Chromatographic separation of glucopyranosyl sinapate from canola meal

The compound 1-O-β-D glucopyranosyl sinapate (GPS), a phenolic glycoside, was separated from ethanolic extracts of defatted canola meal by a two-step chromatographic method. The first step involved Sephadex LH-20 chromatography with methanol as the eluting solvent. The solvent from the fraction containing GPS was evaporated, and glucopyranosyl sinapate was subsequently separated by a semi-preparative high-performance liquid chromatography method with an RP-18 column and a mobile phase consisting of water/acetonitrile/acetic acid (88∶10∶2, vol/vol/vol).     

Inactivation of glucosamine-6-phosphate synthase by N3-oxoacyl derivatives of L-2,3-diaminopropanoic acid

N(3)-Oxoacyl derivatives of L-2,3-diaminopropanoic acid 1-4, containing either an epoxide group or a conjugated double bond system, inactivate Saccharomyces cerevisiae glucosamine-6-phosphate (GlcN-6-P) synthase in a time- and concentration dependent manner. The results of kinetics studies on inactivation suggested a biphasic course, with formation of the enzyme-ligand complex preceding irreversible modification of the enzyme. The examined compounds differed markedly in their affinity to the enzyme active site. Inhibitors containing a phenyl ketone moiety bound much more strongly than their methyl ketone counterparts. The molecular mechanism of enzyme inactivation by phenyl ketone compounds 1 and 3 was elucidated by using a stepwise approach with 2D NMR, MS and UV-visible spectroscopy. A substituted thiazine derivative was identified as the final product of a model reaction between an epoxide compound, 1, and L-cysteine ethyl ester (CEE); and the respective cyclic product, found as a result of reaction between 1 and CGIF tetrapeptide, was identical to the N-terminal fragment of GlcN-6-P synthase. On the other hand, the reaction of a double-bond-containing compound, 3, with CEE, CGIF and GlcN-6-P synthase led to the formation of a C-S bond, without any further conversion or rearrangement. Molecular mechanisms of the reactions studied are proposed.     

Template method synthesis of mesoporous carbon spheres and its applications as supercapacitors

Mesoporous carbon spheres (MCS) have been fabricated from structured mesoporous silica sphere using chemical vapor deposition (CVD) with ethylene as a carbon feedstock. The mesoporous carbon spheres have a high specific surface area of 666.8 m²/g and good electrochemical properties. The mechanism of formation mesoporous carbon spheres (carbon spheres) is investigated. The important thing is a surfactant hexadecyl trimethyl ammonium bromide (CTAB), which accelerates the process of carbon deposition. An additional advantage of this surfactant is an increase the yield of product. These mesoporous carbon spheres, which have good electrochemical properties is suitable for supercapacitors.     

Influence of α‐amylolysis on the formation of electron density inhomogeneities on the surface of starch granules

Low‐temperature nitrogen adsorption and SAXS were used to analyze the granule surface of wheat and rice starches before and after an action of Bacillus subtilis α‐amylase. Results obtained by the first method showed that α‐amylolysis caused surface changes arising of new pores or enlarging diameters of pores already existing. According to the SAXS results, the action of enzymes caused complete sharpening of a solid skeletal boundary in the case of wheat starch granules. Partial sharpening of this boundary in the case of rice starch granules could be attributed to the relatively high content of proteins in rice starch.     

Silver Nanoparticles as a Tool for the Study of Spontaneous Aggregation of Immunoglobulin Monoclonal Free Light Chains

Some misfolded proteins, e.g., immunoglobulin monoclonal free light chains (FLC), tend to form fibrils. Protein deposits in tissue may lead to amyloidosis and dysfunction of different organs. There is currently no technique allowing for the identification of FLC that are prone to aggregate. The development of such a method would enable the early selection of patients at high risk of developing amyloidosis. The aim of this study was to investigate whether silver nanoparticles (AgNPs) could be a useful tool to study the process of aggregation of FLC and their susceptibility to form the protein deposits. Mixtures of AgNPs and urine samples from patients with multiple myeloma were prepared. To evaluate the aggregation process of nanoparticles coated with proteins, UV-visible spectroscopy, transmission electron microscopy, and the original laser light scattering method were used. It has been shown that some clones of FLC spontaneously triggered aggregation of the nanoparticles, while in the presence of others, the nanoparticle solution became hyperstable. This is probably due to the structure of the chains themselves, unique protein-AgNPs interactions and perhaps correlates with the tendency of some FLC clones to form deposits. Nanoparticle technology has proven to be helpful in identifying clones of immunoglobulin FLC that tend to aggregate.     

Three-phase metal kinetics in terrestrial invertebrates exposed to high metal concentrations

Models of metal toxicokinetics are critically evaluated using both newly generated data in the NoMiracle project as well as those originating from older studies. The analysis showed that the most frequently used one-compartment two-phase toxicokinetic model, with one assimilation and one elimination rate constant, does not describe correctly certain data sets pertaining particularly to the pattern of assimilation of trace elements. Using nickel toxicokinetics in carabid beetles and earthworms as examples, we showed that Ni in fact exhibits a three-phase kinetics with a short phase of fast metal accumulation immediately after exposure, followed by partial elimination to an equilibrium concentration at a later stage of a metal exposure phase, and by final elimination upon transfer to an uncontaminated food/soil. A similar phenomenon was also found for data on cadmium kinetics in ground beetles and copper kinetics in earthworms in data already published in the literature that was not accounted for in the earlier analysis of the data. The three-phase model suggests that the physiology of controlling body metal concentrations can change shortly after exposure, at least in some cases, by increasing the elimination rate and/or decreasing metal assimilation. Hence, the three-phase model, that allows for different assimilation and/or elimination rates in different phases of exposure to a toxicant, may provide insight into temporal changes in the physiology of metal handling. Consequently, this alternative model should always be tested when describing metal toxicokinetics when temporal patterns of internal metal concentration exhibit an initial “overshoot” in body metal concentrations.     

Influence of air-jet vortex generator diameter on separation region

Control of shock wave and boundary layer interaction continues to attract a lot of attention. In recent decades several methods of interaction control have been investigated. The research has mostly concerned solid (vane type) vortex generators and transpiration methods of suction and blowing. This investigation concerns interaction control using air-jets to generate streamwise vortices. The effectiveness of air-jet vortex generators in controlling separation has been proved in a previous research. The present paper focuses on the influence of the vortex generator diameter on the separation region. It presents the results of experimental investigations and provides new guidelines for the design of air-jet vortex generators to obtain more effective separation control.     

The Inverse Reconstruction of the Heat Transfer Coefficient for the Free Surface Water Jet

This article presents an application of inverse algorithm for reconstruction of heat transfer coefficient (HTC) for a water jet impinging a flat surface. Such an approach, allows for decoupling complex fluid flow from heat conduction in a solid impinged by jet. The approach starts with parameterization of a functional form of unknown boundary temperature and heat flux occurring at the fluid–solid interface. Later, Newton's law of cooling is used to force temporal invariability of HTC. Unknown coefficients of HTC distribution are determined from a least square fit between measured and computed temperatures. Temperatures entering the objective function are recorded by an infrared camera at the surface opposite to impinged one.