Determination of the appetite suppressant P57 in Hoodia gordonii plant extracts and dietary supplements by liquid chromatography/electrospray ionization mass spectrometry (LC-MSD-TOF) and LC-UV methods

Hoodia gordonii is traditionally used in South Africa for its appetite suppressant properties. P57AS3 (P57), an oxypregnane steroidal glycoside, is the only reported active constituent from this plant as an appetite suppressant. Effective quality control of these extracts or products requires rapid methods to determine P57 content. New methods of liquid chromatography/mass spectrometry (LC/MS) and LC-UV for analysis of P57 from H. gordonii have been developed. The quantitative determination of P57 was achieved with a Phenomenex Gemini (Torrance, CA) reversed-phase column using gradient mobile phase of water and acetonitrile, both containing 0.1% acetic acid. The method was validated for linearity, repeatability, and limits of detection and quantification. Good results were obtained in terms of repeatability (relative standard deviation <5.0%) and recovery (98.5-103.5%). The developed methods were applied to the determination of P57 for H. gordonii plant samples, one related genus (Opuntia ficus-indica), and dietary supplements that claim to contain H. gordonii.     

Diversity in Gold‐Catalyzed Formal Cycloadditions of Ynamides with Azidoalkenes or 2H‐Azirines: [3+2] versus [4+3] Cycloadditions

Gold‐catalyzed cycloadditions of ynamides with azidoalkenes or 2H‐azirines give [3+2] or [4+3] formal cycloadducts of three classes. Cycloadditions of ynamides with 2H‐azirine species afford pyrrole products with two regioselectivities when the C_β‐substituted 2H‐azirine is replaced from an alkyl (or hydrogen) with an ester group. For ynamides substituted with an electron‐rich phenyl group, their reactions with azidoalkenes proceed through novel [4+3] cycloadditions to deliver 1H‐benzo[d]azepine products instead.     

Magnetocapacitance and impedance spectroscopy of Ba0.7Sr0.3TiO3/La0.67Sr0.33MnO3 and Ba0.8Sr0.2TiO3/La0.67Sr0.33MnO3 thin film heterostructures

The paper discuses synthesis of Ba_0.7Sr_0.3TiO₃/La_0.67Sr_0.33MnO₃ and Ba_0.8Sr_0.2TiO₃/La_0.67Sr_0.33MnO₃ thin film heterostructures by sol–gel (citrate gel route) method. The XRD spectra are determined for confirmation of crystalline phases of Ba_0.7Sr_0.3TiO₃, Ba_0.8Sr_0.2TiO₃ and La_0.67Sr_0.33MnO₃ thin films. The observed variation of Cp, tan δ, magnetocapacitance (Mc), real part of dielectric constant ε′, imaginary part of dielectric constant ε″as a function of frequency, magnetoresistance R(H) and magnetoimpedance Z(H) are presented in the paper. Further the observed impedance spectra as a function of frequency f is also presented in the paper. The observed variation of Mc is qualitatively correlated with the stress induced effect and magnetoresistasnce effect occurring simultaneously.     

Evaluation of Probiotic Characteristics of Siderophoregenic <Emphasis Type="Italic">Bacillus</Emphasis> spp. Isolated from Dairy Waste

Siderophoregenic Bacillus strain DET9 has been selectively isolated from dairy waste. It was evaluated for probiotic characteristics and susceptibility pattern against antibiotics. Its spores showed excellent tolerance to simulated gastrointestinal tract conditions and exhibited antimicrobial activity against organisms such as Escherichia coli, Micrococcus flavus, and Staphylococcus aureus. Its susceptibility to antibiotics reduces the prospect to donate resistance determinants if administered in the form of probiotic preparations. It was observed to produce ∼60 mg/l catecholate type of siderophore under iron stressed conditions, identified as a 2,3-dihydroxy benzoic acid by high-performance liquid chromatography, infrared spectroscopy, nuclear magnetic resonance, and mass spectral analysis. Partial 16S-rRNA gene sequencing analysis shows that the isolate exhibited homology with Bacillus thuringiensis and Bacillus weihenstephanensis, whereas biochemical characterization revealed its novelty. DET9 exhibited no mortality of fishes in a 60-day trial, when fishes (surfi tetra) were challenged up to 100 ppm cell concentration, with their daily diet.     

Synthesis of highly functionalized 2(1H)-pyrazinone 3-carboxamide scaffolds

Synthesis of highly functionalized 2(1H)-pyrazinone 3-carboxamide derivatives is reported. A one-pot, two-step process including the base-mediated reaction of N,N-disubstituted aminoacetonitrile derivatives 18 with 3,5-dihalo-2(1H)-pyrazinones 1 afforded substituted aminoacetonitrile pyrazinone derivative 19, which on subsequent oxidation followed by transamidation of the resulting intermediate with primary or secondary amines gave the corresponding highly functionalized 2(1H)-pyrazinone 3-carboxamide derivatives 21.     

A theoretical charge density study on nitrogen-rich 4,4′,5,5′-tetranitro-2,2′-bi-1H-imidazole (TNBI) energetic molecule

The bond topological and electrostatic properties of nitrogen-rich 4,4′,5,5′-tetranitro-2,2′-bi-1H-imidazole (TNBI) energetic molecule have been calculated from the DFT method with the basis set 6-311G** and the AIM theory. The optimized geometry of this molecule is almost matched with the experimental geometric parameters. The electron density at the bond critical point and the Laplacian of electron density of C–NO₂ bonds are not equal, one of them is much weaker than the other. Similar trend exists in the C–N bonds of the imidazole ring of the molecule. The ratio of the bond dissociation energy (BDE) of the weakest bond to the molecular total energy exhibits nearly a linear correlation with the impact sensitivity; its h ₅₀% value is ~32.01 cm. The electrostatic potential around both the nitro groups are found unequal; the NO₂ group of weakest C–NO₂ bond exhibits an extended electronegative region.     

Ionic liquid promoted expeditious synthesis of flavones

A smooth conversion of substituted 1-(2-hydroxy phenyl)-3-phenyl-1,3-propane diones to flavones has been done using n-butyl-3-methyl-imidazolium tetrafluoroborate ionic liquid.     

Some studies on the extraction of plutonium from phosphate containing nitric acid solutions using DBDECMP as extractant

Extraction studies have been carried out to explore the feasibility of separation of Pu(IV) from phosphate containing analytical wastes generated in the laboratory. Distribution data on the extraction of Pu(IV) from DBDECMP (di-butyl, N,N-diethylcarbamoyl methyl phosphonate) in xylene from an aqueous nitric acid and its mixture with sulfuric as well as with sulfuric and phosphoric acids were obtained. Based on the data obtained, the conditions for the recovery of plutonium from such waste solutions are suggested.     

Synthesis and structure elucidation of a series of pyranochromene chalcones and flavanones using 1D and 2D NMR spectroscopy and X‐ray crystallography

A series of novel pyranochromene chalcones and corresponding flavanones were synthesized. This is the first report on the confirmation of the absolute configuration of chromene‐based flavanones using X‐ray crystallography. These compounds were characterized by 2D NMR spectroscopy, and their assignments are reported herein. The 3D structure of the chalcone 3b and flavanone 4g was determined by X‐ray crystallography, and the structure of the flavanone was confirmed to be in the S configuration at C‐2. Copyright © 2014 John Wiley & Sons, Ltd.