JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2022
·
IF 3.571
Qianhui Ma,Meng Li,Huan Gong,Ying Zhang,Yan Cui
Enantioseparation of seven β-receptor blockers, including carvedilol , metoprolol , atenolol , sotalol , propafenone , bisoprolol and arotinolol was investigated using HPLC coupled with pre-column derivatization in this work. The derivative conditions of the ratio of the analytes and the derivative reagent, (S)-N-(4-nitrophenoxycarbonyl) phenylalanine methoxyethyl ester, the amount of sodium tetraborate, the reaction temperature and reaction time were optimized. The effects of the types of chromatographic columns, the composition and ratio of the mobile phase and mobile phase additives on enantioseparation were also evaluated in HPLC analysis. The seven pairs of enantiomers showed a good baseline separation on an InfinityLab Poreshell 120 EC-C18 column (150 mm × 4.6 mm, 4 µm) using the mobile phase of methanol and 5 mM ammonium bicarbonate at a flow rate of 1.0 mL/min. In addition, a LC-MS/MS method coupled with QuEChERS extraction for the enantioselective quantitation of carvedilol in soil was developed. The method was fully validated in terms of selectivity , linearity, matrix effect, accuracy, precision, limit of detection and limit of quantification. The linear ranges of carvedilol enantiomers were both 0.5–100 ng/mL and the limits of quantification were 0.5 ng/mL. Extraction recoveries were more than 83.0% with the intra-day and inter-day precision less than 6.8%. The matrix effect values were in the range from 84.5% to 91.3%. The proposed method was successfully applied to determine carvedilol enantiomers in soil and their degradation process was investigated. The degradation of carvedilol enantiomers in soil at natural condition conformed to the first-order degradation kinetics (R 2 > 0.9790). The half-lives of carvedilol enantiomers were 17.77 and 16.90 days, respectively and the enantiomer fraction (EF) values of carvedilol enantiomers ranged from 0.488 to 0.523 with time in soil, indicating the degradation behaviors, disposition and biotransformation of carvedilol enantiomers in soil showed no enantioselectivity (P > 0.05).
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Journal of Physical Chemistry C
·
2019
·
IF 4.309
Xiaolei Lu,Shuxian Wang,Shuxin Liu,Peng Du,Zhengmao Ye,Xuefei Geng,Xin Cheng
Ca2SiO4 is a phase-change material, and γ- and β-Ca2SiO4 usually coexist in the sintered product. The overlap of the diffraction data between the two polymorphs makes the relevant phase identification difficult. In this work, the Eu3+ rear-earth fluorescence probe is introduced in the preparation of Ca2SiO4, and the obtained result indicates that the introduction of Eu3+ ions facilitates the increase in the content of β-Ca2SiO4 in the final product. In addition, the differences of the local coordination environments between the two Ca2SiO4 phases obviously influence the crystal-field splittings of Eu3+ ions, especially in the 5D0 → 7F0 nondegenerate and 5D0 → 7F1 magnetic dipole transition regions. On the basis of the excitation from the Eu3+–O2– charge-transfer band, the low-temperature spectral changes are systematically discussed. The transition area ratios of 5D0 → 7F0/5D0 → 7F2 and 5D0 → 7F1/5D0 → 7F2 present a positive and negative correlation with the increase of the excitation wavelength, respectively. The four nonequivalent 5D0 → 7F0 emission peaks with low to high wavelengths are identified as Eu3+ ion-occupied Ca(β-2) (571.8 nm), Ca(β-1) (573.8 nm), Ca(γ-2) (577.6 nm), and Ca(γ-1) (578.9 nm) sites. Besides, the relationship between the phase content of γ-Ca2SiO4 and the spectral change for the 5D0 → 7F0 emissions of the Eu3+ ions is also built. It is fitted by an exponential correlation function and is quite suitable for the prediction of the phase content of γ-Ca2SiO4 based on the measured spectra. The findings in this study manifest the promising application of the Eu3+ fluorescent probe in phase identification and enrich the analysis method in inorganic phase-change materials.
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JOURNAL OF ANTIBIOTICS
·
2021
·Vol. 74
·期 9
·574-579
·
IF 2.649
Ge Ying,Kang Peng-Wei,Li Jia-Qi,Gao Han,Zhai Le,Sun Le-Yun,Chen Cheng,Yang Ke-Wu
The superbug infection caused by metallo-β-lactamases (MβLs) carrying drug-resistant bacteria, specifically, New Delhi metallo-β-lactamase (NDM-1) has become an emerging threat. In an effort to develop novel inhibitors of NDM-1, thirteen thiosemicarbazones ( 1a - 1m ) were synthesized and assayed. The obtained molecules specifically inhibited NDM-1, with an IC 50 in the range of 0.88–20.2 µM, and 1a and 1f were found to be the potent inhibitors (IC 50 = 1.79 and 0.88 μM) using cefazolin as substrate. ITC and kinetic assays indicated that 1a irreversibly and non-competitively inhibited NDM-1 in vitro. Importantly, MIC assays revealed that these molecules by themselves can sterilize NDM-producing clinical isolates EC01 and EC08, exhibited 78-312-fold stronger activities than the cefazolin. MIC assays suggest that 1a (16 μg ml −1 ) has synergistic antimicrobial effect with ampicillin, cefazolin and meropenem on E. coli producing NDM-1, resulting in MICs of 4-32-, 4-32-, and 4-8-fold decrease, respectively. These studies indicate that the thiosemicarbazide is a valuable scaffold for the development of inhibitors of NDM-1 and NDM-1 carrying drug-resistant bacteria.
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Journal of Saudi Chemical Society
·
2023
·
IF 5.6
Zhong-Lin Zang,Qi Wang,Zhi-Chao Dong,Sheng-Yao Huang,Hao-Zeng Wu,Cheng-He Zhou,Gui-Xin Cai
α,β -Unsaturated ketone is one of the important building blocks of the plenty of alkaloids, spices and pharmaceutical agents. Herein, we describe a peroxide-free electrochemical strategy to realize site-selective allylic C − H oxidation for the synthesis of α,β -unsaturated ketones. This electrochemically driven oxidation exhibits a broad substrate scope. Mechanistic investigations of this reaction uncovered HOAc and H 2 O as the oxygen source to achieve peroxide-free electrochemical allylic C − H oxidation.
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ORGANIC & BIOMOLECULAR CHEMISTRY
·
2016
·Vol. 14
·期 22
·5136-5140
·
IF 3.559
Dingyi Wang,Rongxing Zhang,Wei Ning,Zhaohua Yan,Sen Lin
An unprecedented method for the synthesis of β-alkoxy sulfides via a NaI/HBr-mediated three-component oxysulfenylation reaction of alkenes with arylsulfinic acids and alcohols is reported. Furthermore, I2-promoted oxysulfenylation of alkenes using sodium arylsulfinates instead of arylsulfinic acids to synthesise various β-alkoxy sulfides is also described.
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INTERNATIONAL JOURNAL OF ENERGY RESEARCH
·
2019
·Vol. 43
·期 6
·2162-2171
·
IF 3.343
Wei Li,Shu-ao He,Xiao Wang,Qiong Ma,Chen-hui Zhao
Summary β-iron oxide hydroxide (β-FeOOH) had been proven to be an effective co-catalyst during H 2 evolution reaction (HER) process. In this research, a BiOCl/β-FeOOH heterojunction was successfully synthesized by a solid-state doping method. Then, the structure, composition, and photo-electrochemical properties of the prepared photocatalysts were studied. For the superior HER photocatalytic activity of ultrasmall β-FeOOH nanoparticles (NPs) and the formation of the BiOCl/β-FeOOH heterojunction, this heterojunction photocatalyst exhibited very superior photocatalytic performance in the HER process. Especially, when the amount of incorporated β-FeOOH NPs was appropriate, the BFOH-2 possessed the highest photocatalytic activity in HER process, and the HER rate was about 16.64 mmol·g −1 ·h −1 during illuminated time of 6 hours under visible light. When appropriate, ultrasmall β-FeOOH NPs were implanted into the structure of BiOCl, the BiOCl/β-FeOOH heterojunction interfaces would form for the existence of interfacial interactions. Therefore, this BiOCl/β-FeOOH heterojunction exhibited superior visible-light response, fast photo-carrier migration, and high-efficient separation of photo-carriers, so that the BFOH-2 heterojunction possessed high-efficient hydrogen evolution reaction (HER) photocatalytic activity.
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ACS Sustainable Chemistry & Engineering
·
2023
·
IF 8.4
Zhenlong Song,Yuzhen Hu,Song Li,Jianguo Liu,Xinghua Zhang,Longlong Ma,Lungang Chen,Qi Zhang
Valorizing lignin into valuable chemicals requires the selective breaking of a large number of C–O bonds found in the β–O–4 structure. In this study, we present a one-pot strategy that utilizes two NiO/TiO2 catalysts for the photocatalytic depolymerization of β–O–4 alcohols. The S-1.6%NiO/TiO2 catalyst is used for the dehydrogenation of β–O–4 alcohols at 450 nm. Then, the L-0.8%NiO/TiO2 catalyst is employed for the hydrogenolysis of β–O–4 ketones at 365 nm. Remarkably, the dehydrogenation–hydrogenolysis tandem reaction can be conducted in one pot, which affords high yields of ketones and phenols (up to 89%) from β–O–4 alcohols. Additionally, the L-0.8%NiO/TiO2 catalyst prepared in this article is the smallest NiO/TiO2 photocatalyst reported to date, and the size of NiO in the S-1.6%NiO/TiO2 catalyst is even small enough to enter the lattice of TiO2. We successfully regulated the reaction selectivity by controlling the loading method and the amount of NiO. Our work offers a promising solution for efficiently cleaving target bonds in lignin and provides insights into the design of efficient photocatalysts.
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LANGMUIR
·
2018
·
IF 3.789
Fei Fang,Xiao-Jun Huang,Yi-Zong Guo,Xiao Hong,Hui-Min Wu,Rong Liu,Da-Jing Chen
Cyclodextrins (CDs) are a family of cyclic oligosaccharides, whose unique hydrophilic outer surface and lipophilic central cavity facilitate the formation of inclusion complexes with various biomolecules, such as cholesterol and phospholipids, via multi-interactions. Low-density lipoprotein (LDL) is the main carrier of cholesterol in bloodstream and is associated with the progression of atherosclerosis. The surface of LDL is composed of a shell of phospholipids monolayer containing most of the free unesterified cholesterol as well as the single copy of apolipoprotein B-100. To date, various LDL adsorbents have been fabricated to interact with the biomolecules on LDL surface. Owing to its elegant structure, CD is considered to be a promising choice for preparation of more economical and effective LDL-adsorbing materials. Therefore, in this study, interaction between β-CD and LDL in solution was investigated by dynamic light scattering, circular dichroism, and ultraviolet spectroscopy. Further, a supramolecular surface based on β-CD was simply prepared by self-assembled monolayer on gold surface. The effect of hydrogen bond and the cavity of β-CD on the interaction between β-CD and LDL was particularly explored by surface plasmon resonance (SPR) analysis. The SPR results showed that such β-CD-modified surface exhibited good selectivity and could be largely regenerated by sodium dodecyl sulfate wash. This study may extend the understanding of the interaction between LDL and LDL adsorbent or the design and development of more efficient and lower-cost LDL adsorbents in the future.
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CRYSTENGCOMM
·
2020
·Vol. 22
·期 38
·6330-6338
·
IF 3.117
Chunyan Cheng,Yueshan Xu,Gejihu De,Jianxun Wang,Wei Wu,Yuexing Tian,Shasha Wang
Rare-earth doped upconversion nanoparticles (UCNPs) have attracted wide-ranging interest due to their potential applications in bioimaging and biolabeling, where a high emission intensity and small particle size are needed. However, common synthesis processes can be somewhat complex or require additional reactants, and the use of small-size NPs is limited by their weak luminescence intensity. In this work, uniform, monodisperse ∼5 nm β-NaGdF4:20% Yb/2% Er NPs were synthesized via a simple one-pot synthesis method in the high boiling-point solvents 1-octadecene (ODE) and oleic acid (OA) using a single dose of NaF at an ultralow NaF concentration of NaF/RE = 4. The effects of NaF/RE, the reaction temperature, and the reaction time on the size and phase of the particles were investigated. High-quality β-NaGdF4:20% Yb/2% Er@β-NaGdF4:20% Yb/10% Nd core–shell NPs with a size of ∼13 nm, enhanced UC luminescence, long UC lifetimes (τ) for green (τ ≈ 150 μs) and red (τ ≈ 105 μs) emission under 980 and 808 nm excitation, revealed via lifetime imaging, and obvious emission in the near-infrared (NIR) II region were synthesized. The synthesized core–shell NPs may result in a decrease in the overheating effect and allow for a deep penetration depth when further used for bioimaging applications. This work could inspire the synthesis of other high-quality RE-doped UCNPs via adding a single dose of a small amount of NaF and could lay the foundation for the use of Gd-based UCNPs in biomedical applications.
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CARBOHYDRATE POLYMERS
·
2013
·
IF 3.479
Xiao-Zhu Sun,Gareth R. Williams,Xiao-Xiao Hou,Li-Min Zhu
Polyvinyl alcohol (PVA) nanofibers loaded with curcumin or its β-cyclodextrin (CD) inclusion complex were successfully prepared using an electrospinning process. The influence of curcumin or CD–curcumin complex content on fiber formation and quality was investigated. X-ray diffraction and differential scanning calorimetry analyses of the fibers, together with electron microscope evidence, demonstrated that curcumin is likely to be present as crystalline aggregates in the fibers, while its CD complex is more evenly distributed. 1 H NMR analysis indicated that the chemical structure of curcumin was preserved during the electrospinning process. Thermogravimetric analysis demonstrated that inclusion into nanofibers enhanced the thermal stability of curcumin. In vitro dissolution tests showed that the drug release profiles of the PVA/curcumin and PVA/complex fibers were different, with release from the latter occurring more rapidly. Release from both fiber types was found to be largely governed by a diffusion-controlled mechanism; two sequential stages for drug release were observed.
研究领域:
生物材料学
·
药剂学
·
纳米医学
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FOOD CHEMISTRY
·
2024
·
IF 8.5
Xiaohan Zheng,Bowen Zou,Ruitao Zhu,Junwei Zhang,Xiaokang Na,Ming Du,Beiwei Zhu,Chao Wu
Structured binary protein networks offer a pathway for designing gel-based foods with less ecological and economic effects. This study investigated the heat-mediated interaction and gelation kinetics of cod-soy mixed proteins at molecular level. Results indicated that denaturation degree of soy proteins was fundamental in determining the protein-protein interactions during heating. Considerable non-natural β-sheet was generated in the heterogeneous structures to initiate their aggregation behavior. Cod actomyosin comprising myosin heavy chains and actin mainly regulated their aggregation below 70 °C. At higher temperatures, the formation of large-sized and intermediary-sized aggregates was dominated by disulfide bond exchange between cod actomyosin and soy A-B aggregates (≤ 85 °C) or dissociated B subunits (> 85 °C). These aggregates were further evidenced as essential components to form gel networks with higher storage modulus (G'). These findings provide fundamental insights for designing gel-based products with desirable nutritional and textural properties based on plant-animal binary proteins.
研究领域:
食品科学
·
分子生物学
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Laser & Photonics Reviews
·
2014
·Vol. 8
·期 4
·575-582
·
IF 9.313
Wu Suli,Liu Ye,Chang Jie,Ning Yanhui,Zhang Shufen
Upconversion emission intensity and morphology are both important features of NaYF 4 :Yb 3+ , Er 3+ microcrystals. In this paper, myristic acid (MA) is selected as a novel stabilizing ligand to synthesize NaYF 4 :Yb 3+ , Er 3+ through a facile hydrothermal method. Upconversion fluorescence spectra indicate that the emission intensity of product prepared with MA as ligand has increased dramatically compared with the sample prepared using commonly used oleic acid (OA) as ligand. Field emission scanning electron microscopy (FE-SEM) results display that the morphology of NaYF 4 :Yb 3+ , Er 3+ obtained using MA as ligand can be tuned from nanodisk, nanorod to nanotube. Especially, nanotube with clear caves can be prepared directly with proper concentration of base (NaOH). And powder X-ray diffraction (XRD) analysis reveals a relationship between the phase transformation process and the amount of NaOH. With increasing the amount of NaOH, the transition process of cubic phase to hexagonal phase is accelerated. The effect of F − and OH − on the fluorescence properties of NaYF 4 :Yb 3+ , Er 3+ are studied systematically. A gradual increase of the amount of NaF results in a regular increase of the emission intensity. On the contrary, the emission intensity decreases with increasing the amount of NaOH. In addition, reasonable explanations of the influence of F − and OH − on emission intensity are given as well.
研究领域:
材料科学
·
光学
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