Structural characterization of heparins from different commercial sources

Seven commercial heparin active pharmaceutical ingredients and one commercial low molecular weight from different manufacturers were characterized with a view profiling their physicochemical properties. All heparins had similar molecular weight properties as determined by polyacrylamide gel electrophoresis (M _N, 10–11 kDa; M _W, 13–14 kDa; polydispersity (PD), 1.3–1.4) and by size exclusion chromatography (M _N, 14–16 kDa; M _W, 21–25 kDa; PD, 1.4–1.6). one-dimensional ¹H- and ¹³C-nuclear magnetic resonance (NMR) evaluation of the heparin samples was performed, and peaks were fully assigned using two-dimensional NMR. The percentage of glucosamine residues with 3-O-sulfo groups and the percentage of N-sulfo groups and N-acetyl groups ranged from 5.8–7.9%, 78–82%, to 13–14%, respectively. There was substantial variability observed in the disaccharide composition, as determined by high performance liquid chromatography (HPLC)-mass spectral analysis of heparin lyase I–III digested heparins. Heparin oligosaccharide mapping was performed using HPLC following separate treatments with heparin lyase I, II, and III. These maps were useful in qualitatively and quantitatively identifying structural differences between these heparins. The binding affinities of these heparins to antithrombin III and thrombin were evaluated by using a surface plasmon resonance competitive binding assay. This study provides the physicochemical and activity characterization necessary for the appropriate design and synthesis of a generic bioengineered heparin.     

Direct fluorination—Useful tool to enhance commercial properties of polymer articles

Fundamental features and industrial applications of the direct fluorination of polymers are reviewed. Fundamental features of the direct fluorination of a set of polymers, such as polystyrene, polyethyleneterephthalate, poly(2,6-dimethyl-1,4-phenylene oxide), PMMA, LDPE (two types), HDPE (six types), polyvinyltrimethylsilane, poly(4-methyl-pentene-1), polyimide Matrimid 5216^®, polysulfones, polyetheretherketone, polycarbonatesiloxane, polysulphone-polybuthadiene block-copolymers, polypropylene, PVF, PVDF, etc. are described. Influence of composition of the fluorinating mixture (F₂-He-N₂-O₂-HF), fluorine partial pressure, temperature and fluorination duration, on the rate of formation of the fluorinated layer and the chemical composition, density, refraction index, surface energy, gas separation properties and friction coefficient of fluorinated layer have been investigated. Processes of formation and termination of long-living and short-living radicals and grafting of acrylonitrile to fluorinated polymers have been studied. Industrial applications of the direct fluorination to enhance the commercial properties of polymeric goods, such as separation factor of polymeric membranes for gas separation, barrier properties of polymer vessels, pipes and packagings, adhesion, printability, wetting and transparency in visible and IR are reviewed.     

High-performance liquid chromatography analysis of ten dyes for control of safety of commercial articles

Two high-performance liquid chromatographic methods, with ultraviolet-visible spectrophotometry detection (HPLC-UV/Vis) and with tandem mass spectrometry triple quadrupole interfaced with positive ion mode electrospray ionization detection (HPLC-ESI+-QqQ-MS/MS), for determination and quantification of ten commercial dyes are proposed for control in commercial products. Multiple peaks observed for some of the studied dyes in HPLC-UV/Vis chromatograms forced to obtain structural information by HPLC-ESI-MS/MS method with scan mode. The quality parameters of the two proposed chromatographic methods were evaluated for different requirements of normative, showing detection (LODs) and quantification (LOQs) limits around 60-890 and 200-2990 microg L(-1) for HPLC-UV/Vis, and 4.54-14.3 and 15.0-47.6 microg L(-1) for HPLC-ESI+-QqQ-MS/MS.     

Revealing the structural dynamics of feline serum albumin

Structural Chemistry - Serum albumin (SA) is a prevalent carrier protein in blood. SA carries a diverse range of nutrients, drugs, and metal ions. It has wide clinical and biochemical applications....     

Revealing the nature of thio-click reactions on the solid phase

Thiol- and yne-functionalized beads were manufactured in a simple microfluidic setup. While CuAAC and thiol-yne reactions were performed on yne-functionalized beads, 9 different thiol-X reactions were compared, in terms of kinetics and conversion, on thiol-functionalized beads.     

Revealing the roles of Hamiltonian coupling in bound-state quantum systems

A Hamiltonian coupling identification (HCI) technique is introduced to reveal the independent and cooperative roles of Hamiltonian matrix elements in determining the bound-state energies of quantum systems. The HCI technique operates by encoding each Hamiltonian matrix element with a unique modulation signal, producing a nonlinear signature in the energy eigenvalues that may be decoded to reveal the contributing coupling structure in the Hamiltonian. The HCI technique is capable of exploring the roles of Hamiltonian coupling structure within and beyond the convergence limits of standard perturbation theory expansions. The flexibility residing in the encoding and decoding processes may be exploited to tailor the analysis to meet the desired degree of sought-after information about the Hamiltonian coupling structure. HCI, based on a Fourier encoding and decoding scheme, is illustrated by extracting information on the role of coupling interactions in the potential matrix elements of several simple model systems.     

Revealing the solid electrolyte interface on calcium metal anodes

Owing to its low potential, crustal abundances and environmental friendliness, calcium metal anode(CMA) is emerging as a powerful contender in post-lithium era. However, the passivation of CMA fatally hinders its development. Recently, several feasible electrolytes have been developed. Nevertheless, as a pivotal part, the solid electrolyte interface(SEI) formed on CMA has not been paid enough attention to. In this review, based on the passivation mechanism of CMA, the favorable composition of SE...     

Revealing the Distribution of the Atoms within Individual Bimetallic Catalyst Nanoparticles

To be able to correlate the catalytic properties of nanoparticles with their structure, detailed knowledge about their make‐up on the atomic level is required. Herein, we demonstrate how atom‐probe tomography (APT) can be used to quantitatively determine the three‐dimensional distribution of atoms within a Au@Ag nanoparticle with near‐atomic resolution. We reveal that the elements are not evenly distributed across the surface and that this distribution is related to the surface morphology and residues from the particle synthesis.     

揭示思维过程突出科学方法的训练

教学心理学告诉我们 ,学生的认识活动与科学家的创造活动相比 ,两者有着相同的本质和相似的规律。以学生的认知过程为主线 ,将科学家的原发现过程 ,从教育和教学的层面进行适当的剪辑和编制 ,让学生追根溯源 ,使教学过程成为学生内心体验和主动参与的“再发现过程”或“亚研究过程” ,这对于培养学生的创新精神和创造能力非常重要。例如 ,在乙醛的化学性质的教学中 ,乙醛和银氨溶液、新制氢氧化铜悬浊液反应的实验是非常重要的教学内容。对于这一教学内容 ,如果只是简单地在演示实验结束之后 ,告诉学生一个静态的结论 ,而不是引导学生寻着科…     

Confirmatory test results on milk from commercial sources that tested positive by beta-lactam antibiotics screening tests.

Fifty-four milk samples from commercial sources that tested positive for beta-lactam antibiotics were analyzed by a multiresidue liquid chromatographic (LC) procedure based on LC fractionation. Penicillin G and cephapirin were the beta-lactam antibiotics found most frequently. Some samples did not contain detectable beta-lactam antibiotics. In a few, the presence of a beta-lactam antibiotic was suspected because certain LC fractions tested positive for antimicrobial activity, which was no longer present in a replicate treated with beta-lactamase. However, the unknowns could not be identified by LC analysis.     

Revealing the Nature of Singlet Fission under the Veil of Internal Conversion

Singlet fission (SF) holds the potential to boost the maximum power conversion efficiency of photovoltaic devices. Internal conversion (IC) has been considered as one of the major competitive deactivation pathways to transform excitation energy into heat. Now, using time‐resolved spectroscopy and theoretical calculation, it is demonstrated that, instead of a conventional IC pathway, an unexpected intramolecular singlet fission (iSF) process is responsible for excited state deactivation in isoindigo derivatives. The ¹TT state could form at ultrafast rate and nearly quantitatively in solution. In solid films, the slipped stacked intermolecular packing of a thiophene‐functionalized derivative leads to efficient triplet pair separation, giving rise to an overall triplet yield of 181 %. This work not only enriches the pool of iSF‐capable materials, but also contributes to a better understanding of the iSF mechanism, which could be relevant for designing new SF sensitizers.     

Revealing the Potential Application of EC-Synthetic Retinoid Analogues in Anticancer Therapy

(1) Background and Aim: All-trans retinoic acid (ATRA) induces differentiation and inhibits growth of many cancer cells. However, resistance develops rapidly prompting the urgent need for new synthetic and potent derivatives. EC19 and EC23 are two synthetic retinoids with potent stem cell neuro-differentiation activity. Here, these compounds were screened for their in vitro antiproliferative and cytotoxic activity using an array of different cancer cell lines. (2) Methods: MTT (3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide) assay, AV/PI (annexin V-fluorescein isothiocyanate (FITC)/propidium iodide (PI)), cell cycle analysis, immunocytochemistry, gene expression analysis, Western blotting, measurement of glutamate and total antioxidant concentrations were recruited. (3) Results: HepG2, Caco-2, and MCF-7 were the most sensitive cell lines; HepG2 (ATRA; 36.2, EC19; 42.2 and EC23; 0.74 µM), Caco-2 (ATRA; 58.0, EC19; 10.8 and EC23; 14.7 µM) and MCF-7 (ATRA; 99.0, EC19; 9.4 and EC23; 5.56 µM). Caco-2 cells were selected for further biochemical investigations. Isobologram analysis revealed the combined synergistic effects with 5-fluorouracil with substantial reduction in IC₅₀. All retinoids induced apoptosis but EC19 had higher potency, with significant cell cycle arrest at subG₀-G₁, -S and G₂/M phases, than ATRA and EC23. Moreover, EC19 reduced cellular metastasis in a transwell invasion assay due to overexpression of E-cadherin, retinoic acid-induced 2 (RAI2) and Werner (WRN) genes. (4) Conclusion: The present study suggests that EC-synthetic retinoids, particularly EC19, can be effective, alone or in combinations, for potential anticancer activity to colorectal cancer. Further in vivo studies are recommended to pave the way for clinical applications.     

Revealing the Cell Entry Dynamic Mechanism of Single Rabies Virus Particle

The rabies virus is a neurotropic virus that causes fatal diseases in humans and animals. Although studying the interactions between a single rabies virus and the cell membrane is necessary for understanding the pathogenesis, the internalization dynamic mechanism of single rabies virus in living cells remains largely elusive. Here, we utilized a novel force tracing technique based on atomic force microscopy(AFM) to record the process of single viral entry into host cell. We revealed that the force of the rabies virus internalization distributed at (65±25) pN, and the time was identified by two peaks with spacings of (237.2±59.1) and (790.3±134.4) ms with the corresponding speed of 0.12 and 0.04 μm/s, respectively. Our results provide insight into the effects of viral shape during the endocytosis process. This report will be meaningful for understanding the dynamic mechanism of rabies virus early infection.     

Revealing the Mechanism of Pressure-Induced Emission in Layered Silver-Bismuth Double Perovskites

Pressure-induced emission (PIE) associated with self-trapping excitons (STEs) in low-dimensional halide perovskites has attracted great attention for better materials-by-design. Here, using 2D layered double perovskite (C₆H₅CH₂CH₂NH₃⁺)₄AgBiBr₈ as a model system, we advance a fundamental physicochemical mechanism of the PIE from the perspective of carrier dynamics and excited-state behaviors of local lattice distortion. We observed a pressure-driven STE transformation from dark to bright states, corresponding a strong broadband Stokes-shifted emission. Further theoretical analysis demonstrated that the suppressed lattice distortion and enhanced electronic dimensionality in the excited-state play an important role in the formation of stabilized bright STEs, which could manipulate the self-trapping energy and lattice deformation energy to form an energy barrier between the potential energy curves of ground- and excited-state, and enhance the electron-hole orbital overlap, respectively.     

Mass Spectrometric Analysis Revealing Phosphorylation Modifications of Periostin

Human periostin was over-expressed in HEK293T cells, which was enriched by nickel ion affinity resin, and further purified by gel electrophoresis. Phosphopeptides contained in the tryptic digestion of the purified periostin were enriched by TiO₂ affinity chromatography, and then analyzed by liquid chromatography-tandem mass spectrometry(LC-MS/MS). LC-MS/MS analysis reveals three phosphorylation modification sites of periostin at IKVIEGpSLQPIIK(682―694), pSLHEKLKQDK(498―507) and p[TT]VLYEC^*C^*PGYM^*R(73―85). The established method could be a great help to profiling the phosphorylation status of periostin under different physiological environments, such as inflammatory and tumor micro-environments.     

Lanthanide Luminescence Revealing the Phase Composition in Hydrating Cementitious Systems

The hydration process of Portland cement in a cementitious system is crucial for development of the high-quality cement-based construction material. Complementary experiments of X-ray diffraction analysis (XRD), scanning electron microscopy (SEM) and time-resolved laser fluorescence spectroscopy (TRLFS) using europium (Eu(III)) as an optical probe are used to analyse the hydration process of two cement systems in the absence and presence of different organic admixtures. We show that different analysed admixtures and the used sulphate carriers in each cement system have a significant influence on the hydration process, namely on the time-dependence in the formation of different hydrate phases of cement. Moreover, the effect of a particular admixture is related to the type of sulphate carrier used. The quantitative information on the amounts of the crystalline cement paste components is accessible via XRD analysis. Distinctly different morphologies of ettringite and calcium−silicate−hydrates (C−S−H) determined by SEM allow visual conclusions about formation of these phases at particular ageing times. The TRLFS data provides information about the admixture influence on the course of the silicate reaction. The dip in the dependence of the luminescence decay times on the hydration time indicates the change in the structure of C−S−H in the early hydration period. Complementary information from XRD, SEM and TRLFS provides detailed information on distinct periods of the cement hydration process.