Determination of 20(S)-protopanaxadiol in rat plasma by LC-MS/MS and its application to the pharmacokinetic study: A comparative study of its solution and two oral formulations

A high-performance liquid chromatography — tandem mass spectrometry method was used in a comparative pharmacokinetic study on 20(S)-protopanaxadiol in its solution, pharmacosomes and hydroxy-propyl-β-cyclodextrin inclusion compound. The calibration linearity range was 2.5–5000 ng/mL and the limit of quantification was 2.5 ng/mL. The intra- and inter-assay coefficients of variation were less than 7% and the recoveries were 67.4, 63.3 and 69.6% at 5, 250 and 4500 ng/mL. In contrast to 20(S)-protopanaxadiol solution, its pharmacosomes and hydroxypropyl-β-cyclodextrin inclusion compound improved the oral bioavailability to different extent and meanwhile were much safer in clinical use.     

Hydrothermal synthesis and structural characterization of a one-dimensional coordination polymer [Zn(Pydc)(Dppz)] n (H2Pydc = 2,6-pyridinedicarboxylic acid, Dppz = dipyrido[3,2-a:2′,3′-c]phenazine)

A new metal-organic coordination polymer [Zn(Pydc)(Dppz)] _n (I) (H₂Pydc = 2,6-pyridinedicarboxylic acid, Dppz = dipyrido[3,2-a:2′,3′-c]phenazine) was hydrothermally synthesized and characterized by elemental analysis, IR and X-ray single-crystal diffraction. The X-ray diffraction analysis reveals that I crystallizes in the monoclinic system, space group P2₁/c. The Pydc^2? ligands adopt O,N,O′-tridentate chelating and monodentate bridging coordination mode to link two adjacent Zn2+ ions to form a one-dimensional (1D) zigzag chain. The adjacent chains are further linked through hydrogen bonds and π-π stacking interactions, forming a three-dimensional (3D) supramolecular framework. The unit cell parameters for I: a = 7.332(3) Å, b = 36.023(9) Å, c = 7.8838(13) Å, β = 105.65(3)^○, V = 2005.1(10) ų, Z = 4.     

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.     

航天相机热实验测试系统设计

为了检测航天相机在高低温环境中的电子学性能及可靠性,针对某型号航天相机地面热实验测试需求,设计开发出了一种热实验测试系统,详细介绍了系统的软硬件设计方案及控温策略。系统使用人机交互界面实现热控策略,能实时完成最高80个测试点(160个温度传感器及80路加热器)的控温任务,可以在－30℃～＋50℃范围内对航天相机进行全方位的温度监控,最高控温精度达到0.5℃。经过实际测试验证,系统具有很好的稳定性,能满足航天相机地面热实验的测试需求,工程应用价值高。     

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.