Validation of the HS-GC-FID method for the determination of ethanol residue in tablets

This paper describes the validation of a HS-GC-FID method (based on the Pharmacopeia’s method) for the determination of ethanol content in tablets. A general view of the procedure development/optimization process is presented. The main point of this study is the calculation of validation parameters. Selectivity of the method was determined. Linearity (r > 0.997) was observed in the range from 9.0 to 3,040 μg of ethanol per sample (because the mass of the tablets used was around 200 mg, this corresponds to 45–15,200 μg g⁻¹). The method showed good recoveries (average 99.0%), and a relative standard deviation for repeatability and intermediate precision of 4.5% and 5.5% respectively. The limit of detection was calculated to be 3.0 μg of ethanol per sample (15 μg g⁻¹). The uncertainty budget was done according to the "Guide to the Expression of Uncertainty in Measurement" (GUM)[1], and a relative expanded uncertainty was estimated as 4.8%.     

Calixarenes in a membrane environment: a monolayer study on the miscibility of three p-tert-butylcalix[4]arene beta-lactam derivatives with 1,2-dimyristoyl-sn-glycero-3-phosphoethanolamine

Literature data indicate that some calixarene derivatives with antimicrobial activities may be useful as drugs; one of the aspects of the biological activity of different classes of antibiotics concerns interactions with lipid membranes. Here, the possibility of incorporation and/or translocation of three amphiphilic p-tert-butylcalix[4]arene derivatives across membranes was studied using lipid monolayers. The derivatives used have 6-aminopenicillanic acid or benzylpenicillin moieties grafted in alternate positions at the calixarene lower rim; 1,2-dimyristoyl-sn-glycero-3-phosphoethanolamine (DMPE), a model bacterial membrane lipid, was used to prepare the monolayers. The miscibility of calixarene-antibiotic conjugates with lipid films was studied using surface pressure and surface potential measurements, as well as Brewster angle microscopy. The results obtained show that the miscibility is significantly different for the 6-aminopenicillanic acid and the two benzylpenicillin derivatives. Molecular modeling allowed the assessment of the lowest energy conformations of the calixarene derivatives and gave more insight into the interactions with the DMPE films.     

Preliminary Studies Using Differential Scanning Calorimetry of Radiation-Induced Transformations in Starch and Flour

Differential scanning calorimetry was applied in studies of the effect of gamma irradiation on the potato starch and wheat flour. Essential differences were noticed between endothermal effects observed in concentrated suspensions of the initial and irradiated potato starch and wheat flour heated at a rate of 2.5°C min^-1, while only small differences were noticed between gelatinization thermal effects recorded for ca. 20% suspensions of the initial and irradiated potato starch samples heated at a rate 10°C min^-1. Moreover, in the case of wheat flour, a decrease of decomposition temperature of the amylose-lipid complex was concluded. This revised version was published online in August 2006 with corrections to the Cover Date.     

Rearrangement products of 3‐methane­sulfonyl‐N‐methyl‐N‐nitro­aniline

Two isomeric products (C₈H₁₀N₂O₄S) of the rearrangement of 3‐methane­sulfonyl‐N‐methyl‐N‐nitro­aniline have been investigated, viz. 3‐methane­sulfonyl‐N‐methyl‐2‐nitro­aniline, which was the main product of the rearrangement, and 5‐methane­sulfonyl‐N‐methyl‐2‐nitro­aniline. In both mol­ecules, the aromatic rings are appreciably deformed towards ortho‐quinonoidal geometry by electronic and steric interactions. The crystal structure is stabilized, in both cases, by weak C—H⋯O hydrogen bonds.     

ICP-MS Multi-Elemental Analysis of the Human Meninges Collected from Sudden Death Victims in South-Eastern Poland

Metals perform many important physiological functions in the human body. The distribution of elements in different tissues is not uniform. Moreover, some structures can be the site of an accumulation of essential or toxic metals, leading to multi-directional intracellular damage. In the nervous system, these disorders are especially dangerous. Metals dyshomeostasis has been linked to a variety of neurological disorders which end up leading to permanent injuries. The multi-elemental composition of the human brain is still the subject of numerous investigations and debates. In this study, for the first time, the meninges, i.e., the dura mater and the arachnoid, were examined for their elemental composition by means of inductively coupled plasma mass spectrometry (ICP-MS). Tissue samples were collected post mortem from those who died suddenly as a result of suicide (n = 20) or as a result of injuries after an accident (n = 20). The interactions between 51 elements in both groups showed mainly weak positive correlations, which dominated the arachnoid mater compared to the dura mater. The study showed differences in the distribution of some elements within the meninges in the studied groups. The significant differences concerned mainly metals from the lanthanide family (Ln), macroelements (Na, K, Ca, Mg), a few micronutrients (Co), and toxic cadmium (Cd). The performed evaluation of the elemental distribution in the human meninges sheds new light on the trace metals metabolism in the central nervous system, although we do not yet fully understand the role of the human meninges.     

Synthesis of Cyano-Benzylidene Xanthene Synthons Using a Diprotic Brønsted Acid Catalyst,and Their Application as Efficient Inhibitors of Aluminum Corrosion in Alkaline Solutions

Novel cyano-benzylidene xanthene derivatives were synthesized using one-pot and condensation reactions. A diprotic Brønsted acid (i.e., oxalic acid) was used as an effective catalyst for the promotion of the synthesis process of the new starting xanthene–aldehyde compound. Different xanthene concentrations (ca. 0.1–2.0 mM) were applied as corrosion inhibitors to control the alkaline uniform corrosion of aluminum. Measurements were conducted in 1.0 M NaOH solution using Tafel extrapolation and linear polarization resistance (LPR) methods. The investigated xanthenes acted as mixed-type inhibitors that primarily affect the anodic process. Their inhibition efficiency values were enhanced with inhibitor concentration, and varied according to their chemical structures. At a concentration of 2.0 mM, the best-performing studied xanthene derivative recorded maximum inhibition efficiency values of 98.9% (calculated via the Tafel extrapolation method) and 98.4% (estimated via the LPR method). Scanning electron microscopy (SEM) was used to examine the morphology of the corroded and inhibited aluminum surfaces, revealing strong inhibitory action of each studied compound. High-resolution X-ray photoelectron spectroscopy (XPS) profiles validated the inhibitor compounds’ adsorption on the Al surface. Density functional theory (DFT) and Monte Carlo simulations were applied to investigate the distinction of the anticorrosive behavior among the studied xanthenes toward the Al (111) surface. The non-planarity of xanthenes and the presence of the nitrile group were the key players in the adsorption process. A match between the experimental and theoretical findings was evidenced.     

Eigenvalues of model Hamiltonian matrices from spectral density distribution moments: The Heisenberg spin Hamiltonian

An approach aimed at approximating the extreme (the lowest and/or the highest) eigenvalues of matrices representing many-electron model Hamiltonians from a knowledge of several spectral density distribution moments is proposed. A detailed discussion of the Heisenberg spin Hamiltonian spectrum is presented as an example of an application. © 1996 John Wiley & Sons, Inc.     

Molecular modeling of phase behavior of polymer blends

Recent advances in the lattice cluster theory are applied to describe polymer blend miscibilities and variations with pressure. Extensive comparisons are made with experiment.     

An Evidence-Based Review of Application Devices for Nitric Oxide Concentration Determination from Exhaled Air in the Diagnosis of Inflammation and Treatment Monitoring

The measurement of nitric oxide (NO) in exhaled air is used in diagnostics and monitoring the pathologies not only in the respiratory system but also in the oral cavity. It has shown a huge increase in its level in asthma and diseases of the oral cavity. It seems reasonable to undertake research on the impact of inflammation on the level of NO in exhaled air. The aim of the study is to make an evidence-based review of the application of NO levels in exhaled air in the diagnosis of inflammation and treatment monitoring on the basis of selected measuring devices. Methods and Results: This paper presents an example of the application of NO measurement in exhaled air in individual human systems. Selected measuring devices, their non-invasiveness, and their advantages are described. Discussion: The usefulness of this diagnostic method in pathologies of the oral cavity was noted. Conclusions: Measuring the level of NO in exhaled air seems to be a useful diagnostic method.