A simple procedure for the quantitative microdetermination of rhamnose

Summary A simple spectrophotometric procedure for microdetermination of rhamnose is described. It is based on breakdown of the sugar with sulphuric acid followed by treatment withp-hydroxydiphenyl. The coloured product is measured spectrophotometrically at 560 nm. A linear relationship exists between the amount of rhamnose (10-0g–) and the absorbance. The method is recommended for determination of rhamnose in samples containing rhamnose, different neutral sugars, amino-sugars, sugar alcohols, uronic acids, and muramic acid.

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Zusammenfassung Ein einfaches spektralphotometrisches Verfahren zur Mikrobestimmung von Rhamnose wurde beschrieben. Es beruht auf der Spaltung des Zuckers mit Schwefelsäure und nachfolgender Behandlung mit p-Hydroxydiphenyl. Das gefärbte Reaktionsprodukt wird spektralphotometrisch bei 560 nm gemessen. Die Extinktion steht mit der Rhamnosemenge in linearer Beziehung. Das Verfahren wird für die Rhamnosebestimmung in Proben empfohlen, die verschiedene Neutralzucker, Aminozucker, Zuckeralkohole, Uronsäuren und Muramsäure enthalten.

     

Enzymatically Extracted Apple Pectin Possesses Antioxidant and Antitumor Activity

The biological activity of apple pectin extracted conventionally or enzymatically using endo-xylanase and endo-cellulase, was tested in vitro. The analyses were performerd in tetraplicates and the statistical significance of the differences were assessed using ANOVA, Tukey post hoc and LSD (the least significant difference) tests. Multivariate regression analysis was applied to determine the structural components that have a crucial importance for antioxidant and antitumor properties of pectins. The pectins extracted by enzymes contained up to four times more ferulic acid and showed twice as great ability to neutralize free radicals and Fe(III) reduction. The antiradical potential positively correlated with phenols, fucose and rhamnose content. In the assays performed on HT-29 human adenocarcinoma and B16F10 melanoma cell cultures, the “green” pectins, contrary to acid isolated ones, exhibited remarkable anti-neoplastic potential while being nontoxic to nontransformed L929 cell line. The pectins in the dose of 1 mg/mL were capable of inhibiting adhesion (max 23.1%), proliferation (max 40.4%), invasion (max 76.9%) and anchorage-independent growth (max 90%) of HT-29 cells (significance level p < 0.001). These pectin preparations were slightly less active towards B16F10 cells. The enzyme-isolated apple pectins may be useful as a functional food additive and an ingredient of the ointment formulas for post-surgical melanoma treatment.     

Application of Deep Eutectic Solvents in the Synthesis of Substituted 2-Mercaptoquinazolin-4(3H)-Ones: A Comparison of Selected Green Chemistry Methods

In this study, deep eutectic solvents (DESs) were used as green and eco-friendly media for the synthesis of substituted 2-mercaptoquinazolin-4(3H)-ones from different anthranilic acids and aliphatic or aromatic isothiocyanates. A model reaction on anthranilic acid and phenyl isothiocyanate was performed in 20 choline chloride-based DESs at 80 °C to find the best solvent. Based on the product yield, choline chloride:urea (1:2) DES was found to be the most effective, while DESs acted both as solvents and catalysts. Desired compounds were prepared with moderate to good yields using stirring, microwave-assisted, and ultrasound-assisted synthesis. Significantly, higher yields were obtained with mixing and ultrasonication (16–76%), while microwave-induced synthesis showed lower effectiveness (13–49%). The specific contribution of this research is the use of DESs in combination with the above-mentioned green techniques for the synthesis of a wide range of derivatives. The structures of the synthesized compounds were confirmed by ¹H and ¹³C NMR spectroscopy.     

MSE-MRI sequence optimisation for measurement of bi- and tri-exponential T2 relaxation in a phantom and fruit

The transverse relaxation signal from vegetal cells can be described by multi-exponential behaviour, reflecting different water compartments. This multi-exponential relaxation is rarely measured by conventional MRI imaging protocols; mono-exponential relaxation times are measured instead, thus limiting information about of the microstructure and water status in vegetal cells. In this study, an optimised multiple spin echo (MSE) MRI sequence was evaluated for assessment of multi-exponential transverse relaxation in fruit tissues. The sequence was designed for the acquisition of a maximum of 512 echoes. Non-selective refocusing RF pulses were used in combination with balanced crusher gradients for elimination of spurious echoes. The study was performed on a bi-compartmental phantom with known T₂ values and on apple and tomato fruit. T₂ decays measured in the phantom and fruit were analysed using bi- and tri-exponential fits, respectively. The MRI results were compared with low field non-spatially resolved NMR measurements performed on the same samples.     

Prime Rings with Involution Equipped with Some New Product

Let R be a ring with involution *. We consider R as a ring equipped with a new product r s = rs + sr^*. The relationship between (ordinary) ideals of R and right ideals of R with respect to the product is studied.AMS Subject Classification (2000): 16W10, 16D25     

Stereoelectronic effects on 1H nuclear magnetic resonance chemical shifts in methoxybenzenes

Investigation of all O-methyl ethers of 1,2,3-benzenetriol and 4-methyl-1,2,3-benzenetriol (3-16) by 1H NMR spectroscopy and density-functional calculations disclosed practically useful conformational effects on 1H NMR chemical shifts in the aromatic ring. While the conversion of phenol (2) to anisole (1) causes only small positive changes of 1H NMR chemical shifts (Delta delta < 0.08 ppm) that decrease in the order Hortho > Hmeta > Hpara, the experimental O-methylation induced shifts in ortho-disubstituted phenols are largest for Hpara, Delta delta equals; 0.19 +/- 0.02 ppm (n = 11). The differences are due to different conformational behavior of the OH and OCH3 groups; while the ortho-disubstituted OH group remains planar in polyphenols due to hydrogen bonding and conjugative stabilization, the steric congestion in ortho-disubstituted anisoles outweighs the conjugative effects and forces the Ar-OCH3 torsion out of the ring plane, resulting in large stereoelectronic effects on the chemical shift of Hpara. Conformational searches and geometry optimizations for 3-16 at the B3LYP/6-31G** level, followed by B3LYP/6-311++G(2d,2p) calculations for all low-energy conformers, gave excellent correlation between computed and observed 1H NMR chemical shifts, including agreement between computed and observed chemical shift changes caused by O-methylation. The observed regularities can aid structure elucidation of partly O-methylated polyphenols, including many natural products and drugs, and are useful in connection with chemical shift predictions by desktop computer programs.     

Smart poly(2-hydroxyethyl methacrylate/itaconic acid) hydrogels for biomedical application

pH- and temperature-sensitive hydrogels, based on 2-hydroxyethyl methacrylate (HEMA) and itaconic acid (IA) copolymers, were prepared by γ-irradiation and characterized in order to examine their potential use in biomedical applications. The influence of comonomer ratio in these smart copolymers on their morphology, mechanical and thermal properties, biocompatibility and microbe penetration capability was investigated. The mechanical properties of copolymers were investigated using the dynamic mechanical analysis (DMA), while their thermal properties and morphology were examined by thermogravimetric analysis (TGA) and scanning electron microscopy (SEM). The morphology, mechanical and thermal properties of these hydrogels were found to be suitable for most requirements of biomedical applications. The in vitro study of P(HEMA/IA) biocompatibility showed no evidence of cell toxicity nor any considerable hemolytic activity. Furthermore, the microbe penetration test showed that neither Staphylococcus aureus nor Escherichia coli passed through the hydogel dressing; thus the P(HEMA/IA) dressing could be considered a good barrier against microbes. All results indicate that stimuli-responsive P(HEMA/IA) hydrogels have great potential for biomedical applications, especially for skin treatment and wound dressings.     

Phase equilibria and transformations in low-density polyethylene–<Emphasis Type="Italic">p</Emphasis>-xylene system

The state diagram of the low-density polyethylene–p-xylene system that contains the solubility curve of p-xylene in the polymer is first built using the optical method with the involvement of the DSC data. It has been shown that, at 72°C, in a blend with a polymer mass fraction of 0.28, the full amorphization of the polymer proceeds simultaneously with the dissolution of p-xylene in it. Blends with a lower polymer content are also homogenized at the same temperature, although the duration of this process can take several days. In blends with a high polymer content, homogenization occurs at a higher temperature. This process is preceded by the formation of microheterogeneous single-phase gel with network junctions as polymer crystallites and amorphous regions saturated by p-xylene. Cooling of the homogeneous blends to–20°С is not accompanied by the full separation of low- and high-molecular-mass phases; in this case p-xylene not only forms an individual crystalline phase, but also partially crystallizes in amorphous regions of the polymer.     

2-Substituted 2-Propenoic Acid Esters via Reaction of a Masked Acrylate Ester with Carbonyl Compounds

β-Amino ester enolate reacts readily with selected aldehydes and ketones. Deprotection via the N-oxide provides good yields of the 2-substituted acrylate ester.