One‐Pot Lipase Entrapment Within Silica Particles to Prepare a Stable and Reusable Biocatalyst for Transesterification

In order to enhance the reusability, Rhizomucor miehei lipase was entrapped in a single step within silica particles having an oleic acid core (RML@SiO₂). Characterization of RML@SiO₂ by scanning and transmission electron microscopy and Fourier transform infrared studies supported the lipase immobilization within silica particles. The immobilized enzyme was employed for transesterification of cottonseed oil with methanol and ethanol. Under the optimum reaction conditions of a methanol‐to‐oil molar ratio of 12:1 or ethanol‐to‐oil molar ratio of 15:1, stirring speed of 250 revolutions/min (flask radius = 3 cm), reaction temperature of 40 °C, and biocatalyst concentration of 5 wt% (with respect to oil), more than 98 % alkyl ester yield was achieved in 16 and 24 h of reaction duration in case of methanolysis and ethanolysis, respectively. The immobilized enzyme did not require any buffer solution or organic solvent for optimum activity; hence, the produced biodiesel and glycerol were free from metal ion or organic molecule contamination. The activation energies for the immobilized enzyme‐catalyzed ethanolysis and methanolysis were found to be 34.9 ± 1.6 and 19.7 ± 1.8 kJ mol^?1, respectively. The immobilized enzyme was recovered from the reaction mixture and reused in 12 successive runs without significant loss of activity. Additionally, RML@SiO₂ demonstrated better reusability as well as stability in comparison to the native enzyme as the former did not lose the activity even upon storage at room temperature (25–30 °C) over an 8‐month period.     

Doxorubicin-loaded cholic acid-polyethyleneimine micelles for targeted delivery of antitumor drugs: synthesis,characterization, and evaluation of their in vitro cytotoxicity

Doxorubicin-loaded micelles were prepared from a copolymer comprising cholic acid (CA) and polyethyleneimine (PEI) for the delivery of antitumor drugs. The CA-PEI copolymer was synthesized via pairing mediated by N,N’-dicyclohexylcarbodiimide and N-hydroxysuccinimide using dichloromethane as a solvent. Fourier transform infrared and nuclear magnetic resonance analyses were performed to verify the formation of an amide linkage between CA and PEI and doxorubicin localization into the copolymer. Dynamic light scattering and transmission electron microscopy studies revealed that the copolymer could self-assemble into micelles with a spherical morphology and an average diameter of <200 nm. The CA-PEI copolymer was also characterized by X-ray diffraction and differential scanning calorimetry. Doxorubicin-loaded micelles were prepared by dialysis method. A drug release study showed reduced drug release with escalating drug content. In a cytotoxicity assay using human colorectal adenocarcinoma (DLD-1) cells, the doxorubicin-loaded CA-PEI micelles exhibited better antitumor activity than that shown by doxorubicin. This is the first study on CA-PEI micelles as doxorubicin carriers, and this study demonstrated that they are promising candidates as carriers for sustained targeted antitumor drug delivery system.     

Synthesis of Novel Tetra(µ3-Methoxo) Bridged with [Cu(II)-O-Cd(II)] Double-Open-Cubane Cluster: XRD/HSA-Interactions,Spectral and Oxidizing Properties

A new double-open-cubane core Cd(II)-O-Cu(II) bimetallic ligand mixed cluster of type [Cl₂Cu₄Cd₂(NNO)₆(NN)₂(NO₃)₂].CH₃CN was made available in EtOH/CH₃CN solution. The 1-hydroxymethyl-3,5-dimethylpyrazole (NNOH) and 3,5-dimethylpyrazole (NNH) act as N,O-polydentate anion ligands in coordinating the Cu(II) and Cd(II) centers. The structure of the cluster in the solid state was proved by XRD study and confirmed in the liquid state by UV-vis analysis. The XRD result supported the construction of two octahedral and one square pyramid geometries types around the four Cu(II) centers and only octahedral geometry around Cd(II) two centers. Interestingly, NNOH ligand acts as a tetra-µ³-oxo and tri-µ²-oxo ligand; meanwhile, the N-N in NNH acts as classical bidentate anion/neutral ligands. The interactions in the lattice were detected experimentally by the XRD-packing result and computed via Hirschfeld surface analysis (HSA). The UV-vis., FT-IR and Energy Dispersive X-ray (EDX), supported the desired double-open cubane cluster composition. The oxidation potential of the desired cluster was evaluated using a 3,5-DTB-catechol 3,5-DTB-quinone as a catecholase model reaction.     

Effects of repeated frying on physicochemical characteristics,oxidative stress,and free radical scavenging potential of canola oil and ghee

The repeated use of cooking oils and ghee for the deep frying of food materials may affect their nutritional quality. The present study evaluated the effect of repeated frying on the physicochemical characteristics and antiradical potential of canola oil and ghee. The oil and ghee were used for frying of fish and chicken for 2, 4, 6, 8, and 10 frying cycles followed by the analysis of physicochemical, oxidative stress, and antiradical parameters. Regression analysis of the data showed a frying cycle-dependent significant linear increase in saponification (R² = 0.9507–0.9748), peroxide and acid values (R² = 0.956–0.9915), and malondialdehyde (MDA) production (R² = 0.9058–0.9557) of canola oil and ghee subjected to fish and chicken frying but exponential increase in saponification value (R² = 0.9778) and MDA production (R² = 0.7407) of canola oil and ghee used for fish frying. The increase in the number of frying cycles linearly decreased the iodine value (R² = 0.9781–0.9924), and 1, 1-diphenyl-2-picrylhydrazyl, hydroxyl, and 2, 2′-azino-bis(3-ethylbenzthiazoline-6-sulfonic acid) radical scavenging potential (R² = 0.9089–0.9979) of canola oil and ghee. Repeated frying in cooking oil and ghee increases oxidative stress and decreases their physicochemical and antioxidant qualities. Canola oil was comparatively more oxidative resistant than canola ghee. The regression equations derived from regression analysis will guide researchers to conduct similar types of univariate studies.     

Novel processing,testing and characterization of copper/carbon nanotube (Cu/CNT) yarn composite conductor

Sustainable electrified aircraft propulsion (EAP) is likely to lead to an increase in the electrical wiring contained within a single aircraft. Since the electrical resistance and mass of copper (Cu) conductors are associated with power losses, it is desirable to design high-conductivity lightweight conductor materials, thus reducing the mass of components like motor windings, low-voltage signal cables, and transmission cables for data and power to improve the overall energy efficiency. This paper describes a unique framework for manufacturing metalized carbon nanotube (CNT) composite conductors, measuring their electrical conductivity and strength, and modeling the overall conductivity and current sharing within such composites. Tensile testing was conducted on the processed composite conductor cables with the use of acoustic emission and electrical resistivity to determine stress-dependent-failure mechanisms while monitoring the electrical conductivity. The average of measured electrical conductivities of annealed Cu/CNT samples from batch 5 was greater than theoretical predictions by 9.8 percent and was also greater than the conductivity of pure annealed Cu by 4.8 percent and had comparable ultimate tensile strengths. Additionally, those Cu/CNT samples provide a 13.5% weight saving over current state of the art copper wires. Theories explaining improved intrinsic conductivity are discussed.     

Proton Nuclear Magnetic Resonance-Based Method for the Quantification of Epoxidized Methyl Oleate

Epoxidized methyl esters (EMO) with their high oxirane ring reactivity, acts as a raw material in the synthesis of various industrial chemicals including polymers, stabilizers, plasticizers, glycols, polyols, carbonyl compounds, biolubricants etc. EMO has been generally quantified by the gas chromatography (GC) and high-performance liquid chromatography (HPLC) techniques. Taking into the account of the limitations of these techniques, two qHNMR-based equations have been proposed for the quantification of EMO in the mixture of EMO and methylesters (MO). The validity of the proposed method was determined using standard mixtures of MO and EMO having different molar concentrations. The developed equations have been applied on the samples of EMO prepared from oleic acid in two-step process viz., esterification followed by epoxidation. The qHNMR-based EMO quantification showed acceptable agreement with the results obtained from HPLC analysis.     

Microstructural Aspects of Damage and Fracture in AZ31 Sheet Materials

There are considerable data in the literature dealing with deformation mechanisms in AZ31 sheets. However, there is little information on the damage and fracture processes in this material. In this contribution, digital image correlation is used to follow deformation patterns occurring during tensile and v-bending tests at room temperature. A variety of surface analysis techniques and three-dimensional x-ray tomography have been used to examine the relationship between deformation, damage initiation, and the final fracture processes. The results show that premature diffuse necking occurs in the tensile tests without transit into localized necking. Deformation twins cluster by an autocatalytic process to form shear bands serving as preferential sites for strain localization and crack initiation. Damage appears in the form of microcracks within the shear bands at a late stage of necking and lead to the final fracture. The presence and the distribution of second-phase particles and their distributions help accelerate the final fracture processes.     

Effect of thermal degradation on the impact properties of PVC compounds

An instrumented drop weight impact test was used to study the effect of thermal degradation on the impact properties of PVC compounds. The impact resistance of the aged compounds related well with their weight loss and hence, with thermal degradation. Each compound showed a specific weight loss percentage that correlated with a 50% loss in its impact properties (failure point), irrespective of the aging temperature. The results were also used to estimate a thermal index (TI) of each compound in a rapid and reliable way.     

Biodiesel from mutton fat using KOH impregnated MgO as heterogeneous catalysts

The use of MgO impregnated with KOH as heterogeneous catalysts for the transesterification of mutton fat with methanol has been evaluated. The mutton fat (fat) with methanol (1:22 M ratio) at 65 °C showed > 98% conversion to biodiesel with 4 wt% of MgO–KOH-20¹ (MgO impregnated with 20 wt% of KOH) in 20 min. The reaction conditions optimized were; the amount of KOH impregnation (5–20 wt%), the amount of catalyst (1.5–4 wt%, catalyst/fat), the reaction temperature (45–65 °C), fat to methanol molar ratio (1:11–1:22) and the effect of addition of water/oleic acid/palmitic acid (upto 1 wt%). Although, transesterification of fresh fat (moisture content 0.02 wt% and free fatty acids 0.002 wt%) with methanol in the presence of KOH (homogenous catalyst) resulted in the complete conversion to biodiesel, but in the presence of additional 1 wt% of either free fatty acid or moisture content, formation of soap was observed. The MgO–KOH-20 catalyst was found to tolerate additional 1 wt% of either the moisture or FFAs in the fat.