Synthesis of enantiopure imidazolines through a Ritter reaction of 2-(1-aminoalkyl)aziridines with nitriles

The Ritter reaction of enantiopure 2-(1-aminoalkyl)aziridines 1 with different nitriles afford enantiopure tetrasubstituted imidazolines 2. The opening of the aziridine ring takes place with total regio- and stereoselectivity. A mechanism to explain the described addition reaction is proposed. [reaction: see text]     

Stereoselective synthesis of functionalized gamma-amino esters: azetidinium salts and epoxy esters

Addition of several lithium ester enolates to chiral 1-aminoalkyl chloromethyl ketones 1 affords enantiomerically pure 3-hydroxyazetidinium salts 3 or 3-(1'-aminoalkyl)-3,4-epoxy esters 4, depending on the reaction conditions. [reaction: see text]     

Analysis of human transferrin glycopeptides by capillary electrophoresis and capillary liquid chromatography-mass spectrometry. Application to diagnosis of alcohol dependence

In this study, capillary electrophoresis and capillary liquid chromatography coupled to mass spectrometry (CE-TOF-MS and μLC-TOF-MS) were used to detect and characterise human transferrin (Tf) glycopeptide glycoforms obtained by tryptic digestion. After selecting μLC-TOF-MS because of improved performance in analysis of N₄₁₃ and N₆₁₁ glycopeptide glycoforms, the proposed methodology was applied to serum samples. Two immunoaffinity columns were employed to isolate Tf from serum samples. Both columns were activated with the same anti-Tf antibody but using two different bonding chemistries. After immunoaffinity purification and digestion, serum samples from a teetotal individual (as control) and from individuals with low and high alcohol dependence were analysed by μLC-TOF-MS. Relative abundance of each glycoform was useful to estimate the degree of alcohol dependence of each individual. Finally, the established methodology was used to analyse serum samples from specific individuals with an unknown degree of alcohol dependence.     

Hibiscus Acid from Hibiscus sabdariffa L. Inhibits Flagellar Motility and Cell Invasion in Salmonella enterica

Extracts of Hibiscus sabdariffa L. (commonly called Rosselle or “Jamaica flower” in Mexico) have been shown to have antibiotic and antivirulence properties in several bacteria. Here, an organic extract of H. sabdariffa L. is shown to inhibit motility in Salmonella enterica serovars Typhi and Typhimurium. The compound responsible for this effect was purified and found to be the hibiscus acid. When tested, this compound also inhibited motility and reduced the secretion of both flagellin and type III secretion effectors. Purified hibiscus acid was not toxic in tissue-cultured eukaryotic cells, and it was able to reduce the invasion of Salmonella Typhimurium in epithelial cells. Initial steps to understand its mode of action showed it might affect membrane proton balance.     

A natural selection from the core of a TU game: the core-center

We present a new allocation rule for the class of games with a nonempty core: the core-center. This allocation rule selects a centrally located point within the core of any such game. We provide a deep discussion of its main properties.     

Possibilities and limitations of the sequential injection chromatography technique for the determination of anticoccidial agents in water, pharmaceutical formulations and feed

This paper explores the potential of applying reversed-phase sequential injection chromatography (SIC) to determine the anticoccidial agents Lasalocid and Toltrazuril in various matrices including ground water, pharmaceutical formulations and feed. SIC was performed by connecting a 25 × 4.6 mm monolithic C18 column to a 2 m long pathlength capillary flow cell, where the usage of a flow cell lowers the detection limit compared to a conventional short-distance flow cell, providing a simple detection system for these two compounds which are initially poorly UV absorbents.The proposed set-up provides a high injection throughput of 12 h^{− 1}, as well as a limit of detection of 0.019 and 0.010 mg/L for Toltrazuril and Lasalocid, respectively. The repeatabilities obtained (n = 10) were lower than 2% and 4% for Toltrazuril and Lasalocid, respectively.     

Chip-Based Spectrofluorimetric Determination of Iodine in a Multi-Syringe Flow Platform with and without In-Line Digestion—Application to Salt,Pharmaceuticals, and Algae Samples

In this work, a flow-based spectrofluorimetric method for iodine determination was developed. The system consisted of a miniaturized chip-based flow manifold for solutions handling and with integrated spectrofluorimetric detection. A multi-syringe module was used as a liquid driver. Iodide was quantified from its catalytic effect on the redox reaction between Ce(IV) and As(III), based on the Sandell–Kolthoff reaction. The method was applied for the determination of iodine in salt, pharmaceuticals, supplement pills, and seaweed samples without off-line pre-treatment. An in-line oxidation process, aided by UV radiation, was implemented to analyse some samples (supplement pills and seaweed samples) to eliminate interferences and release iodine from organo-iodine compounds. This feature, combined with the fluorometric reaction, makes this method simpler, faster, and more sensitive than the classic approach of the Sandell–Kolthoff reaction. The method allowed iodine to be determined within a range of 0.20–4.0 µmol L⁻¹, with or without the in-line UV digestion, with a limit of detection of 0.028 µmol L⁻¹ and 0.025 µmol L⁻¹, respectively.     

Sulfoxide‐Directed Metal‐Free ortho‐Propargylation of Aromatics and Heteroaromatics

A sulfoxide‐directed, metal‐free ortho‐propargylation of aromatics and heteroaromatics exploits intermolecular delivery of a propargyl nucleophile to sulfur followed by an intramolecular relay to carbon. The operationally simple cross‐coupling procedure is general, regiospecific with regard to the propargyl nucleophile, and shows complete selectivity for products of ortho‐propargylation over allenylation. The use of secondary propargyl silanes allows metal‐free ortho‐coupling to form carbon–carbon bonds between aromatic and heteroaromatic rings and secondary propargylic centres. The ‘safety‐catch’ nature of the sulfoxide directing group is illustrated in a selective, iterative double cross‐coupling process. The products of propargylation are versatile intermediates and they have been readily converted into substituted benzothiophenes.     

Isobaric (vapour + liquid + liquid) equilibrium data for (di-n-propyl ether + n-propyl alcohol + water) and (diisopropyl ether + isopropyl alcohol + water) systems at 100 kPa

Isobaric (vapour + liquid + liquid) equilibria were measured for the (di-n-propyl ether + n-propyl alcohol + water) and (diisopropyl ether + isopropyl alcohol + water) system at 100 kPa.The apparatus used for the determination of (vapour + liquid + liquid) equilibrium data was an all-glass dynamic recirculating still with an ultrasonic homogenizer couple to the boiling flask.The experimental data demonstrated the existence of a heterogeneous ternary azeotrope for both ternary systems. The (vapour + liquid + liquid) equilibria data were found to be thermodynamically consistent for both systems.The experimental data were compared with the estimation using UNIQUAC and NRTL models and the prediction of UNIFAC model.