Chiral resolution of multichiral center racemates by different modalities of chromatography

It is a continuous chase of researchers to separate chiral racemates due to their dominance in the pharmaceutical industry, agrochemicals, and food additives. There are many analytical techniques which have been used to resolve one chiral center racemates, but, little the literature report is scanty for the resolution of multiple stereogenic center racemates. Therefore, in this article the efforts were made to describe the enantiomeric resolution of multiple stereogenic center racemates by different modalities of chromatography. The various modalities discussed are high-performance liquid chromatography, capillary electrophoretic chromatography, miceller electrokinetic chromatography, supercritical fluid chromatography, nanoliquid chromatography, and gas chromatography. Besides, the attempts have also been made to discuss the future challenges and prospectives of the enantiomeric resolution of multichiral racemates.     

Determination of fatty acids by high-performance liquid chromatography and fluorescence detection using precolumn derivatization with 9-fluorenylmethyl chloroformate

A new high-performance liquid chromatographic method is described for the determination of fatty acids in seed oils. The method was based on precolumn derivatization with 9-fluorenylmethyl chloroformate as a labeling agent and fluorescence detection. Fatty acids were extracted from the samples and subjected to derivatization with the reagent at 60°C for 10?min. The chromatographic separation of 14 fatty acids (C10–C22) was achieved on a combined loading compression octadecyl sulfate (CLC-ODS) column with a run time of 30?min. Three-step gradient elution of a mobile phase consisted of acetonitrile and water was used, and the signal was monitored at excitation and emission wavelengths of 265 and 315?nm, respectively. The method indicated favorable sensitivity and reproducibility for fatty acids’ derivatives. The detection limits, at a signal-to-noise ratio of 3, were 0.01–0.05?µg/ml and relative standard deviations (RSDs) were less than 0.27%. Excellent linear responses were observed with coefficients of 0.9995. This method was applied to quantify fatty acids in white, brown, and black sesame seeds’ oil.     

Energy transfer rate in double-layer graphene systems: Linear regime

We theoretically investigate the energy transfer phenomenon in a double-layer graphene (DLG) system. We use the balance equation approach in linear regime and random phase approximation screening function to obtain energy transfer rates at different electron temperatures, densities and interlayer spacings. We find that the rate of energy transfer in the DLG is qualitatively similar to that obtained in the double-layer two-dimensional electron gas but its values are an order of magnitude greater. Also, at large electron temperature differences between two graphene layers, the electron density dependence of energy transfer is significantly different, particularly in case of unequal electron densities.     

Thickness and local field effects on energy transfer rate in coupled quantum wells system: Linear regime

We investigate theoretically the dependence of energy transfer rate in Double-Quantum-Well system on the well thickness by using the balance equation formalism. Also, by including the local field correction in our calculations through the zero- and finite-temperature Hubbard approximations, we study the effect of the short-range interactions on the energy transfer phenomenon. Calculations consider both the static and dynamic screening approximations. Our numerical results predict that the energy transfer rate increases considerably by increasing the layers' thicknesses and by taking into account the short-range interactions, as well.     

Development and validation of a UV-spectrophotometric method for the determination of pheniramine maleate and its stability studies

A sensitive, precise, and cost-effective UV-spectrophotometric method is described for the determination of pheniramine maleate (PAM) in bulk drug and tablets. The method is based on the measurement of absorbance of a PAM solution in 0.1 N HCl at 264 nm. As per the International Conference on Harmonization (ICH) guidelines, the method was validated for linearity, accuracy, precision, limits of detection (LOD) and quantification (LOQ), and robustness and ruggedness. A linear relationship between absorbance and concentration of PAM in the range of 2–40 μg/ml with a correlation coefficient (r) of 0.9998 was obtained. The LOD and LOQ values were found to be 0.18 and 0.39 μg/ml PAM, respectively. The precision of the method was satisfactory: the value of relative standard deviation (RSD) did not exceed 3.47%. The proposed method was applied successfully to the determination of PAM in tablets with good accuracy and precision. Percentages of the label claims ranged from 101.8 to 102.01% with the standard deviation (SD) from 0.64 to 0.72%. The accuracy of the method was further ascertained by recovery studies via a standard addition procedure. In addition, the forced degradation of PAM was conducted in accordance with the ICH guidelines. Acidic and basic hydrolysis, thermal stress, peroxide, and photolytic degradation were used to assess the stability-indicating power of the method. A substantial degradation was observed during oxidative and alkaline degradations. No degradation was observed under other stress conditions.     

Shape-directing role of cetyltrimethylammonium bromide in the preparation of silver nanoparticles

We report a simple chemical reduction method for the synthesis of different colored silver nanoparticles, AgNP, using tyrosine as a reducing agent. Effects of cetyltrimethylammonium bromide, CTAB, and tyrosine concentrations are analyzed by UV-visible measurements and scanning electron microscopy (SEM) to evaluate the mode of AgNP aggregation. The position and shape of the surface resonance plasmon absorption bands strongly depend on the reaction conditions, i.e., [CTAB], [tyrosine], and reaction time. Sub-, post-, and dilution-micellar effects are accountable for the fast and slow nucleation and growth processes. Spectrophotometric measurement also shows that the average size and the polydispersity of AgNP increase with [CTAB] in the solution. CTAB acted as a shape-directing agent.     

Cyclopalladated complexes of 2-phenylaniline and their catalytic activity in Suzuki and Heck reactions under mild conditions

A series of palladium complexes bearing monodentate and bidentate ligands were applied in the Suzuki reaction of aryl halides and the Heck reaction of styrene with phenylboronic acid. The complexes were found to be effective catalysts for these reactions affording the cross-coupled products in moderate to excellent yields.     

Antibacterial Activity of a Novel Oligosaccharide from Streptomyces californics against Erwinia carotovora subsp. Carotovora

The present study aims to characterize and predict models for antibacterial activity of a novel oligosaccharide from Streptomyces californics against Erwinia carotovora subsp. carotovora using an adaptive neuro-fuzzy inference system and an artificial neural network. The mathematical predication models were used to determine the optimal conditions to produce oligosaccharide and determine the relationship between the factors (pH, temperature, and time). The characteristics of the purified antibacterial agent were determined using ultraviolet spectroscopy (UV/Vis), infrared spectroscopy (FT-IR), nuclear magnetic resonance spectroscopy (¹H- and ¹³C-NMR), and mass spectrometry (MS). The best performances for the model were 39.45 and 35.16 recorded at epoch 1 for E. carotovora Erw₅ and E. carotovora EMCC 1687, respectively. The coefficient (R²) of the training was more than 0.90. The highest antimicrobial production was recorded after 9 days at 25 °C and a pH of 6.2, at which more than 17 mm of the inhibition zone was obtained. The mass spectrum of antimicrobial agent (peak at R.T. = 3.433 of fraction 6) recorded two molecular ion peaks at m/z = 703.70 and m/z = 338.30, corresponding to molecular weights of 703.70 and 338.30 g/mol, respectively. The two molecular ion peaks matched well with the molecular formulas C₂₉H₅₃NO₁₈ and C₁₄H₂₆O₉, respectively, which were obtained from the elemental analysis result. A novel oligosaccharide from Streptomyces californics with potential activity against E. carotovora EMCC 1687 and E. carotovora Erw₅ was successfully isolated, purified, and characterized.     

An Experimental Design Approach to Quantitative Expression for Quality Control of a Multicomponent Antidiabetic Formulation by the HILIC Method

A rapid and reproducible hydrophilic liquid chromatography (HILIC) process was established for concomitant determination of remogliflozin etabonate (RE), vildagliptin (VD), and metformin (MF) in a formulation. A face-centered central composite experimental design was employed to optimize and predict the chromatographic condition by statistically studying the surface response model and design space with desirability close to one. A HILIC column with a simple mobile phase of acetonitrile (65% v/v) and 20 mM phosphate buffer (35% v/v, pH 6, controlled with orthophosphoric acid) was used to separate RE, VD, and MF. RE, VD, and MF were separated in 3.6 min using an isocratic mode mobile phase flow at a flow rate of 1.4 mL at room temperature, and the analytes were examined by recording the absorption at 210 nm. The developed HILIC method was thoroughly validated for all parameters recommended by ICH, and linearity was observed in the ranges 20–150 µg/mL, 10–75 µg/mL, and 50–750 µg/mL for RE, VD, and MF, respectively, along with excellent regression coefficients (r² > 0.999). The calculated percentage relative deviation and relative error ascertained the precision and accuracy of the method. The selectivity and accuracy were further confirmed by the high percentage recovery of added standard drugs to the formulation using the standard addition technique. The robustness of the HILIC processes was confirmed by developing a half-normal probability plot and Pareto chart, as the slight variation of a single factor had no significant influence on the assay outcomes. Utilization of the optimized HILIC procedure for concurrent quantification of RE, VD, and MF in solid dosage forms showed accurate and reproducible results. Hence, the fast HILIC method can be regularly employed for the quality assurance of pharmaceutical preparations comprising RE, VD, and MF.     

Efficient aerial oxidation of different types of alcohols using ZnO nanoparticle–MnCO3-graphene oxide composites

Graphene–metal nanocomposites have been found to remarkably enhance the catalytic performance of metal nanoparticle-based catalysts. In continuation of our previous report, in which highly reduced graphene oxide (HRG)-based nanocomposites were synthesized and evaluated, we present nanocomposites of graphene oxide (GRO) and ZnO nanoparticle-doped MnCO₃ ([ZnO–MnCO₃/(1%)GRO]) synthesized via a facile, straightforward co-precipitation technique. Interestingly, it was noticed that the incorporation of GRO in the catalytic system could noticeably improve the catalytic efficiency compared to a catalyst (ZnO–MnCO₃) without GRO, for aerial oxidation of benzyl alcohol (BzOH) employing O₂ as a nature-friendly oxidant under base-free conditions. The impacts of various reaction factors were thoroughly explored to optimize reaction conditions using oxidation of BzOH to benzaldehyde (BzH) as a model substrate. The catalysts were characterized using X-ray diffraction, thermogravimetric analysis, Fourier transform infrared spectroscopy, field-emission scanning electron microscopy, Energy dispersive X-ray spectroscopy (EDX), Brunauer-Emmett-Teller (BET), and Raman spectroscopy. The (1%)ZnO–MnCO₃/(1%)GRO exhibited significant specific activity (67 mmol.g⁻¹.hr⁻¹) with full convversion of BzOH and >99% BzH selectivity within just 6 min. The catalytic efficiency of the (1%)ZnO–MnCO₃/(1%)GRO nanocomposite was significantly better than the (1%)ZnO–MnCO₃/(1%)HRG and (1%)ZnO–MnCO₃ catalysts, presumably due to the existence of oxygen-possessing groups on the GRO surface and as well as a very high surface area that could have been instrumental in uniformly dispersing the active sites of the catalyst, i.e., ZnO–MnCO₃. Under optimum circumstances, various kinds of alcohols were selectively transformed to respective carbonyls with full convertibility over the (1%)ZnO–MnCO₃/(1%)GRO catalyst. Furthermore, the highly effective (1%)ZnO–MnCO₃/(1%)GRO catalyst could be successfully reused and recycled over five consecutive runs with a marginal reduction in its performance and selectivity.