Simultaneous Determination of α- and γ-Mangostins in Mouse Plasma by HPLC–MS/MS Method: Application to a Pharmacokinetic Study of Mangosteen Extract in Mouse

Recently, extracts from the pericarp of mangosteen, Garcinia mangostana L., exhibited various pharmacological properties such as anti-oxidative, anti-inflammatory, anti-bacterial and chemopreventive activities. Albeit it has diverse application, there is little information about its pharmacokinetic aspects. Thus, the present study was undertaken to develop the simultaneous determination of α- and γ-mangostins (α- and γ-MG), major and active compounds, from extracts for the application of pharmacokinetic studies in mice using combined liquid chromatography–tandem mass-spectrometry and microsampling systems. The intra- and inter-validation, precision, accuracy, stability, recovery and matrix effects of α- and γ-MG were conducted in mouse plasma. Based on the developed analytical methods, pharmacokinetic parameters of α- and γ-MG after intravenous and oral administration of mangosteen extract were calculated. In sample preparation steps, the biological samples were deproteinized by acetonitrile and chromatographic separation was accomplished on a C₁₈ column. The detection was accomplished by multiple-reaction monitoring scanning after electrospray ionization source in the positive ionization mode. The optimized mass transition ion pairs (m/z) for quantitation were 411.062 → 354.900, 397.384 → 340.900, and 808.379 → 527.200 for α- and γ-MG and docetaxel (internal standard), respectively. The total run time was 5 min. The results provided a meaningful basis for the preclinical and clinical application of mangosteen extract.     

Direct Conversion of Silyl Ethers Into Carbonyl Compounds with Jones Reagent in the Presence of Potassium Fluoride

Treatment of silyl ethers with Jones reagent in acetone in the presence of potassium fluoride resulted in the silicon-oxygen bond cleavage and oxidation to give carbonyl compounds directly.     

One-Pot Synthesis of Cefpirome Sulfate from GCLE

Abstract

Cefpirome was synthesized in 37.7% overall yield from 3-chloromethyl-7-phenylacetylamino cephalosporanic acid p-methoxybenzyl ester (GCLE) by sequential substitution of C-3 chloride with iodide and 2,3-cyclopentenopyridine, followed by a one-pot procedure including deprotection of carboxyl group, hydrolysis of 7-phenylacetamido, and reaction with 2-mercaptobenzothiazolyl-(Z)-2-(2-aminothiazol-4-yl)-2-methoxyiminoacetate (MAEM). The reaction conditions were as follows: obtained from GCLE at low temperature (?5 to 0 °C) and absence of light, 3-iodomethyl-7-phenylacetylamino cephalosporanic acid p-methoxybenzyl ester (GILE) without purification was reacted directly with 2,3-cyclopentenopyridine, in which the molar ratio of GCLE, NaI, and 2,3-cyclopentenopyridine was 1:2:4, and the molar ratio of the resulting compound p-methoxybenzyl 7-phenylacetylamido-3-(2,3-cyclopenteno-1-pyridinio)methyl-3-cephem-4-carboxylate iodide and MAEM was 1:1.1. The structure of the intermediate and the target compound obtained were determined by nuclear magnetic resonance spectra and mass spectroscopy.     

Synthesis and application of moisture-stable methallylsilanated phosphorylcholine as a surface modifier

New methallylsilanated phosphorylcholine (MASPCs) were synthesized via a copper-catalyzed ‘click’ reaction and demonstrated excellent moisture stability. Hydroxylated silicon compounds, silanol, and silica were grafted or modified by MASPCs in the presence of triflic acid (TfOH) and they possessed a good grafting efficiency and high loading rate.     

Convenient synthesis of 1a,1b,2,5-tetrahydro-1H-5a-aza-cyclopropa[a]indenes by base promoted cyclodimerization of 1,1-dicyano-2-aryl-3-benzoylcyclopropanes

1,1-Dicyano-2-aryl-3-benzoylcyclopropanes in acetonitrile in the presence of triethylamine underwent cyclodimerization reaction to afford the novel polyfunctionalized 1a,1b,2,5-tetrahydro-1H-5a-aza-cyclopropa[a]indenes in moderate yields. These polycyclic compounds can be more conveniently synthesized by the one-pot domino reaction of N-phenacylpyridinium bromides with arylidene malononitriles.     

Inclusion of thymol into cucurbiturils: density functional theory approach with dispersion correction and natural bond orbital analysis

Journal of Inclusion Phenomena and Macrocyclic Chemistry - Stability of inclusion complexes of thymol (a natural flavour) with cucurbit[n]urils was interpreted by using density functional theory...     

Phase‐Junction Electrocatalysts towards Enhanced Hydrogen Evolution Reaction in Alkaline Media

To ensure sustainable hydrogen production by water electrolysis, robust, earth‐abundant, and high‐efficient electrocatalysts are required. Constructing a hybrid system could lead to further improvement in electrocatalytic activity. Interface engineering in composite catalysts is thus critical to determine the performance, and the phase‐junction interface should improve the catalytic activity. Here, we show that nickel diphosphide phase junction (c‐NiP₂/m‐NiP₂) is an effective electrocatalyst for hydrogen production in alkaline media. The overpotential (at 10 mA cm^?2) for NiP₂‐650 (c/m) in alkaline media could be significantly reduced by 26 % and 96 % compared with c‐NiP₂ and m‐NiP₂, respectively. The enhancement of catalytic activity should be attributed to the strong water dissociation ability and the rearrangement of electrons around the phase junction, which markedly improved the Volmer step and benefited the reduction process of adsorbed protons.