Cu-catalyzed tandem C-N bond formation for the synthesis of pyrroles and heteroarylpyrroles

A highly efficient Cu-catalyzed tandem C-N bond-forming reaction of 1,4-dihalo-1,3-dienes has been developed. The transformation allows the synthesis of pyrroles and heteroarylpyrroles with a wide variety of functional groups and substitution patterns from readily available precursors.     

A series of mono and diesters of itaconic acid: Synthesis and structural determination

Summary A series of mono and diesters of itaconic acid containing alkoxy and sulfide side chains of variable lengths has been synthesized. Their structures have been established on the basis of their spectral data.

---

Eine Serie von Mono- und Diestern von Itaconsäure: Synthese und Strukturbestimmung

Zusammenfassung Es wurde eine Serie von Mono- und Diestern von Itaconsäure mit Alkoxy- und Sulfidseitenketten variabler Länge synthetisiert. Die Strukturaufklärung erfolgte mittels spektroskopischer Daten.

     

A new phenanthrene-based bis-oxime chemosensor for Fe(III) and Cr(III) discrimination

The synthesis of two new 2,7-disubstituted phenanthrene-based bis oximes is described. The ability of these two compound for complexing heavy metal cations have been studied and complexation constants and complex stoichiometry for Cr³⁺ and Fe³⁺ complex have been determined. The fluorescent properties of ligand 2 make this compound able to act as a sensor able to discriminate between Cr³⁺ and Fe³⁺. Detection limits for these two cations have been evaluated.     

Microwave-assisted selective and efficient synthesis of 1,3,5-triazinyl mono and bisureas

An efficient and sustainable microwave-assisted approach for the one-step preparation of a wide range of 1,3,5-triazinyl mono- and bisureas has been developed, combining solvent-free conditions and microwave irradiation. In these conditions the very unreactive amino groups of 1,3,5-triazine-2,4-diamines successfully react with phenylisocyanate to yield selectively mono and bisureas.     

Reversible Clustering of Gold Nanoparticles under Confinement

A limiting factor of solvent‐induced nanoparticle self‐assembly is the need for constant sample dilution in assembly/disassembly cycles. Changes in the nanoparticle concentration alter the kinetics of the subsequent assembly process, limiting optical signal recovery. Herein, we show that upon confining hydrophobic nanoparticles in permeable silica nanocapsules, the number of nanoparticles participating in cyclic aggregation remains constant despite bulk changes in solution, leading to highly reproducible plasmon band shifts at different solvent compositions.     

Effect of testing conditions on the laser flash thermal diffusivity measurements of ceramics

Several experimental techniques either under steady state or transient heat transfer conditions, have been developed to evaluate thermal conductivity and thermal diffusivity of materials. However, testing difficulties resulting from specimen size, extended testing time and heat losses, have somewhat impaired the applicability of many of them. In this respect, the use of the laser flash technique for thermal diffusivity measurements, is a very convenient alternative, considering its basic modeling equation is independent of the temperature gradient as well as the heat flow, and in addition the heat losses can be analytically treated. Another important advantage of the technique is its rapid experimental execution. In this work, it is presented as an investigation concerning how the testing conditions such as specimen coating, laser power and pulse duration, base line adoption, heat losses correction methods, and specimen thickness, may affect the thermal diffusivity measurements of some ceramic materials using the laser flash technique.     

Copper nanoclusters conjugated silica nanoparticles modified on carbon paste as an electrochemical sensor for the determination of dopamine

An electrochemical sensor based on modification of carbon paste electrode by glutathione‐capped copper nanoclusters silica nanoparticles (CuNCs/SiO₂NPs) composite for determination of dopamine in the presence of ascorbic acid was presented. Transmission electron microscopy, scanning electron microscopy, energy dispersive X‐Ray analysis, X‐ray photoelectron spectroscopy, Fourier‐transform infrared spectroscopy, X‐ray diffraction and electrochemical impedance spectroscopy were used for characterization of the developed electrode. The electrochemical behavior of dopamine on CuNCs/SiO₂NPs/carbon paste electrode was investigated by cyclic voltammetry and differential pulse voltammetry. Dopamine was determined in the range of 10.0 – 900.0 μM, and the limit of detection was obtained as 0.43 μM. The electrochemical behaviors of the coexisting electroactive species, which often cause interference with the determination of dopamine, were investigated. The results show that the developed electrode does not show any interference with respect to coexisting species, even in the presence of ascorbic acid. The developed electrochemical sensor was further employed for the determination of dopamine in human blood plasma, with a good recovery.     

Investigation of Sequence Clipping and Structural Heterogeneity of an HIV Broadly Neutralizing Antibody by a Comprehensive LC-MS Analysis

CAP256 is one of the highly potent, broadly neutralizing monoclonal antibodies (bNAb) designed for HIV-1 therapy. During the process development of one of the constructs, an unexpected product-related impurity was observed via microfluidics gel electrophoresis. A panel of complementary LC-MS analyses was applied for the comprehensive characterization of CAP256 which included the analysis of the intact and reduced protein, the middle-up approach, and a set of complementary peptide mapping techniques and verification of the disulfide bonds. The designed workflow allowed to identify a clip within a protruding acidic loop in the CDR-H3 region of the heavy chain, which can lead to the decrease of bNAb potency. This characterization explained the origin of the additional species reflected by the reducing gel profile. An intra-loop disulfide bond linking the two fragments was identified, which explained why the non-reducing capillary electrophoresis (CE) profile was not affected. The extensive characterization of CAP256 post-translational modifications was performed to investigate a possible cause of CE profile complexity and to illustrate other structural details related to this molecule’s biological function. Two sites of the engineered Tyr sulfation were verified in the antigen-binding loop, and pyroglutamate formation was used as a tool for monitoring the extent of antibody clipping. Overall, the comprehensive LC-MS study was crucial to (1) identify the impurity as sequence clipping, (2) pinpoint the clipping location and justify its susceptibility relative to the molecular structure, (3) lead to an upstream process optimization to mitigate product quality risk, and (4) ultimately re-engineer the sequence to be clip-resistant.

Open image in new window

Graphical Abstract ?

     

Tartrazine: physical,thermal and biophysical properties of the most widely employed synthetic yellow food-colouring azo dye

Journal of Thermal Analysis and Calorimetry - The food-colouring dye tartrazine is a significant additive and in the same time a biologically active material. Thermal behaviour of trisodium...     

Sustainable self-assembly strategies for emerging nanomaterials

1. Download : Download high-res image (338KB)
2. Download : Download full-size image