrin (HP-β-CD) imprinted coating based on polyhedral oligomeric silsesquioxane (POSS) for open tubular electrochromatography was prepared. The mixture of methacryl-POSS (MA0735), HP-β-CD (template), methacrylic acid (MAA, monomer), N,N′-methylenebisacrylamide (MBA, crosslinker) and toluene-dimethyl sulfoxide (porogen) was used to synthesize the chiral selective coating. The influence of synthesis parameters on the imprinting effect and separation performance, including the amount of HP-β-CD, POSS, and MAA, was investigated systemically. The optimum polymerization was prepared by mixing HP-β-CD, MA0735, MAA, and MBA with the molar ratio of 1 : 1.87 : 1.60 : 1.60. Five racemates were separated by the modified capillary columns using aqueous buffer. Column efficiency on the POSS-based MIPs coating column was greater than 22 000 plates/m. MIPs-POSS hybrid coating capillaries had improved resolution (3.36 times) and the greatest resolution was up to 6.15 within 10 min.
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SEPARATION AND PURIFICATION TECHNOLOGY
·
2022
·
IF 9.136
Huixian Liu,Xin Qiu,Jian Ke,Wenbei Chen,Xiaoping Bai,Yibing Ji,Jianqiu Chen
Enantiomeric separation based on membrane techniques has the advantages of energy efficiency, sustainable operation, and no additives, but there are no commercially available chiral membranes. The main reasons restricting the development of chiral membranes are separation specificity, poor mechanical properties, and membrane fouling. Therefore, we developed a novel chiral membrane with a stainless steel mat mesh as the base and β-cyclodextrin blended in cellulose acetate as the functional layer. The organic layer was loaded on the inorganic base by nonsolvent-induced phase inversion, and the two post treatments were optimized. The results indicate that the optimal percent enantiomeric excess (ee%) was 96.98 ± 5.22 % for d , l -tryptophan, 46.38 ± 1.65 % for d , l -phenylalanine, 11.50 ± 2.52 % for (RS) -propranolol, and 5.16 ± 0.88 % for (RS) -warfarin. The mechanical properties of stainless steel chiral composite membranes are better than those of other chiral membranes, and the Young's modulus values reached 3234 MPa. In addition, ultrasonic cleaning and electrolytic cleaning were successfully tested to solve the membrane fouling problem, and a comparative study indicated that electrolytic cleaning has low energy consumption and is a fast and effective cleaning method that can achieve flux recovery. These results indicate that conductive chiral membranes can achieve long-term separation of chiral compounds and have great potential for industrial applications.
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OPTICS AND LASER TECHNOLOGY
·
2022
·
IF 4.939
Yifeng Shi,Gerile Naren,Ying Zhang,Jiakang Han,Aorigele Bohnuud
Amino acid rare-earth complexes are widely used due to their unique physical and chemical properties. In this study, three kinds of neodymium (III) complexes with octanoyl-aminocarboxylate ligands (abbr. Nd(oct-ala) 3 , Nd(oct-phe) 3 , Nd(oct-ser) 3 ) were prepared by a chemical reaction method in methanol as the solvent. The chemical formulas and coordination modes of the neodymium complexes were determined by elemental analysis, 1 H NMR and FT-IR. Additional analyses by X-ray diffraction (XRD) and scanning electron microscopy (SEM) show that the neodymium complexes have lamellar irregular shapes and long-range disordered amorphous structures. The thermal performance of the complexes was determined by differential scanning calorimetry (DSC) and thermal gravimetry-differential thermal analysis (TG-DTA). Nd(oct-phe) 3 and Nd(oct-ser) 3 appeared glassy when heated. The solubility of the complexes in various organic reagents was also measured. The optical properties of the complexes were examined using UV–Vis absorption, polarizing microscopy observations, fluorescence spectra, quantum yield, and fluorescence lifetime. The luminescence properties of the complexes as a function of temperature were further observed by analysis of temperature-dependent emission spectra. The polarizing microscopy observations show that the three neodymium complexes exhibited the characteristic properties of thermotropic liquid crystals. UV–Vis, fluorescence spectroscopy, and quantum yield results show that they have excellent light absorption and luminescence properties. Temperature-dependent emission spectra show that the complexes have good luminescence properties in the temperature range of 25–160 °C. The powdered complexes and the complexed solutions in methanol were irradiated with 380 nm UV light, resulting in blue-violet light emission. A warm white-light device was constructed to further verify the luminescence of the complexes after combining with three kinds of rare-earth complexes (Nd(oct-phe) 3 , Eu(oct-phe) 3 , and Tb(oct-phe) 3 . The color rendering index (CRI) and color temperature (CCT) were measured. In addition, the density functional theory (DFT) was used to determine the geometric structures ( Fig S1 ), and obtain 1 H NMR, FT-IR spectra of the neodymium complexes ( Fig S2, S3 ). Their structures were further examined by comparing the calculated with the experimental spectra. The results show that the ligands coordinate to the central Nd 3+ through the bidentate chelation mode.
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SEPARATION AND PURIFICATION TECHNOLOGY
·
2021
·
IF 7.312
Huan Luo,Xiaoping Bai,Huixian Liu,Xin Qiu,Jianqiu Chen,Yibing Ji
Membrane-based chiral separation has attracted widespread research attention. However, traditional chiral membranes remain an unbridgeable trade-off between permeability and selectivity. Chiral covalent organic frameworks (CCOFs) with inherently high porosity and intrinsic chirality are highly promising solutions. Herein we report novel CCOF membranes for enantioseparation of chiral drugs. A β-cyclodextrin covalent organic framework (β-CD COF) was used as the chiral selector to fabricate two types of β-CD COF membranes by physically and chemically modifying cellulose acetate substrates, including a β-CD COF mixed matrix membrane (β-CD COF MMM) and a β-CD COF thin film nanocomposite membrane (β-CD COF TFN). In particular, the β-CD COF TFN was the first reported interfacial polymerized COF membrane for enantioseparation and performed more preferentially than β-CD COF MMM. The optimal enantioselectivities of d , l -tryptophan (e.e% = 100%), ( RS )-mandelic acid (e.e% = 58.1%), d , l -phenylalanine (e.e% = 36.3%), and ( RS )-propranolol (e.e% = 18.0%) and comparable solute flux (Flux = 1.9–5.4 nmol·cm −2 ·h −1 ) were achieved using β-CD COF TFN. Benefiting from the remarkable chemical stability of β-CD COF, such membranes also had excellent thermal stability, acid resistance, and long-term storage stability. Moreover, the chiral recognition mechanism was investigated using molecular docking simulations. Fabricated membranes with high enantioseparation performance and stability provide a new perspective on establishing chiral membranes and show potential for industrial application.
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BIOSENSORS & BIOELECTRONICS
·
2020
·
IF 10.257
Xixia Liu,Yaoyao Hou,Sirui Chen,Juewen Liu
Dopamine is one of the most important neurotransmitters . A high-quality DNA aptamer for dopamine was reported in 2018. However, fundamental understanding of its binding and folding is lacking, which is critical for related biosensor design. Herein, we performed careful assays using a label-free technique called isothermal titration calorimetry (ITC) to study its secondary structure . We divided this aptamer into four regions and individually examined each of them. We confirmed two stems, but the third stem is believed to be part of a loop. The aptamer was then truncated. The original aptamer had a K d of 2.2 ± 0.3 μM at 25 °C. Shortening the structure by one or two base pairs increased the K d to 6.9 and 44.4 μM, respectively. Dopamine binding was promoted by both increasing the Mg 2+ concentration and decreasing the temperature. At 5 °C, a K d of 0.4 μM was achieved. Based on this understanding, we designed two fluorescence resonance energy transfer (FRET) quenching biosensors that differ only by a base pair. The shorter sensor had 3-fold higher sensitivity and a detection limit of 0.9 μM. In 1% fetal bovine serum, the sensor retained a similar limit of detection of 1.14 μM. A two-fluorophore ratiometric FRET sensor was also demonstrated with a low detection limit of 0.12 μM. This work indicated the feasibility of designing folding-based sensors for dopamine, and this design can be extended to other sensing modalities such as electrochemistry and colorimetry .
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高影响因子
MICROCHIMICA ACTA
·
2023
·Vol. 190
·期 7
·1-11
·
IF 5.7
Li Yuchen,Xu Guangfu,Chen Jiaquan,Yu Tao,Miao Pandeng,Du Yingxiang
A novel chiral molecularly imprinted polymer TiO 2 nanoparticle was synthesized in one step for the enantioseparation of phenylalanine in coated capillary electrochromatography. To the author’s knowledge, the chiral molecularly imprinted nanomaterials have still not been reported, to date. Chiral molecularly imprinted TiO 2 nanomaterials (L-PHE@MIP(APTES-TEOS)@TiO 2 ) were used as a chiral stationary phase to separate the phenylalanine enantiomers in coated capillary electrochromatography (CEC). The imprinted coating was prepared from L-phenylalanine (L-PHE) as the template, TiO 2 nanoparticles (NPs) as the support substrate, 3-aminopropyltriethoxysilane (APTES) as the functional monomer, and tetraethyl silicate (TEOS) as the cross-linker. Scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS) were used for the characterization of the L-PHE@MIP(APTES-TEOS)@TiO 2 @capillary. Fourier transform infrared spectra (FT-IR), transmission electron microscopy (TEM), and thermogravimetric analysis (TGA) were employed for the characterization of the L-PHE@MIP(APTES-TEOS)@TiO 2 . The effects of the applied voltage, pH value, buffer concentration, and acetonitrile content were investigated experimentally to determine the optimum conditions for CEC. The best resolution for phenylalanine enantiomers by CEC reached a value of 3.48. In addition, the specific recognition effect of L-PHE@MIP(APTES-TEOS)@TiO 2 on PHE enantiomers was studied by selective experiment. Finally, adsorption kinetic research, adsorption equilibrium isotherm study, and adsorption thermodynamic experiment were carried out to investigate the separation mechanism of PHE enantiomers with the L-PHE@MIP (APTES-TEOS)@TiO 2 @capillary, and the results were consistent with those of CEC experiments. Graphical Abstract
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Journal of Environmental Chemical Engineering
·
2022
·
IF 7.968
Qian Ye,Jin Li,Yinyin Huang,Hanbin Wu,Yilin Li,Bin Yan
Due to their unique properties, the efficient separation of racemic mixtures remains a great challenge. Recently, membrane separation has been demonstrated as a promising chiral separation technique with the advantages of continuous operation, high throughput, and cost effectiveness. In this work, a cyclodextrin-metal-organic framework (CD-MOF) was prepared and then composited with polyvinylidene fluoride (PVDF) polymer by the phase inversion via immersion precipitation method to form a CD-MOF/PVDF composite membrane for chiral amino acid separation for the first time. The composite membranes prepared under different conditions were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) thermogravimetric analysis (TGA)and differential scanning calorimetry (DSC). The effects of preparation conditions including CD-MOF load, polymer concentration, and casting solution temperature on the hydrophilicity, water flux , bovine serum albumin (BSA) rejection and chiral separation performance of the membrane were investigated. It is found that the composite membrane (V-5%−12) prepared with the CD-MOF load of 5%, polymer concentration of 12%, and casting solution of 70 ℃ shows the best performance with the water flux of 466.4 L/m 2 ∙h, BSA rejection rate of 24.3% and stable 100% separation efficiency for phenylalanine (Phe) enantiomers for 4 h. The interaction energies between the CD-MOF and D -Phe and L -Phe were calculated using the Gaussian 09 program package and the chiral separation mechanism of the composite membrane was proposed at the molecular level. Our work demonstrates great development potentials of the CD-MOF/PVDF composite membrane in the chiral separation of drugs.
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