β-Cyclodextrin-based chiral nanocomposite for thin-layer chromatographic detection of enantiomers of fluoxetine

Enantioselective analysis or separation is very essential for improved therapeutic effects of drugs as the pure enantiomeric drug formulations display potential benefits over racemates. In this work, we carried out (i) the synthesis of a nanocomposite of β-cyclodextrin and 3D graphene (G/β-CD NC), and (ii) its application for the detection of fluoxetine enantiomers [(RS)-FLX)] using a thin-layer chromatographic method. The synthesized nanocomposite was introduced into silica gel slurry while preparation of thin-layer plates. The separation conditions were optimized by altering pH, temperature, and mobile phase composition. The method is simple and easy to be optimized, and it can therefore be exploited to assess and monitor routine work of enantiomeric purity of drug enantiomers. The average precision (as measured by RSD) was in the region of 1.35‒1.65% for the enantiomers of (RS)-FLX. The measured limit of detection and limit of quantification for (RS)-FLX enantiomers were 1.8 and 5.4 mg mL^‒1, respectively.

     

Identification and quantification of anthocyanins,flavonoids, and phenolic acids in flowers of Rhododendron arboreum and evaluation of their antioxidant potential

The current study aimed to investigate the anthocyanins, non-anthocyanins (flavonoids and phenolic acids), and free radicals scavenging potential in the flowers of Rhododendron arboreum using ultra high performance liquid chromatography with ion mobility quadrupole time of flight tandem mass spectrometry. A total of 25 constituents including nine anthocyanins, six phenolic acids, and ten flavonoids were identified in the flower extract. The major anthocyanins identified were cyanidin-3-O-β-galactoside ( 1 ), cyanidin-3-O-α-arabinoside ( 4 ), and cyanidin-3-O-rhamnoside ( 8 ), while quercetin glycosides were the main identified flavonoids in R. arboreum flowers. Additionally, ultra high performance liquid chromatography methods were developed and validated for the quantification of nine compounds (anthocyanins, flavonoid glycosides, and phenolic acids); five of them were quantified using internal standards. The extracts were analyzed for total phenolics (123.6 mg GAE/g), anthocyanin content (1.76% w/w), and evaluated for antioxidant properties against 2,2-diphenyl-1-picrylhydrazyl radical (IC₅₀: 102.06 and 96.92 μg/mL) and 2,2′-azino-bis (3-ethylbenzothiazoline-6-sulfonic acid) radical cation (112.25 and 45.59 μM TE/g) assays. The profiling of R. arboreum for anthocyanins is reported for the first time. The findings suggest that the flowers are a promising source of bioactive constituents and could be used as functional food, antioxidants, and nutraceuticals.     

Allyl ether of aralkyl phenolic resin with low melt viscosity and its Alder‐ene blends with bismaleimide: synthesis,curing, and laminate properties

This paper outlines the synthesis and characterization of O‐allyl aralkyl phenolic (O‐allyl Xylok, OAX) resins having low melt viscosity and its Alder‐ene blends with 2, 2′‐bis 4‐[(4′‐maleimido phenoxy) phenyl] propane. The blends manifested a three‐stage curing pattern that converged to a two‐stage pattern on enhancing the maleimide content. The polymerization kinetics of typical allyl and maleimide rich resin systems showed apparent activation energy increasing and pre‐exponential factor decreasing from ene to the Diels–Alder step. Increased allyl content improved mechanical and impact properties of the composites at ambient temperature, although it diminished the retention of interlaminar shear strength at elevated temperature. Increased maleimide content of the resin was conducive for the higher rigidity for the composite and its retention at elevated temperature. A substantial increase in T_g (from 153°C to 280°C) and thermal stability was observed with an increase in maleimide content. High allyl content resulted in improved mechanical properties thanks to better resin–reinforcement interaction as revealed from morphological analysis. Copyright © 2014 John Wiley & Sons, Ltd.     

A rapid polyol combustion strategy towards scalable synthesis of nanostructured LiFePO4/C cathodes for Li-ion batteries

In the present study, carbon-coated lithium iron phosphate (LiFePO₄/C) is prepared directly by a polyol-assisted pyro-synthesis performed under reaction times of a few seconds in open-air conditions. The polyol solvent, tetraethylene glycol (TTEG), acts as a low-cost fuel to facilitate combustion and the released exothermic energy promotes the nucleation and growth processes of the olivine nanoparticles. In addition, phosphoric acid (used as the phosphorous source) acts as a catalyst to accelerate polyol carbonization. The structure analysis of the as-prepared LiFePO₄/C using X-ray, neutron diffraction and ⁷Li NMR studies suggested the efficacy of the rapid technique to produce highly crystalline phase-pure olivine nanocrystals. The electron microscopy and particle-size distribution studies revealed that the average particle diameters lie below 100 nm and confirmed the presence of a surface carbon layer of 2–3 nm thickness. The thermal and elemental studies indicated that the carbon content in the sample was approximately 5 %. The prepared LiFePO₄/C cathode delivered capacities of 162 mA h g^-1 at 0.1 °C rates with impressive capacity retention for extended cycling. The polyol-assisted pyro-synthesis, which evades the use of external energy sources, is not only a straightforward, simple and timely approach but also offers opportunities for large-scale LiFePO₄/C production.     

Molecular and Biochemical Characteristics of Recombinant β-Propeller Phytase from Bacillus licheniformis Strain PB-13 with Potential Application in Aquafeed

Phytic acid is the major storage form of organic phosphorus in nature- and plant-based animal feed. It forms insoluble complexes with nutritionally important metals and proteins that are unavailable for monogastric or agastric animals. Phytases initiate the stepwise hydrolysis of phytic acid and release inorganic orthophosphate. In the present investigation, the phytase gene from a phytase producing Bacillus licheniformis strain PB-13 was successfully expressed in Escherichia coli BL21. Recombinant phytase ‘rPhyPB13’ was found to be catalytically active, with an activity of 0.97 U/mL and specific activity of 0.77 U/mg. The rPhyPB13 was purified to 14.10-fold using affinity chromatography. Similar to other β-propeller phytases, purified rPhyPB13 exhibited maximal activity at pH 6.0–6.5 and 60 °C in the presence of 1 mM Ca²⁺ and was highly active over a wider pH range (pH 4.0–8.0) and high temperature (80 °C). It has shown maximum activity towards Na-phytate as substrate. The observed K _m , V _max and k _cat of purified rPhyPB13 were 1.064 mM, 1.32 μmol/min/mg and 27.46 s^?1, respectively. PhyPB13 was resistant to trypsin inactivation, activated in presence of Ca²⁺ and inhibited in presence of EDTA. Crude rPhyPB13 has good digestion efficiency for commercial feed and soybean meal. These results indicate that PhyPB13 is a β-propeller phytase that has application potential in aquaculture feed.     

Probing the Binding of Syzygium-Derived α-Glucosidase Inhibitors with N- and C-Terminal Human Maltase Glucoamylase by Docking and Molecular Dynamics Simulation

Human maltase glucoamylase (MGAM) is a potent molecular target for controlling post prandial glucose surplus in type 2 diabetes. Binding of small molecules from Syzygium sp. with α-glucosidase inhibitory potential in MGAM has been investigated in silico. Our results suggest that myricetin was the most potent inhibitor with high binding affinity for both N- and C-terminals of MGAM. Molecular dynamics revealed that myricetin interacts in its stretched conformation through water-mediated interactions with C-terminal of MGAM and by normal hydrogen bonding with the N-terminal. W1369 of the extended 21 amino acid residue helical loop of C-terminal plays a major role in myricetin binding. Owing to its additional sugar sites, overall binding of small molecules favours C-terminal MGAM.     

Supramolecular self-assembly and nanoencapsulation of [60]fullerene by bis-β-cyclodextrin

Bis-β-cyclodextrin connected via ethylene diamine on the primary side of the β-cyclodextrin was synthesized and used for the supramolecular non-covalent inclusion complex with C₆₀ in a mixed solvent system at room temperature. The apparent association constant of the 2:2 inclusion complex determined by combination of UV–Vis absorbance and Benesi–Hildebrand equation was found to be 1.78 × 10⁶ M^?1. The product obtained was highly water-soluble and superior in stability in aqueous medium as compared to previously known β-cyclodextrin/C₆₀ complex. The non-covalent self-assembly of bis-β-cyclodextrin and C₆₀ was characterized and confirmed from FT-IR, UV–Vis, XRD and TGA. The supramolecular aggregation behavior and particle size of the inclusion complex was found from transmission electron microscope and static light scattering measurements. The size of the inclusion complex was found to be ~30 ± 5 nm.     

Sodium alginate/HPMC/liquid paraffin emulsified (o/w) gel beads,by factorial design approach; and in vitro analysis

The present study involved development of a novel sodium alginate (SA)/HPMC/light liquid paraffin emulsified (o/w) gel beads containing Diclofenac sodium (DS) as an active pharmaceutical ingredient and its site specific delivery by using hard gelatin capsule fabricated by enteric coated Eudragit L-100 polymer. Emulsified gel beads were formulated by 3-level factorial design, ionic gelatin method. The obtained beads were characterized by Fourier transform infrared, X-ray diffraction and Field emission scanning electron microscope analysis. The variables such as SA (X₁), HPMC (X₂), were optimized for drug loading and in vitro drug release with the help of response surface methodology (RSM). The RSM analysis predicted that SA was significant for both drug loading (p = 0.0005) and drug release (p = 0.0041). HPMC was only significant for drug release (p = 0.0154). The cross-product contribution (2FI) and quadratic model were found to be adequate and statistically accurate with correlation value (R²) of 0.9054 and 0.9450 to predict the drug loading and drug release respectively. An increase in concentration of HPMC and SA decreases the drug loading as well as the drug release. The obtained optimum values of drug loading and DS released were 7.43 % and 85.54 % respectively, which were well in agreement with the predicted value by RSM.     

Polycaprolactone solution–based ink for designing microfluidic channels on paper via 3D printing platform for biosensing application

This work reports a novel fabrication technique for development of channels on paper‐based microfluidic devices using the syringe module of a 3D printing syringe–based system. In this study, printing using polycaprolactone (PCL)‐based ink (Mw 70 000‐90 000) was employed for the generation of functional hydrophobic barriers on Whatman qualitative filter paper grade 1 (approximate thickness of 180 μm and pore diameter of 11 μm), which would effectively channelize fluid flow to multiple assay zones dedicated for different analyte detection on a microfluidic paper‐based analytical device (μPAD). The standardization studies reveal that a functional hydrophilic channel for sample conduction fabricated using the reported technique can be as narrow as 460.7 ± 20 μm and a functional hydrophobic barrier can be of any width with a lower limit of about 982.2 ± 142.75 μm when a minimum number of two layers of the ink is extruded onto paper. A comparison with the hydrodynamic model established for writing with ink is used to explain the width of the line printed by this system. A fluid flow analysis through a single channel system was also carried out to establish its conformity with the Washburn model, which governs the fluid flow in two‐dimensional μPAD. The presented fabrication technique proves to be a robust strategy that effectively taps the advantages of this 3D printing technique in the production of μPADs with enhanced speed and reproducibility.     

Crystal and Molecular Structure of Tosyl Pyrrolidine-2-Methanol (C12H17SO3N)

C₁₂H₁₇SO₃N, M_r = 255.33, Orthorhombic, P2₁2₁2₁, a = 11.703(1) Å, b = 14.797(3) Å, c = 14.971(2) Å, V = 2592.52 ų, Z = 8, D_m = 1.309 Mgm⁻³, D_c = 1.308 Mgm⁻³, mμ = 21.57 cm⁻¹, F(000) = 1088, T = 290 K, final R = 0.080 for 2416 unique reflections. There are two crystallographically independent molecules in the unit cell of the title compound.