Supramolecular helical fluid columns from self-assembly of homomeric dipeptides

Herein, we demonstrate that with the widespread theme of residue patterning and stereochemical restraints of self-complimenting proteinogenic amino acids, a new and rich class of homomeric dipeptides exhibiting two-dimensional fluid aggregates with hierarchical ordering can be obtained. In particular, a simple way of achieving a class of functional dipeptides, wherein the first and the second residues chosen are L-/D-alanines and L-/D-leucines, has been accomplished. The supramolecules synthesized can be regarded as intermediates between polycatenars and taper-shaped amphiphiles because they possess two lipophilic segments interlinked by a peptide unit (spacer). Two pairs of enantiomers and their respective diastereomers derived from these amino acids are evidenced to self-organize into a helical columnar phase through hydrogen bonding by means of FTIR, UV/Vis, and chiroptical circular dichroism (CD) spectral analyses as well as by optical, calorimetric, electrical switching, and X-ray studies. The CD and X-ray studies have revealed that the form chirality (handedness) and the magnitude of out-of-plane fluctuations of the lattice planes of the fluid supramolecular columnar structures are solely directed by the stereochemistry encoded in the spacer. Of special significance, the less frequently found oblique helical columnar phase formed by a pair of enantiomers derived from L-/D-alanines, unlike those derived from other amino acids, exhibit ferroelectric behavior; the measured spontaneous polarization is as high as 440 nC cm(-2). Besides, all these supramolecules form stable organogels in ethanol and the CD and SEM studies on a representative gel suggest the presence of helical structures.     

Challenge in understanding size and shape dependent toxicity of gold nanomaterials in human skin keratinocytes

As the nanotechnology field continues to develop, assessing nanoparticle toxicity is very important for advancing nanoparticles for biomedical application. Here we report cytotoxicity of gold nanomaterial of different size and shape using MTT test, absorption spectroscopy and TEM. Spherical gold nanoparticles of different sizes are not inherently toxic to human skin cells, but gold nanorods are highly toxic due to the presence of CTAB as coating material. Due to toxicity of CTAB, and aggregation of gold nanomaterials in the presence of cell media, we have demonstrated that it is difficult to understand the cytotoxicity of gold nanomaterials individually.     

Synthesis of functionalized pyrroles and fused pyrroles through intermolecular [3 + 2] cycloaddition reaction

A facile and efficient synthesis of pyrrole and pyrrole-fused heterocyclic compounds has been demonstrated. The current protocol involves the in situ generation of azomethine ylides which undergoes intermolecular cycloaddition reaction and subsequent treatment with DDQ provides the pyrrole and fused heterocyclic compounds in good yields.     

Towards green synthesis of nanoparticles: From bio-assisted sources to benign solvents. A review

Current advancements in green synthesis of materials especially nanoparticles have led to conservation of natural and non-renewable resources along with reduction in environmental pollution. Development of cost-effective, simple and eco-friendly routes for the synthesis of nanoparticles is very important. All over the world, a wide variety of biogenic sources have been put to trial as a source of green agents to facilitate synthesis process. In addition to this, environmentally benign solvents are also being used these days in order to promote green synthesis. In this review, an attempt has been made to familiarise the readers with the different green routes for the synthesis of nanoparticles.     

Nonlinear direct inverse method: a shortcut method for simultaneous calibration and isotherm determination

This work addresses a way to combine isotherm determination and nonlinear calibration. In this method, like the classical inverse method, experimental elution profiles are compared with the results of a detailed model that accounts for nonlinearity in equilibrium, axial dispersion, and mass transfer kinetics. However, unlike the classical inverse method, the calibration of detector is carried out simultaneously with isotherm determination thereby reducing cost and saving time. In this study no limitation is imposed on the linearity of the detector signal or on the overlapping of elution profiles for the separation of enantiomers. The method has been experimentally validated for the separation of a mixture of guaifenesin enantiomers over a wide range of concentration.     

A Validated Chiral LC Method for the Enantiomeric Separation of Cinacalcet Hydrochloride

A rapid isocratic chiral LC method has been developed for the separation of (S)-cinacalcet from (R)-cinacalcet. Good resolution with R _S  > 3 was obtained using a Chiralpak-IA column (250 × 4.6 mm, particle size 5 μm) and n-hexane, ethanol and trifluoroacetic acid as the mobile phase (95:5:0.1, v/v) at ambient temperature. Flow rate was kept at 1.0 mL min^–1 and elution was monitored by UV detection at 223 nm. This method was further used to determine the presence of (S)-cinacalcet in enantiopure pharmaceutical formulations containing (R)-cinacalcet. This method allowed for the detection and quantitation of (S)-cinacalcet of levels at 0.04 and 0.16 μg mL^–1, respectively. The method was validated following ICH guidelines.     

Investigation of thermally stimulated charge relaxation mechanism in SiO<Subscript>2</Subscript> filled polycarbonate nanocomposites

The thermally stimulated charge relaxation properties of polycarbonate (PC) filled with SiO₂ nanofiller were studied by means of thermally stimulated discharge current (TSDC). The nanocomposite samples were further characterized by UV–vis spectroscopy, scanning electron microscopy, energy dispersive X-ray spectra, and differential scanning calorimetry (DSC) techniques to investigate the dispersion of nanofillers in polymer matrix and glass transition temperature. All pristine and nanocomposites samples of thickness about 25 μm were prepared using solution mixing method. The suitable weight percentage of SiO₂ nanofillers has been chosen to prevent the nonuniform dispersion. TSDC measurement of PC (Pristine) and PC+ (7% SiO₂) shows the single peak, while TSDC characteristic of other nanocomposites are showing two peaks. The higher temperature TSDC peak of pristine and nanocomposites samples is originated due to the charge relaxation from shallower and deeper trapping sites, however, low temperature peak is caused by dipolar relaxation of charge carriers. Since the position of higher temperature TSDC peak is generally an analysis of glass transition temperature of polymer/polymer nanocomposites. The authors have observed that the temperature of this peak is almost same as the T _g measured by DSC with 0 to ±5% variation. This article presents the deeper understanding of charge relaxation mechanism caused by SiO₂ nanofillers in polycarbonate.     

Measurement of the bremsstrahlung spectra generated from thick targets with <Emphasis Type="Italic">Z</Emphasis>=2–78 under the impact of 10 keV electrons

We present new experimental data on thick target bremsstrahlung spectra generated from the interaction of energetic electrons with bulk matter. The ‘photon yields’ in terms of double differential cross-sections (DDCS) are measured for pure elements of thick targets: Ti (Z = 22), Ag (Z = 47), W (Z = 74) and Pt (Z = 78) under the impact of 10 keV electrons. Comparison of DDCS obtained from the experimental data is made with those predicted by Monte-Carlo (MC) calculations using PENELOPE code. A close agreement between the experimental data and the MC calculations is found for all the four targets within the experimental error of 16%. Furthermore, the ratios of DDCS of bremsstrahlung photons emitted from Ag, W and Pt with those from Ti as a function of photon energy are examined with a relatively lower uncertainty of about 10% and they are compared with MC calculations. A satisfactory agreement is found between the experiment and the calculations within some normalizing factors. The variations of DDCS as a function of Z and of photon energy are also studied which show that the DDCS vary closely with Z; however, some deviations are observed for ‘tip’ photons emitted from high Z targets.     

A comparative study of Keane''s and Stacey''s equations of state

Chitosan acetate-ammonium nitrate (NH₄NO₃) films have been prepared by the solution-cast technique. Fourier transform infrared spectroscopy (FTIR) showed that complexation has occurred. FTIR exhibited shifts in amine and carbonyl bands from 1553 to 1520 cm⁻¹ and 1636 to 1617 cm⁻¹. A new peak was also observed at 1746 cm⁻¹. XRD shows that all complexes are amorphous. The highest conductivity at room temperature is 2.53×10⁻⁵ S cm⁻¹ for the film containing 45 wt% NH₄NO₃. The conductivity of the samples is dependent on the number of mobile ions and mobility.