Synthesis of copper dendrite nanostructures by a sonoelectrochemical method

Copper dendrites have been prepared by a sonoelectrochemical process from an aqueous solution of Cu(2+) in the presence of polyvinyl alcohol. A SEM image of the morpholohy of the copper formed on the electrode after one electric pulse is presented. A subsequent sonic pulse removes the copper from the electrode surface, cleaning it for the next step. The formation of the dendrites is accounted for by the "drying-mediated self-assembly of nanoparticles" theory.     

ESR and photoluminescence properties of Cu doped ZnS nanoparticles

Nanoparticles of Zn1-xCuxS with Cu concentrations of x=0.0, 0.1, 0.2, 0.3 and 0.4 were prepared by a co-precipitation reaction method from homogeneous solutions of zinc and copper salts. Both the ZnS and ZnS:Cu nanoparticles excited at about 370 nm exhibits a broad green emission band peaking around 491 nm, which confirms the characteristic feature of Zn2+ as well as Cu2+ ions as luminescent centers in the lattice. The TEM micrographs showed spherical morphology for ZnS nanocrystals and the average size of the particles was estimated to be around 8.5 nm. At liquid nitrogen temperature, ESR signal characteristic of Cu2+ ions was observed in samples of all concentrations. ESR spectra analysis also indicated that Cu2+ ions enter the host lattice by replacing Zn2+ ions with distorted tetrahedral site symmetry.     

A Validated LC Method for the Determination of Chiral Purity of (1S)-6,11-Dioxo-1,2,3,4,6,11-Hexahydropyridazino[1,2-b]Phthalazine-1-Carboxylic Acid: A Key Intermediate of Cilazapril

A simple and accurate normal phase liquid chromatographic method was developed for the determination of chiral purity of (1S)-6,11-dioxo-1,2,3,4,6,11-hexahydropyridazino[1,2-b]phthalazine-1-carboxylic acid, S-enantiomer used as key intermediate in the manufacturing of cilazapril bulk drug. Chromatographic separation between (1S)-6,11-dioxo-1,2,3,4,6,11-hexahydropyridazino[1,2-b]phthalazine-1-carboxylic acid, and its opposite enantiomer (1R)-6,11-dioxo-1,2,3,4,6,11-hexahydropyridazino[1,2-b]phthalazine-1-carboxylic acid, R-enantiomer was achieved using a Chiralpak AD-H column using a mobile phase containing hexane, isopropyl alcohol and tri-fluoro acetic acid (80:20:0.1 v/v/v). The resolution between the two enantiomers was found to be more than 3.2. The limit of detection (LOD) and limit of quantitation (LOQ) of the R-enantiomer was 0.15 and 0.5 μg mL^?1, respectively, for 10 μL injection volume. The percentage recoveries of the R-enantiomer ranged from 96.5 to 105.3 in the bulk samples of (1S)-6,11-dioxo-1,2,3,4,6,11-hexahydropyridazino[1,2-b]phthalazine-1-carboxylic acid. The test solution and mobile phase was observed to be stable up to 24 h after the preparation. The developed method was validated as per International Conference on Harmonization guidelines in terms of LOD, LOQ, precision, linearity, accuracy, robustness and ruggedness.     

Effect of surface charge of magnetite nanoparticles on their internalization into breast cancer and umbilical vein endothelial cells

Internalization of magnetite nanoparticles with diameter of approximately 40 nm into normal and cancer cells was examined by microscopic observation and flow cytometry. Magnetite nanoparticles were synthesized by hydrolysis in an aqueous solution containing ferrous chloride with organic amines as a base. It was demonstrated that the difference in surface charge of magnetite nanoparticles brought about the difference in uptake efficiency. The nanoparticles with positive charge showed higher internalization into human breast cancer cells than the nanoparticles with negative charge, while the degree of internalization of the positively- and negatively-charged nanoparticles into human umbilical vein endothelial cells (HUVEC) was almost the same.     

Molecular basis of healing and fracture at polymer interfaces

The interdiffusion of polymer chains across a polymer–polymer interface, and subsequent fracture to re-create the interface is reviewed. In particular, films formed via latex coalescence provide a very large surface area. Of course, latex film formation is a very important practical problem. Healing of the interface by interdiffusion is treated using the de Gennes reptation theory and the Wool minor chain reptation model. The self-diffusion coefficients of polystyrene and the polymethacrylates obtained by small-angle neutron scattering, SANS, direct non-radiative energy transfer, DET, and other techniques are compared. Reduced to 150,000 g/mol and 135°C, both polystyrene and poly(methyl methacrylate) have diffusion coefficients of the order of 10^?16?10^?17 cm²/sec. Variations in the diffusion coefficient values are attributed to the experimental approaches, theoretical treatments and molecular weight distribution differences. An activation energy of 55 kcal/mol was calculated from an Arrhenius plot of all polystyrene data reduced to a number-average molecular weight of 150,000 g/mol, using an inverse square molecular weight conversion method. Interestingly, this is in between the activation energies for the α and β relaxation processes in polystyrene, 84 and 35 kcal/mol, respectively. Fracture of polystyrene was considered in terms of chain scission and chain pull-out. A dental burr apparatus was used to fracture the films. For low molecular weights, chain pull-out dominates, but for high molecular weights, chain scission dominates. At 150,000 g/mol, the energy to fracture is divided approximately equally between the two mechanisms. Above a certain number average molecular weight (about 400,000 g/mol), the number of chain scissions remains constant at about 10²⁴ scissions/m³. Energy balance calculations for film formation and film fracture processes indicate that the two processes are partly reversible, but have important components of irreversibility. From the interdiffusion SANS data, the diffusion rate is calculated to be about 1 Å/min, which is nine orders of magnitude slower than the dental burr pull-out velocity of about 0.8 cm/sec.     

Structural and optical characterization of ZnS nanoparticles co-doped with Mn and Te

Nanoparticles of Zinc sulfide co-doped with equal atomic percentages of Mn and Te (5, 10 and 15 at%) were synthesized for the first time by chemical co-precipitation method. Thiophenol was used to passivate the surface of the particles. The as-prepared samples were amorphous in nature and nano-crystallinity was induced after calcining at 300 °C/2 h. The nanoparticles were characterized by EDAX, XRD, TEM, optical absorption and PL studies. EDAX spectra revealed only minor deviations of the dopant concentrations from the target compositions. The nanoparticles showed cubic structure. The particle size estimated from XRD/TEM was in the range 3–5 nm. Optical absorption studies showed a blue-shift of the fundamental absorption edge with respect to that of bulk ZnS. PL spectra showed emission in the red region with composition dependent emission wavelength. ZnS nanoparticles doped with Mn (5 and 10 at%) were also synthesized and characterized for comparison.     

LC-HRMS-based targeted metabolomics for high-throughput and quantitative analysis of 21 growth inhibition-related metabolites in Chinese hamster ovary cell fed-batch cultures

Chinese hamster ovary (CHO) cells have been widely used in the biopharmaceutical industry for production of therapeutic proteins. CHO cells in fed-batch cultures produce various amino acid–derived intermediate metabolites. These small molecule metabolic byproducts have proven to be critical to cell growth, culture performance, and, more interestingly, antibody drug productivity. Herein, we developed an LC-HRMS-based targeted metabolomics approach for comprehensive quantification of total 21 growth inhibition-related metabolites generated from 14 different amino acids in CHO cell fed-batch cultures. High throughput derivatization procedures, matrix-matched calibration curves, stable isotope-labeled internal standards, and accurate mass full MS scan were utilized to achieve our goal for a wide range of metabolite screening as well as validity and reliability of metabolite quantification. We further present a novel analytical strategy for extending the assay's dynamic range by utilizing naturally occurring isotope M + 1 ion as a quantification analog in the circumstances where the principal M ion is beyond its calibration range. The integrated method was qualified for selectivity, sensitivity, linearity, accuracy, precision, isotope analysis, and other analytical aspects to demonstrate assay robustness. We then applied this metabolomics approach to characterize metabolites of interest in a CHO cell-based monoclonal antibody (mAb) production process with fed-batch bioreactor culture mode. Absolute quantification combined with multivariate statistical analysis illustrated that our target analytes derived from amino acids, especially from branched-chain amino acids, closely correlated with cell viability and significantly differentiated cellular stages in production process.