High-performance liquid chromatography and thin-layer chromatography assays for Devil's Club (Oplopanax horridus)

Devil's root, Oplopanax horridus, is a widely used folk medicine in Alaska and British Columbia. The inner bark of the root and stem has been used to treat colds, cough, fever, and diabetes. The present study involves the development of high-pressure liquid chromatography (HPLC) and thin-layer chromatography (TLC) methods to detect the presence of trans-nerolidol and sterols in the root bark. The HPLC and TLC analytical methods presented are suitable for the characterization and identification of Oplopanax horridus.     

Surface characterization of recycled tire rubber to be used in cement paste matrix

The surface modification of tire rubber after treatment with saturated NaOH aqueous solution was investigated by HATR infrared analysis, potentiometric titration, and contact angle measurements. Infrared analysis of the powdered treated rubber showed a decrease in absorption at 1540, 1450, and 1395 cm(-1). This decrease is attributed to the removal of zinc stearate, an additive present in tire formulations that often migrates and diffuses to the surface, resulting in poor adhesion between the rubber and other materials. The potentiometric titration of the suspension of powdered rubber in 0.1 M NaCl showed that more hydrochloric acid was consumed by the untreated rubber, most likely a result of the hyrdrolysis of the zinc stearate to the organic acid. Contact angles of flat tire pieces showed an homogeneity enhancement of the treated rubber surface. The decrease of the zinc stearate on the treated rubber surface explains the improvement in the adhesion of this material to the cement matrix, observed in a previous research. The promising results of this study are a starting point for future research on incorporating rubber particles into cementitious materials as a means of successfully utilizing the vast amounts of tire waste currently in landfills.     

2-Phosphinophenolate complexes: formation and crystal structure of a novel trinuclear mu-O nickel(II)-tris(P(intersection)O-chelate)

A novel linear trinuclear mu-O-bridging 2-phosphinophenolate nickel(II) complex with fac-tris(P(intersection)O- chelates) in the terminal positions and the three oxygen atoms each facing the central nickel(II) cation was synthesized and structurally characterized by X-ray crystallography. To the best of our knowledge, this is the first example of an octahedral Ni(II) tris(P(intersection)O- chelate).     

Energetic ion bombardment of Ag surfaces by C<Stack><Subscript>60</Subscript><Superscript>+</Superscript></Stack> and Ga<Superscript>+</Superscript> projectiles

The ion bombardment-induced release of particles from a metal surface is investigated using energetic fullerene cluster ions as projectiles. The total sputter yield as well as partial yields of neutral and charged monomers and clusters leaving the surface are measured and compared with corresponding data obtained with atomic projectile ions of similar impact kinetic energy. It is found that all yields are enhanced by about one order of magnitude under bombardment with the C60+ cluster projectiles compared with Ga+ ions. In contrast, the electronic excitation processes determining the secondary ion formation probability are unaffected. The kinetic energy spectra of sputtered particles exhibit characteristic differences which reflect the largely different nature of the sputtering process for both types of projectiles. In particular, it is found that under C60+ impact (1) the energy spectrum of sputtered atoms peaks at significantly lower kinetic energies than for Ga+ bombardment and (2) the velocity spectra of monomers and dimers are virtually identical, a finding which is in pronounced contrast to all published data obtained for atomic projectiles. The experimental findings are in reasonable agreement with recent molecular dynamics simulations.     

Inductively coupled plasma compared with direct current arc spectrometry for analysis of minor elements in aluminium baths

A validation study was carried out in order to evaluate the efficiency of inductively coupled plasma-optical emission spectrometry (ICP-OES) for the analysis of minor elements (manganese, chromium, copper, iron, and titanium) in aluminium alloys. Aluminium casting samples were obtained by adding compressed powder compacts of each alloying element and aluminium (minitablets) to aluminum baths in a laboratory crucible furnace. Digestion of solid samples was performed using concentrated HCI and H202 35% (v/v) previous to analysis by ICP-OES without any matrix separation. This solution-based method was validated considering direct current arc spectrometry as the reference method based on direct analysis without any pretreatment of the solid samples considered. Univariate statistical procedures were carried out, for which precision <3% and trueness of the analytical results were taken into account.     

Diastereoselective synthesis of new psi[(E)-CH=CMe]- and psi[(Z)-CH=CMe]-type alkene dipeptide isosteres by organocopper reagents and application to conformationally restricted cyclic RGD peptidomimetics

Diastereoselective synthesis of new psi[(E)-CH=CMe]- and psi[(Z)-CH=CMe]-type alkene dipeptide isosteres corresponding to dipeptides having one N-methylamino acid, and application to bioactive peptides, are described. In a key reaction introducing the chiral alpha-alkyl group of the isosteres, organocopper-mediated alkylation of syn-beta-methylated gamma-mesyloxy-alpha,beta-enoate 26a afforded E- and Z-isomers of anti-S(N)2' products in a solvent-dependent manner. The resulting two isosteres, D-Phe-psi[(E)-CH=CMe]-L-Val 27a and D-Phe-psi[(Z)-CH=CMe]-L-Val 28b, which corresponded to trans- and cis-conformers of D-Phe-L-MeVal, respectively, were utilized in a structure-activity relationship study on cyclic RGD peptides 1 and 2, in company with a psi[(E)-CH=CH]-type alkene dipeptide isostere, D-Phe-psi[(E)-CH=CH]-L-Val. The cyclic isostere-containing pseudopeptides 3, 4, and 40 were synthesized and biological activity against integrin alpha(V)beta(3) and alpha(IIb)beta(3) receptors were also evaluated.     

Detection of processed genetically modified food using CIM monolithic columns for DNA isolation

The availability of sufficient quantities of DNA of adequate quality is crucial in polymerase chain reaction (PCR)-based methods for genetically modified food detection. In this work, the suitability of anion-exchange CIM (Convective Interaction Media; BIA Separations, Ljubljana, Slovenia) monolithic columns for isolation of DNA from food was studied. Maize and its derivates corn meal and thermally pretreated corn meal were chosen as model food. Two commercially available CIM disk columns were tested: DEAE (diethylaminoethyl) and QA (quaternary amine). Preliminary separations were performed with standard solution of salmon DNA at different pH values and different NaCl concentrations in mobile phase. DEAE groups and pH 8 were chosen for further isolations of DNA from a complex matrix-food extract. The quality and quantity of isolated DNA were tested on agarose gel electrophoresis, with UV-scanning spectrophotometry, and by amplification with real-time PCR. DNA isolated in this way was of suitable quality for further PCR analyses. The described method is also applicable for DNA isolation from processed foods with decreased DNA content. Furthermore, it is more effective and less time-consuming in comparison with the existing proposed methods for isolation of DNA from plant-derived foods.