Rotation Planar Extraction and Medium-Pressure Solid—Liquid Extraction of Onion (Allium cepa)

JPC – Journal of Planar Chromatography – Modern TLC - Extraction of onion (Allium cepa L.) with 80:20 (v/v) methanol—water in water by rotation planar extraction (RPE) and medium-...     

Formation and hydrolysis of gas‐phase [UO2(R)]+: R═CH3, CH2CH3, CH═CH2, and C6H5

The goals of the present study were (a) to create positively charged organo‐uranyl complexes with general formula [UO₂(R)]⁺ (eg, R═CH₃ and CH₂CH₃) by decarboxylation of [UO₂(O₂C─R)]⁺ precursors and (b) to identify the pathways by which the complexes, if formed, dissociate by collisional activation or otherwise react when exposed to gas‐phase H₂O. Collision‐induced dissociation (CID) of both [UO₂(O₂C─CH₃)]⁺ and [UO₂(O₂C─CH₂CH₃)]⁺ causes H⁺ transfer and elimination of a ketene to leave [UO₂(OH)]⁺. However, CID of the alkoxides [UO₂(OCH₂CH₃)]⁺ and [UO₂(OCH₂CH₂CH₃)]⁺ produced [UO₂(CH₃)]⁺ and [UO₂(CH₂CH₃)]⁺, respectively. Isolation of [UO₂(CH₃)]⁺ and [UO₂(CH₂CH₃)]⁺ for reaction with H₂O caused formation of [UO₂(H₂O)]⁺ by elimination of ·CH₃ and ·CH₂CH₃: Hydrolysis was not observed. CID of the acrylate and benzoate versions of the complexes, [UO₂(O₂C─CH═CH₂)]⁺ and [UO₂(O₂C─C₆H₅)]⁺, caused decarboxylation to leave [UO₂(CH═CH₂)]⁺ and [UO₂(C₆H₅)]⁺, respectively. These organometallic species do react with H₂O to produce [UO₂(OH)]⁺, and loss of the respective radicals to leave [UO₂(H₂O)]⁺ was not detected. Density functional theory calculations suggest that formation of [UO₂(OH)]⁺, rather than the hydrated U^VO₂⁺, cation is energetically favored regardless of the precursor ion. However, for the [UO₂(CH₃)]⁺ and [UO₂(CH₂CH₃)]⁺ precursors, the transition state energy for proton transfer to generate [UO₂(OH)]⁺ and the associated neutral alkanes is higher than the path involving direct elimination of the organic neutral to form [UO₂(H₂O)]⁺. The situation is reversed for the [UO₂(CH═CH₂)]⁺ and [UO₂(C₆H₅)]⁺ precursors: The transition state for proton transfer is lower than the energy required for creation of [UO₂(H₂O)]⁺ by elimination of CH═CH₂ or C₆H₅ radical.     

Syntheses of 3-, 4-, and 5-O-feruloylquinic acids

The efficient synthesis of 3-, 4-, and 5-O-feruloylquinic acids starting from d-(?)-quinic acid is described. Esterification of suitably protected quinic acid derivatives with 3-(4-acetoxy-3-methoxyphenyl)-acryloyl chloride and subsequent hydrolysis of all the protecting groups afforded the title products in overall yields of 33%, 15%, and 45%, respectively, (from quinic acid).     

Reactions of Dimethyl Carbonate with Aliphatic Amines Under High Pressure

A facile synthesis of methyl carbamates from primary amines and dimethyl carbonate has been achieved at room temperature using high pressure. High-pressure synthesis of methyl carbamates described herein provides access to the target molecules in an efficient and environmentally friendly way without solvent or catalyst. Better conversion and selectivity than previously published procedures were obtained.

The possibilities of voltammetry in the study reactivity of dissolved organic carbon (DOC) in natural waters

Journal of Solid State Electrochemistry - This paper describes the application of a methodology, which primarily involves low-cost voltammetry, to rapidly track the reactivity (i.e. surfactant...     

Synthesis and structure of novel 4-arylhexahydro-1H,3H-pyrido[1,2-c]pyrimidine derivatives

A series of new 4-aryl-hexahydro-1H,3H-pyrido[1,2-c]pyrirnidine-1,3-dione derivatives 4a-k were prepared by catalytic hydrogenation of 4-aryl-1H,2H-pyrido[1,2-c]pyrirnidine-1,3-diones 3a-k. The structures of compounds were determined by ¹H and ¹³C nmr spectroscopy in solution. Steric hindrance caused twisting of the phenyl ring with respect to the pyridopyrimidine system, the effect was confirmed by X-ray diffraction.     

Monitoring of biogenic amines and drugs of various therapeutic groups in urine samples with use of HPLC

A high‐performance liquid chromatography method for simultaneous separation and determination of biogenic amines [dopamine, epinephrine, serotonin and its six metabolites (normetanephrine, metanephrine, 3,4‐dihydroxyphenylacetic acid, 4‐hydroxy‐3‐methoxyphenylglycol, homovanilic acid and 5‐hydroxyindoloacetic acid)] with drugs from different therapeutically groups [analgesics (paracetamol, metamizol), diuretics (furosemide) and antibiotics (cefazolin, fluconazole)] was developed. A chromatographic column with pre‐column with octadecylsilane phase (C_18e) and two detectors – diode array serial connected and fluorescence – was used. Gradient elution of mixture of acetate buffer (pH 4.66) and methanol as a mobile phase was applied. The limit of detection (LOD) of 8–10 ng/mL and limit of quantitation (LOQ) of 24–30 ng/mL for biogenic amines, as well as the LOD of 50–100 ng/mL and the LOQ of 150–300 ng/mL for drugs, were determined. The applied sample preparation method allowed recoveries of 93% for the biogenic amines and 92% for the drugs to be achieved. The developed procedure has been applied to simultaneous determination of the examined compounds in urine samples and could be used in clinical analysis. Copyright © 2015 John Wiley & Sons, Ltd.     

Solution behaviour of a formate capped surfactant—the oxidation product of an alcohol ethoxylate

The solution behaviour has been investigated for an alcohol ethoxylate terminated with a formic acid ester. This compound has previously been reported to be an important degradation product in the auto-oxidation of alcohol ethoxylates. In this work we have investigated the solution behaviour of the formic acid ester surfactant C₁₂H₂₅(OCH₂CH₂)₄OCHO (C12E4---OCHO). The pure formate was found to be sparsely soluble in water with no clear point at 0.1%. The critical micelle concentration was found to be 129 μM at 35°C, compared to 50 μM for the parent surfactant C₁₂H₂₅(OCH₂CH₂)₅OH (C12E5). To mimic the behaviour of the oxidised surfactant, the formate was mixed in different ratios with C12E5 and the cloud point, surface tension and critical micelle concentration (cmc) of these mixtures were studied. The gradual increase of formate was found to shift the cloud point and isotropic regions to lower temperatures. The cmc of the mixture was found to be lower than for the pure surfactant. The favourable interaction was analysed according to the non-ideal model by Rubingh and the interaction parameter, β, was determined to be −4±0.53, which is unusually large for a mixture of two non-ionic surfactants. These results indicate that the reduction of cloud point observed during oxidation of non-ionic surfactants can in part be attributed to the formation of formate esters.     

Changes of 1,2,4-Triazole Retention and Lipophilicity Descriptor Values in RP-TLC and MLC–TLC Systems in the Presence of an External Magnetic Field

JPC – Journal of Planar Chromatography – Modern TLC - As it was shown in earlier experiments, magnetic field can influence various processes taking part in nature. One of them might be...     

Preparation and properties of textile materials modified with triclosan‐loaded polylactide microparticles

A convenient and simple method for preparation of commercial nonwovens with antimicrobial properties was elaborated. The process consists in preparation of poly(l ‐lactide) microspheres (from poly(l ‐lactide) with M _n  = 10,560 and M _w /M _n  = 1.39) containing triclosan (5‐chloro‐2‐(2,4‐dichlorophenoxy) phenol) and loading them onto the nonwovens. The microspheres were prepared by spray drying (D _n  = 3.91 μm, D _w /D _n  = 2.43) and oil‐in‐water emulsification‐solvent evaporation method (D _n  = 5.84 μm, D _w /D _n  = 1.25). Content of triclosan in microspheres ranged from 4.65 to 4.95 wt%. The antibacterial nonwovens were prepared by padding of the fibers with the microspheres using the microsphere suspension. The resulting antibacterial nonwovens were examined using inhibition zone measurement method. Inhibition zones from 4 to 9 mm indicated that the modified nonwovens had antibacterial properties against Gram (+)—Staphylococcus aureus and Gram (?)—Klebsiella pneumoniae . Nonwovens were conditioned up to 12 months at relative humidity <5%, 50%, and 100% in desiccators and up to 6 months air‐conditioning system at relative humidity = 65%. Antimicrobial activity of the modified nonwovens was examined as a function of time and air humidity. Time of conditioning has strong influence on antibacterial activity, whereas the impact of the air humidity was negligible. All nonwovens had antibacterial properties even after 12 months of conditioning. Copyright © 2017 John Wiley & Sons, Ltd.