Unusual solid-state conformation of D-glucitol hexa(p-chlorobenzoate)

The carbon atom chain in the molecule ofd-glucitol hexa (p-chlorobenzoate) adopts a planar, zigzag conformation in the solid state, as determined by X-ray crystallography. The preference for such conformation in the crystal can be ascribed to the stacking interactions in which an infinite number of p-chlorobenzoyloxy substituents is involved.     

Thermal Decomposition of Bi(III), Cd(II), Pb(II) and Cu(II) Thiocyanates

Thermal decomposition of Bi(SCN)₃, Cd(SCN)₂, Pb(SCN)₂ and Cu(SCN)₂ has been studied. The thermal analysis curves and the diffraction patterns of the solid intermediate and final products of the pyrolysis are presented. The gaseous products of the decomposition (SO₂ and CO₂) were detected and quantitatively determined. Thermal, X-ray and chemical analyses have been used to establish the nature of the reactions occurring at each stage in the decomposition.This revised version was published online in November 2005 with corrections to the Cover Date.     

Syntheses with organoboranes. IX. Vinyl- and 1-alkenyldichloroboranes as ethylene and 1-alkene equivalents for the Diels–Alder reaction

Vinyl- and 1-alkenyldichloroboranes were used as dienophiles for the Diels–Alder reaction with representative aliphatic and cyclic 1,3-dienes. The organoborane adducts were transformed into the corresponding olefins either by protonolysis or by oxidation–mesylation–reduction. Direct protonolysis of the adducts gave in most cases mixtures of olefins whereas the reduction of mesylates with lithium triethylborohydride produced pure olefins in good yields.     

Partial transposition and nonextendible maps

The wide class of nonextendible positive maps inC ^*-algebras [1, 3] is studied. An example is given showing that the set of nonextendible positive maps betweenC ^*-algebras and is not closed inL( ) in the weak topology.     

Laser-Rf double-resonance studies of the hyperfine structure of metastable atomic states of55Mn

The hyperfine structure (hfs) of the metastable atomic states 3d⁶4s⁶ D _{1/2, 3/2, 5/2, 7/2, 9/2} of⁵⁵Mn was measured using theABMR- LIRF method (atomicbeammagneticresonance, detected bylaserinducedresonancefluorescence). The hfs constantsA andB, corrected for second order hfs perturbations, could be derived from these measurements. The theoretical interpretation of these correctedA- andB-factors was performed in the intermediate coupling scheme taking into account the configurations 3d ⁵4s ², 3d ⁶4s and 3d ⁷. Examining the influence of the composition of the eigenvectors on the hfs parameters \(\left\langle {r^{ - 3} } \right\rangle ^{k_s k_l } \) it was found, that for the configuration 3d ⁶4s the two-body magnetic interaction should be considered in the calculation of the eigenvectors. Investigating second order electrostatic configuration interactions and relativistic effects and using calculated relativistic correction factors we obtained for the nuclear quadrupole moment of the nucleus⁵⁵Mn a value ofQ=0.33(1) barn, which is not perturbed by a shielding or antishielding Sternheimer factor. The following hfs constants have been obtained: $$\begin{gathered} A\left( {{1 \mathord{\left/ {\vphantom {1 2}} \right. \kern-\nulldelimiterspace} 2}} \right) = 882.056\left( {12} \right)MHz \hfill \\ A\left( {{3 \mathord{\left/ {\vphantom {3 2}} \right. \kern-\nulldelimiterspace} 2}} \right) = 469.391\left( 7 \right)MHzB\left( {{3 \mathord{\left/ {\vphantom {3 2}} \right. \kern-\nulldelimiterspace} 2}} \right) = - 65.091\left( {50} \right)MHz \hfill \\ A\left( {{5 \mathord{\left/ {\vphantom {5 2}} \right. \kern-\nulldelimiterspace} 2}} \right) = 436.715\left( 3 \right)MHzB\left( {{5 \mathord{\left/ {\vphantom {5 2}} \right. \kern-\nulldelimiterspace} 2}} \right) = - 46.769\left( {30} \right)MHz \hfill \\ A\left( {{7 \mathord{\left/ {\vphantom {7 2}} \right. \kern-\nulldelimiterspace} 2}} \right) = 458.930\left( 3 \right)MHzB\left( {{7 \mathord{\left/ {\vphantom {7 2}} \right. \kern-\nulldelimiterspace} 2}} \right) = 21.701\left( {40} \right)MHz \hfill \\ A\left( {{9 \mathord{\left/ {\vphantom {9 2}} \right. \kern-\nulldelimiterspace} 2}} \right) = 510.308\left( 8 \right)MHzB\left( {{9 \mathord{\left/ {\vphantom {9 2}} \right. \kern-\nulldelimiterspace} 2}} \right) = 132.200\left( {120} \right)MHz \hfill \\ \end{gathered} $$      

Einfluß der Vibration auf die Geschwindigkeit der Saccharosekristallisation

The influence of the vibration amplitude on the crystallization rate of saccharose with constant vibration frequency of 100 Hz is investigated. Supersaturation was low (1.05), temperatures 40, 60, and 80 °C. Increase of amplitudes 1 up to 4 mm positively influenced the crystallization rate (by 45%) in solutions of high purity and low temperature. At 80 °C the increase lay at about 20%. With low purity solutions no acceleration was observed. – The apparatus and methods of measuring are described.     

Cornelian Cherry (Cornus mas L.) Extracts Exert Cytotoxicity in Two Selected Melanoma Cell Lines—A Factorial Analysis of Time-Dependent Alterations in Values Obtained with SRB and MTT Assays

Despite the fact that phytochemicals of Cornaceae species have long been discussed as possible auxiliary agents in contemporary treatment, the insights on their properties remain relatively scarce. This study focuses on Cornus mas L. (Cornelian cherry), the extracts of which are reported to exert a pleiotropic effect shown in both in vivo and in vitro studies. This study aimed to explore the cytotoxic effect of extracts from fruits of red (Cornus mas L. ‘Podolski’) and yellow (Cornus mas L. ‘Yantarnyi’ and ‘Flava’) Cornelian cherries on two melanoma cell lines (A375 and MeWo). The extracts were characterized in the context of the concentration of bioactive compounds of antioxidative properties. Cytotoxicity was investigated with the use of the following two assays: SRB and MTT. An additional, alternative protocol for the SRB assay was used in this study so as to account for possible bias. Cytotoxicity was assessed as a difference in the whole time series of cell viability, instead of analyzing differences in raw values (often found in the literature). Both extracts from Cornus mas L. induced cytotoxicity in both A375 and MeWo cell lines, although the response of these cells was different. Moreover, based on this study, there is no evidence for claiming a different magnitude of cytotoxicity between these two extracts.     

Acrylamide-Derived Ionome,Metabolic, and Cell Cycle Alterations Are Alleviated by Ascorbic Acid in the Fission Yeast

Acrylamide (AA), is a chemical with multiple industrial applications, however, it can be found in foods that are rich in carbohydrates. Due to its genotoxic and cytotoxic effects, AA has been classified as a potential carcinogen. With the use of spectrophotometry, ICP-OES, fluorescence spectroscopy, and microscopy cell growth, metabolic activity, apoptosis, ROS production, MDA formation, CAT and SOD activity, ionome balance, and chromosome segregation were determined in Schizosaccharomyces pombe. AA caused growth and metabolic activity retardation, enhanced ROS and MDA production, and modulated antioxidant enzyme activity. This led to damage to the cell homeostasis due to ionome balance disruption. Moreover, AA-induced oxidative stress caused alterations in the cell cycle regulation resulting in chromosome segregation errors, as 4.07% of cells displayed sister chromatid non-disjunction during mitosis. Ascorbic acid (AsA, Vitamin C), a strong natural antioxidant, was used to alleviate the negative impact of AA. Cell pre-treatment with AsA significantly improved AA impaired growth, and antioxidant capacity, and supported ionome balance maintenance mainly due to the promotion of calcium uptake. Chromosome missegregation was reduced to 1.79% (44% improvement) by AsA pre-incubation. Results of our multiapproach analyses suggest that AA-induced oxidative stress is the major cause of alteration to cell homeostasis and cell cycle regulation.     

DSC,FT-IR and NIR with Chemometric Assessment Using PCA and HCA for Estimation of the Chemical Stability of Oral Antidiabetic Drug Linagliptin in the Presence of Pharmaceutical Excipients

Pharmaceutical excipients should not interact with active substances, however, in practice, they sometimes do it, affecting the efficacy, stability and safety of drugs. Thus, interactions between active substances and excipients are not desirable. For this reason, two component mixtures of oral antidiabetic drug linagliptin (LINA) with four excipients of different reactivity, i.e., lactose (LAC), mannitol (MAN), magnesium stearate (MGS) and polyvinylpyrrolidone (PVP), were prepared in a solid state. A high temperature and a high humidity of 60 °C and 70% RH, respectively, were applied as stressors in order to accelerate the potential interactions between LINA and excipients. Differential scanning calorimetry (DSC) as well as Fourier transform infrared (FT-IR) and near infrared (NIR) spectroscopy were used to estimate the changes due to potential interactions. In addition, chemometric computation of the data with principal component analysis (PCA) and hierarchical cluster analysis (HCA) was applied to adequately interpret the findings. Of the excipients used in the present experiment, all of them were not inert in relation to LINA. Some of the interactions were shown without any stressing, whereas others were observed under high-temperature/high-humidity conditions. Thus, it could be concluded that selection of appropriate excipients for LINA is very important question to minimize its degradation, especially when new types of formulations with LINA are being developed and manufactured.     

Biochemical and Molecular Investigation of the Effect of Saponins and Terpenoids Derived from Leaves of Ilex aquifolium on Lipid Metabolism of Obese Zucker Rats

Ilex paraguariensis, the holly tree, is a plant with recognized biological properties, whose aqueous infusions are known as “Yerba mate”, that regulate lipid metabolism, reduce obesity, and improve brain stimulation. In the present study, the effect of standardized saponin and terpenoid fractions of a European taxon, Ilex aquifolium, on blood biochemical parameters in a rat model of metabolic disorder, (fa/fa) Zucker, are presented. The profiles of the volatile fractions of two species and six European varieties of Ilex were investigated. After selecting the best variety, the saponin and terpenoid fractions were isolated and standardized, and animals were fed 10 mg kg⁻¹ b.w. for 8 weeks. A statistically significant decrease in liver adiposity was observed, confirmed by histology and quantitative identification (gas chromatography–mass spectrometry analyses of hepatic lipids. RT-qPCR analysis of gene expression in the aorta revealed that the administration of the terpenoid fraction downregulated LOX-1, suggesting a reduction in atherosclerotic stimuli. In addition, a statistically significant reduction (p < 0.05) in PPARγ for the saponin fraction was observed in the liver. The expression of the ACAT-1 gene in the liver, responsible for the formation of cholesterol esters, increased significantly in the group receiving the terpenoid fraction compared to the control, which was also confirmed by the analysis of individual blood biochemical parameters. The opposite effect was observed for saponins. Taking the above into account, it is shown for the first time that Ilex aquifolium can be a source of compounds that positively influence lipid metabolism.