Coordination of the natural ligand lapachol to iron(II): synthesis,theoretical study and antiproliferative activity

Transition Metal Chemistry - Lapachol is a natural naphthoquinone known for having a variety of biological properties, and in recent years, it has been used in the synthesis of metal complexes with...     

Cannabidiol Discovery and Synthesis—a Target-Oriented Analysis in Drug Production Processes

The current state of evidence and recommendations for cannabidiol (CBD) and its health effects change the legal landscape and aim to destigmatize its phytotherapeutic research. Recently, some countries have included CBD as an antiepileptic product for compassionate use in children with refractory epilepsy. The growing demand for CBD has led to the need for high-purity cannabinoids on the emerging market. The discovery and development of approaches toward CBD synthesis have arisen from the successful extraction of Cannabis plants for cannabinoid fermentation in brewer's yeast. To understand different contributions to the design and enhancement of the synthesis of CBD and its key intermediates, a detailed analysis of the history behind cannabinoid compounds and their optimization is provided herein.     

Ceramic glaze analysis by simultaneous in-beam PGAA and XRFS

Twenty-one ready-to-use hobby glazes, of which 18 were labeled safe for food containers (SFFC), were analyzed for Al, B, Ba, Ca, Cd, Co, Cr, Cu, Fe, Gd, Hf, K, Mn, Na, Pb, Si, Sm, Sr, Ti, Zn, and Zr by neutron capture prompt -ray activation analysis (PGAA). Simultaneously, Pb was also determined by X-ray fluorescence spectrometry (XRFS) using Pb K X-rays induced by the -ray component of the neutron beam. The XRFS limits of detection were 200–400 g Pb·g^–1 (dry weight), a factor of 100 better than those for PGAA. Pb concentrations (by dry weight; with weight losses ranging from 28 to 49% after air-drying) found were 0.16–27.2% in the SFFC glazes and 0.86–32% in the other glazes. The SFFC glazes contained from <0.6 to 202 g Cd·g^–1, and Co, Cr, and Cu (elements which may enhance Pb leaching from fired glazes) were found in concentrations up to 1.2, 2.7, and 5.6%, respectively. Method accuracy was demonstrated with the analysis of soil, fly ash, and glass standard reference materials.     

Alternative approach to enhancing cation selectivity in ion chromatography

A new approach to enhance cation selectivity in ion chromatography (IC) is described. Two packings, one carrying a conventional carboxylate cation exchanger and the other carrying a crown ether (CE) phase are packed into two separate columns and used in series. The resolution between sodium and ammonium and between ammonium and potassium is increased significantly. The two stationary phases may also be mixed and packed into a single column. The selectivity of the cations can be adjusted easily by varying the dimensions of the carboxylate and CE columns (in the two-column configuration), or by changing the ratio of the carboxylate cation exchanger to the CE packing (in the single-column configuration). These new systems separate ammonium and sodium, even when the sodium concentration is 5000 times higher. Amines such as ethanolamine and triethanolamine can also be separated from the alkali and alkaline-earth cations.     

TRANSMITTANCE OF NONIONIZING RADIATION IN HUMAN TISSUES*

Abstract— Spectral transmittance of 400–865 nm radiation through various human structures, including the skull with scalp, the chest wall, abdominal wall and scrotum, is presented. There is essentially no visible light of wavelengths shorter than 500 nm transmitted through the chest or the abdominal wall. In contrast, 10^?5–10^?4 of blue light can reach the brain and testes. Transmittance of all tissues increases progressively with wavelength from 600 to 814nm. The maximal transmittances are 10^?2–10^?1 for skulls and scrota, and 10^?3–10^?2 for chest and abdominal walls. Tissue thickness, optical absorption and scattering are major influencing factors.     

Chemistry and insulin-mimetic properties of bis(acetylacetonate)oxovanadium(IV) and derivatives

The syntheses and the solid state structural and spectroscopic solution characterizations of VO(Me-acac)2 and VO(Et-acac)2 (where Me-acac is 3-methyl-2,4-pentanedionato and Et-acac is 3-ethyl-2,4-pentanedionato) have been conducted since both VO(acac)2 and VO(Et-acac)2 have long-term in vivo insulin-mimetic effects in streptozotocin-induced diabetic Wistar rats. X-ray structural characterizations of VO(Me-acac)2 and VO(Et-acac)2 show that both contain five-coordinate vanadium similar to the parent VO(acac)2. The unit cells for VO(Et-acac)2 and VO(Me-acac)2 are both triclinic, P1, with a = 9.29970(10) A, b = 13.6117(2) A, c = 13.6642(2) A, alpha = 94.1770(10) degrees, beta = 106.4770(10) degrees, gamma = 106.6350(10) degrees for VO(Et-acac)2 and a = 7.72969(4) A, b = 8.1856(5) A, c = 11.9029(6) A, alpha = 79.927(2) degrees, beta = 73.988(2)degrees, gamma = 65.1790(10)degrees for VO(Me-acac)2. The total concentration of EPR-observable vanadium(IV) species for VO(acac)2 and derivatives in water solution at 20 degreesC was determined by double integration of the EPR spectra and apportioned between individual species on the basis of computer simulations of the spectra. Three species were observed, and the concentrations were found to be time, pH, temperature, and salt dependent. The three complexes are assigned as the trans-VO(acac)2.H2O adduct, cis-VO(acac)2.H2O adduct, and a hydrolysis product containing one vanadium atom and one R-acac- group. The reaction rate for conversion of species was slower for VO(acac)2 than for VO(malto)2, VO(Et-acac)2, and VO(Me-acac)2; however, in aqueous solution the rates for all of these species are slow compared to those of other vanadium species. The concentration of vanadium(V) species was determined by 51V NMR. The visible spectra were time dependent, consistent with the changes in species concentrations that were observed in the EPR and NMR spectra. EPR and visible spectroscopic studies of solutions prepared as for administration to diabetic rats documented both a salt effect on speciation and formation of a new halogen-containing complex. Compound efficacy with respect to long-term lowering of plasma glucose levels in diabetic rats traces the concentration of the hydrolysis product in the administration solution.     

Fingerprinting bacterial strains using ion mobility spectrometry

Ion mobility spectrometry (IMS) is currently in widespread use for the detection and identification of narcotic and explosive compounds without prior sample clean-up or concentration steps. IMS analysis is rapid, less than a minute, and sensitive, with detection limits in the nanogram to picogram range, depending on the target analyte. Our studies indicate that this technique has potential for detection of specific components of bacterial cells and for identification and differentiation of bacterial strains and species within a minute, and with no specialized test kits or reagents required. When microgram quantities of whole bacterial cells are thermally desorbed, complex positive or negative ion patterns (plasmagrams) are obtained. These plasmagrams differ reproducibly for different strains and species and for different conditions of growth, and can be used for the classification and differentiation of specific strains and species of bacteria, including pathogens. Methods for improved ion peak detection, most notably sequential sample desorption at stepped increases in temperature (programmed temperature ramping), are described.     

Novel Experimental Method to Determine the Cutting Effectiveness of Grinding Grits

This work presents a novel experimental apparatus to determine the cutting effectiveness of grinding grits. The apparatus consists of a custom high-speed scratch tester, a force measurement system, and an offline 3D optical profilometer. Preliminary results based on a spherical tool are presented to demonstrate the usefulness of the system. Experiments were performed at depths of cut ranging from 0.3 μm to 7.5 μm at cutting speeds of 5 m/s to 30 m/s in 5 m/s increments. High resolution scans of the scratch profiles provided insight into the change in the cutting mechanics as the depth of cut and cutting speed were increased. In general, lower cutting speeds produced higher pile-up heights while higher cutting speeds produced lower pile-up heights. The force measurements indicated that the normal forces increased with cutting speed due to strain rate hardening of the workpiece material while the tangential forces decreased with cutting speed due to a reduction in the coefficient of friction and a change in the cutting mechanics. The force ratio data and the specific energy data both demonstrated high slopes at low depths of cut due to asperity contact between the tool and the workpiece. The modular nature of the developed system allows different grit geometries to be investigated.     

In vitro inhibition of protein glycation and advanced glycation end products formation by hydroethanolic extract and two fractions of Simaba trichilioides roots

Abstract

Long-term hyperglycemia maintenance is responsible for increased protein glycation and formation of advanced glycation end products (AGEs), both are associated with the onset of diabetes mellitus complications. Efforts have been made to discover new agents having antiglycation potential. The aim of this study was to investigate the effects of the hydroethanolic extract and the ethyl acetate and methanolic fractions of Simaba trichilioides roots on the formation of AGEs. In an in vitro model system of protein glycation, incubations with hydroethanolic extract, ethyl acetate or methanolic fractions of S. trichilioides decreased the fluorescent AGEs, and markers of tyrosine and tryptophan oxidation. Protein crosslinking was reduced in the presence of the ethyl acetate fraction of S. trichilioides. Simaba trichilioides roots seem to be a promising source of compounds having ability to prevent glycoxidation changes, with potential applications in complementary therapies for management of diabetic complications.     

Studies into diastereoselective Dötz benzannulations for the synthesis of axially chiral biaryls

A series of racemic chiral ortho substituents on 1-phenylhex-1-yne have been found to control the atroposelective formation of a biaryl from Dötz benzannulation with pentacarbonyl(methoxyphenylmethylene)chromium(0). The results show there is a subtle balance between the chiral ortho substituent controlling atroposelectivity with a dr 3-5:1 and allowing benzannulation to proceed in yields of 44-67%.