CHEMOSPHERE
·
2022
·
IF 8.943
Chao Ren,Hongtao Wang,Junfeng Ji,Wei Li
Calcination is an effective way to improve the F − adsorption capacity of layered double hydroxide (LDH) materials, however, a molecular scale understanding of the enhanced defluoridation capability of calcined LDHs (CLDH) is lacking. This study investigated the mechanisms of F − adsorption by CLDH using 19 F solid-state NMR, X-ray photoelectron spectroscopy (XPS), and high-resolution TEM . Under calcination process, LDH underwent three periods: surface dehydration below 200 °C, structural dehydroxylation at 200–400 °C, and release of interlayer carbonate groups above 400 °C. Additionally, XPS and XRD characterization showed that CLDH could not recover to the original structural symmetry even after rehydration and reconstitution. The F − affinity was greatly enhanced for the calcined LDH, especially at high pH. At pH 10, the adsorption capacity could reach 22.0 mg F − /g for CLDH (500 °C calcined), about 6 times larger than that of LDH. The XRD analyses revealed that the F-adsorbed CLDH had a poorer crystalline degree as the calcination temperature increased, consistent with the TEM observation of abundant defects and Mg/Al oxides on the CLDH sheets. 19 F solid-state NMR spectra of the CLDH after F − adsorption showed that the formation of surface Al–F is the predominant F − adsorption mode at pH 7, whereas the Mg–F local coordination mode is the pronounced F − adsorption mechanism under alkaline conditions (pH 10). The present study provided a comprehensive understanding of CLDH in F − adsorption and suggested that calcination is a promising treatment for promoting the efficacy of polluted anion scavenging.
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DOI
PubMed
高影响因子
NATURAL PRODUCT RESEARCH
·
2026
·
IF 1.8
Wen-Kai Zhao,Tao-Li Hao,Ya-Zhou Kuang,Tong Sun,Hong-Bing Zhang,Yu-Ming Liu
By combining NMR fingerprint with rapid activity screening of eight crude fractions, eleven guanidine alkaloids were obtained from Buthus martensii Karsch, including one new natural product 7 and one new compound 10. Fraction 6 (IC50 = 141.40 ± 0.21 μg/mL) and Fraction 7 (IC50 = 50.89 ± 1.43 μg/mL) showed radical scavenging activity, and compound 8 exhibited the most potent free radical scavenging activity with an IC50 value of 5.09 ± 0.12 μg/mL. Their anti-ferroptotic capacities were validated across FerroOrange staining, which revealed that compounds 1 and 7 significantly inhibited erastin-induced ferroptosis in H9c2 cardiomyocytes. Through network pharmacology, these alkaloids appeared to exert their effects by modulating core targets related to ferroptosis, such as AKT1, EGFR, SRC, HSP90AA1, CASP3, and ESR1, with the notable impacts on the PI3K-Akt signalling pathway and Lipid and atherosclerosis. Molecular docking analysis confirmed the strong binding affinities and stabilities between guanidine alkaloids and these targets.
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高影响因子
ACS Sustainable Chemistry & Engineering
·
2021
·
IF 8.198
Qi Zhao,Hui Ma,Christian M. Pedersen,Mengyu Dou,Yan Qiao,Xianglin Hou,Yongqin Qi,Yingxiong Wang
Pure shift, a novel nuclear magnetic resonance (NMR) spectroscopy technique is here applied to analyze the hydrogenation/hydrogenolysis products of the biomass-derived platform compounds. The complex and very overlapped 1H NMR signals of the model mixtures from several biomass hydrogenation/hydrogenolysis reactions, such as glucose hydrogenation, sorbitol hydrogenolysis, levulinic acid (LA) formation, tetrahydrofurfuryl alcohol hydrogenolysis, and a real reaction system, were successfully analyzed and assigned by suppressing homonuclear couplings. Thus, we can clearly achieve component analysis and distinguish most signals according to one-dimensional (1D) pure shift obtained by chirp excitation (PSYCHE) spectra. For sophisticated mixtures, e.g., α-d-glucose, sorbitol, and mannitol, or LA, γ-valerolactone, and 2-methyltetrahydrofuran, and finally the real reaction mixture, the 1D total correlation spectroscopy (TOCSY)-PSYCHE approach was used as a supplementary tool to obtain full signals in one component. This allowed us to further resolve the signals where the PSYCHE technique failed to distinguish the signals sufficiently. The results demonstrated that the combined use of 1D PSYCHE and 1D TOCSY-PSYCHE techniques successfully analyzed various catalytic hydrogenation/hydrogenolysis mixtures and enabled us to provide precise signal assignments. Therefore, the pure shift NMR tool (a combination of 1D PSYCHE and 1D TOCSY-PSYCHE) can significantly simplify and successfully be used to assign the NMR spectra of the biomass-derived complex mixture, such as hydrogenation/hydrogenolysis reaction mixtures.
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高影响因子
Analytical Methods
·
2019
·Vol. 11
·期 48
·6176-6183
·
IF 2.378
Fei-Fei Li,Hui-Xiang Liu,Yan-Li Zhang,Shu-Qi Wang
Absorbable vascular sealing medical glue, which belongs to Class III medical devices, is a special new material for preventing the leakage of cerebrospinal fluid. Medical four-arm poly(ethylene glycol)-N-hydroxysuccinimide-glutarate (4-arm-PEG-SG) with a molecular weight of 20 000 is the main component of the absorbable medical glue. According to its quality standard, the quality control of residues 1,3-dicyclohexylurea (DCU), glutaric acid (GA) and triethylamine (TEA) is required. A rapid analytical method of quantitative 1H nuclear magnetic resonance (1H NMR) for the determination of residues DCU, GA and TEA in medical 4-arm-PEG-SG was established in the present study. The peaks at δ 1.56 (4H, m), δ 2.71 (4H, t, J = 6.7 Hz), and δ 2.42 (6H, q, J = 7.2 Hz) were selected for quantifying DCU, GA and TEA, respectively, with deuterated pyridine as the solvent and tetramethylsilane as the internal standard. The 1H NMR assay was validated by several experimental parameters including specificity, linearity, accuracy, precision, robustness, limit of detection (LOD), limit of quantification (LOQ) and stability. The average recoveries obtained were in the range of 99.48–102.02% for all three residues. Compared with the HPLC and GC approaches, the proposed 1H NMR method proved to be a powerful tool for quantification due to its unique advantages of simplicity, rapidity and high robustness, especially not requiring standard compounds for calibration curve preparation.
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高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2016
·
IF 3.169
Yidi Yang,Xi Zhu,Fei Zhang,Wei Li,Ying Wu,Li Ding
Stress testing was carried out under acidic, alkaline, oxidative, thermal and photolytic conditions to evaluate the intrinsic stability of posaconazole injection. A total of four degradation products were detected and the drug was found to be susceptible to oxidative and thermal degradations. Three unknown degradants formed under oxidative stress condition were isolated by preparative HPLC and unambiguously elucidated by LC–TOF/MS, LC–MS/MS, 1 H NMR, 13 C NMR and 2D NMR techniques. Based on the spectrometric and spectroscopic information, these novel degradation products were unequivocally assigned as the N-oxides of posaconazole. Probable mechanisms for the formation of the degradants were proposed. A new and selective HPLC method was developed and validated to separate, detect and quantify all the degradants in posaconazole injection.
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DOI
PubMed
高影响因子
ENVIRONMENTAL SCIENCE AND POLLUTION RESEARCH
·
2019
·Vol. 26
·期 6
·5804-5813
·
IF 2.914
Meng Zhiyuan,Zhu Wentao,Wang Dezhen,Li Ruisheng,Jia Ming,Yan Sen,Yan Jin,Zhou Zhiqiang
The widespread application of bisphenols (BPs) in the industry has made them ubiquitous in the environment, causing potential environmental risks. Its unknown impacts on human being have received more and more attention. In this study, we have assessed the metabolic effects of perinatal exposure to bisphenol A (BPA) and its substitutes (bisphenol S (BPS), bisphenol F (BPF), and bisphenol AF (BPAF)) in female mice adolescent offspring and female mice adulthood offspring. 1 H NMR-based serum metabolomics showed that metabolic profiles were disturbed with BPA and its three substitutes exposure in female mice adolescent offspring and female mice adulthood offspring. In addition, age-related metabolic effects were found based on changes in serum endogenous metabolites and metabolic pathways. Specifically, metabolic pathway analysis showed that major disturbed metabolic pathways in female mice adulthood offspring compare with female mice adolescent offspring also changed significantly. With the increase of age of the female mice offspring, changes in the metabolic pathways became more obvious in the BPA treatment group. Conversely, partially disturbed metabolic pathways were restored in the BPS, BPF, and BPAF treatment groups. In conclusion, perinatal exposure to BPA and its three substitutes significantly interferes with metabolic profiles and metabolic pathways, and this metabolic effects were age-related. These results offer more detailed information about the age-related metabolic effects of perinatal exposure to BPA, BPS, BPF, and BPAF in female mice offspring and provide data for systematic evaluation of the health risk assessment of BPA and its substitutes.
研究领域:
环境毒理学
·
代谢组学
·
发育生物学
·
生殖毒理学
·
分子毒理学
·
环境健康
·
生命早期暴露
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高影响因子
DALTON TRANSACTIONS
·
2024
·Vol. 53
·期 46
·18674-18687
·
IF 3.5
Yuan Gou,Xiaohui Li,Xiaoge Wang,Mengjia Zhang,Jinxiao Zhang,Qiang Li,Xianran Xing,Xiaojun Kuang
Solid-state nuclear magnetic resonance (NMR) spectroscopy serves as a powerful technique for probing local structures. However, the interpretation of NMR signals mainly based on empirical knowledge could lead to imprecise local structural determinations. To address this, density functional theory (DFT)-based theoretical NMR calculations, aided by experimental three-dimensional continuous rotation electronic diffraction (3D cRED) technique, were performed for ZnxY1−xBO3−0.5x borate oxide ion conductors. The calculations provided fine local structure identification for the experimental 11B NMR spectra of ZnxY1−xBO3−0.5x, providing rich information on multiple experimental 11B NMR signals towards the complex boron oxide anions associated with bridging oxygen vacancies and the coexistence of the monoclinic (C2/c), hexagonal (P63/m), and trigonal (R32) phases in ZnxY1−xBO3−0.5x. Owing to the advantages of solid-state NMR in identifying closely related phases compared to X-ray/neutron diffraction technique, along with the advanced 3D cRED technique that allows for rapid phase identification and structure determination, we provide a fine local structure identification and a more inclusive insight into the coexistence of multiple phases in borate with the same composition. More importantly, this work provides guidance for phase and property modulation. Phase modulation in ZnxY1−xBO3−0.5x was carried out with thermodynamic and kinetic modulation and eventually realized the tuning of the local structures and the resultant oxide ion conductivity of ZnxY1−xBO3−0.5x. This work provides a theoretical and experimental platform to access the flexible structural assignment of boron oxide anions and therefore offers new guidance and insights into the defect structures and the phase-property modulation of inorganic solid functional materials beyond borate oxide ion conductors.
研究领域:
材料科学
·
固态化学
·
计算化学
·
核磁共振（NMR）
·
能源材料
·
离子导体
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高影响因子
INTERNATIONAL JOURNAL OF BIOLOGICAL MACROMOLECULES
·
2020
·
IF 5.162
Yue Shi,Xiao Wang,Ning Wang,Fei-Fei Li,Yu-Lin You,Shu-Qi Wang
Glioblastoma (GBM) is the most malignant central nervous system tumor, with poor prognosis. Temozolomide (TMZ) has been used as a first–line drug for the treatment of GBM for over a decade, but its treatment benefits are limited by acquired resistance. Polysaccharides from Cibotium barometz (CBPs) are polysaccharides purified from the root of Cibotium barometz (L.) J . Sm., possessing sensitizing activity. The purpose of this study was to investigate the anti–cancer effect of CBP from different processing methods on U87 cells using a 1 H NMR–based metabolic approach, complemented with qRT–PCR and flow cytometry, to identify potential markers and discover the targets to explore the underlying mechanism. Cibotium barometz is usually processed under sand heating in clinical applications. Polysaccharides from both the processed (PCBP) and raw (RCBP) C. barometz were prepared, and the effect on enhancing the sensitivity to TMZ was investigated in vitro. CBP can significantly increase the toxicity of TMZ to the U87 cell line, promote apoptosis, enhance cell cycle changes, and arrest cells in S phase, and RCBP demonstrated better activity. Multivariate statistical analyses, such as principal component analysis (PCA) and orthogonal projection to latent structure with discriminant analysis (OPLS–DA), were used to identify metabolic biomarkers, and 12 metabolites in the cell extract samples were clearly identified as altered after RCBP exposure. NMR–based cell metabolomics provided a holistic method for the identification of CBP's apoptosis–enhancing mechanisms and the exploration of its potential applications in preclinical and clinical studies.
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PubMed
高影响因子
NEW JOURNAL OF CHEMISTRY
·
2016
·Vol. 40
·期 3
·2530-2540
·
IF 3.277
Hongqin Yang,Yanmei Huang,Di Wu,Jin Yan,Jiawei He,Hui Li
Sofosbuvir (SOF), an oral nucleotide inhibitor of the nonstructural protein 5B RNA of the hepatitis C virus (HCV), was approved for treating chronic HCV infection by the Food and Drug Administration in 2013. Understanding drug–protein interactions is a crucial factor in determining the pharmacokinetics and pharmacodynamics of a drug. In this study, the interaction between SOF and human serum albumin (HSA) was investigated using 1H nuclear magnetic resonance (NMR) spectroscopy, the molecular docking method, fluorescence studies, Fourier transform infrared (FT-IR) spectroscopy, and circular dichroism (CD) spectroscopy. The analysis of saturation transfer difference (STD) and WaterLOGSY data indicated that SOF was bound to HSA, and the STD signals showed that the methyl and aromatic protons of the hydrophobic components of SOF have the most intimate contact with protein. The negative free energies (−7.17 kcal mol−1 and −6.18 kcal mol−1) obtained from molecular docking and fluorescence studies clearly suggested the spontaneity of the interaction of the SOF–HSA complex. STD, WaterLOGSY and fluorescence displacement experiments demonstrated that SOF was preferentially bound to site I of HSA, and this finding was supported by the docking results. In addition, synchronous and three-dimensional (3D) fluorescence, FT-IR, and CD spectrocopy provided complementary information on the micro-environmental and conformational changes of HSA with the addition of SOF. The combination of 1H NMR and conventional methods provided useful information to further elucidate the binding mechanisms of antiviral drugs with HSA.
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高影响因子
AAPS PHARMSCITECH
·
2021
·Vol. 22
·期 5
·1-14
·
IF 3.246
Luo Zheng,Liu Chao,Quan Peng,Zhang Yimeng,Fang Liang
Chemical penetration enhancers (CPEs) are commonly added into transdermal patches to impart improved skin permeation of drug. However, significant unexplained variability in drug release kinetics in transdermal patches is possible as a result of the addition of CPEs; investigations into the underlying mechanisms are still limited. In the present study, a diverse set of CPEs was employed to draw broad conclusions. Solubility parameters of CPEs and acrylate pressure-sensitive adhesive were calculated by molecular dynamics simulation and Fedors group contribution method to evaluate drug-adhesive miscibility. CPE-adhesive interaction was characterized by FT-IR study, 13 C NMR spectroscopy, and molecular docking simulation. Results showed that release enhancement ratio ( ER R ) of CPEs for zolmitriptan was rank ordered as isopropyl myristate > azone > Plurol Oleique ® CC497 > Span ® 80 > N -methylpyrrolidone > Transcutol ® P. It was found that solubility parameter difference (Δ δ ) between CPE and adhesive was negatively related with ER R . It was proved that hydrogen bonding between CPE and adhesive would increase drug release rate, but only if the CPE showed good miscibility with adhesive. CPE like isopropyl myristate, which had good miscibility with adhesive, could decrease drug-adhesive interaction leading to the release of drug from adhesive.
研究领域:
药剂学
·
药学化学
·
生物物理学
·
材料科学
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高影响因子
Food Frontiers
·
2026
·Vol. 7
·期 3
·e70274
·
IF 6.3
Shanshan Zhang,Jun Wu,Renjie Niu,Qian Zhou,Mingfu Wang
Stilbenes are bioactive phytochemicals with notable health benefits, yet their extraction is hindered by hydrophobicity and reliance on toxic solvents. This study introduces a green, sustainable approach for stilbene extraction using hydrophilic natural deep eutectic solvents (NADES), with cajaninstilbene acid (CSA) from pigeon pea ( Cajanus cajan ) as the model compound. After screening, the optimal NADES and ultrasound-assisted extraction conditions were identified, achieving a predicted CSA yield of 0.832 mg/g. The method demonstrated excellent reusability and sustainability. Spectroscopic analyses (ATR-FTIR, 1 H NMR, 1 3 C NMR, 2D NOESY), COSMO-RS, and molecular dynamics (MD) simulations revealed that NADES-4 forms a hydrogen-bonded supramolecular structure involving betaine, glycerol, and water. MD simulations further clarified the thermodynamics and synergistic non-covalent interactions driving CSA solubilization. These findings provide mechanistic insights into NADES-based stilbene extraction and support the development of eco-friendly technologies for plant resource utilization.
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高影响因子
JOURNAL OF ANALYTICAL AND APPLIED PYROLYSIS
·
2023
·
IF 6
Feng Wang,Zheng Zhang,Ying Yang,He Liu,Kun Chen,Zongxian Wang,Aijun Guo
The factors leading to olefinic hydrogen signal shielding in the 1 H NMR spectra of thermally cracked vacuum residue (VR) and its heavy fractions were revealed using a series of model compound systems, and the effect of olefinic hydrogen signal shielding on the determination of olefinic hydrogen content was elucidated. There were two main factors leading to the olefinic hydrogen signal shielding in the 1 H NMR spectra of olefins in heavy fractions, i.e. intramolecular and intermolecular. For the olefin itself in heavy fractions, the chemical shift of the olefinic hydrogen closest to the aromatic ring was in the aromatic region rather than the olefinic region due to the π-π conjugation effect between the double bond and the intramolecular aromatic ring. Notably, the response intensity of the olefinic hydrogen signal could be weakened or even disappear due to the suppressive effect of the intermolecular aromatic structures in other polycyclic aromatic hydrocarbons (PAHs), while alkanes and monocyclic aromatics had little effect on the olefinic hydrogen signal response. Although the olefinic hydrogen signal was detected merely at about 5.30 ppm in the 1 H NMR spectra of heavy fractions, these olefinic structures may be predominantly of the R─CH═CH 2 type rather than the R─CH═CH─R′ type. More importantly, the measured olefinic hydrogen content of thermally cracked VR and its heavy fractions may be considerably lower than the actual content, with the measured content being only about 30–40 % of the actual content. This is mainly due to the weakening and disappearance of the olefinic hydrogen signal, coupled with the fact that the integral area of the possible olefinic hydrogen signal in the aromatic region was overlooked when calculating the total integral area of the olefinic hydrogen signal in the 1 H NMR spectrum.
研究领域:
分析化学
·
石油化学
·
有机化学
·
光谱学
·
能源化学
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高影响因子
危险品化学品经营许可证（带存储）