Simultaneous determination of sibutramine and its active metabolites in human plasma by LC‐MS/MS and its application to a pharmacokinetic study

A simple and sensitive liquid chromatography–electrospray ionization–tandem mass spectrometry (LC‐ESI‐MS/MS) technique was developed and validated for the determination of sibutramine and its N‐desmethyl metabolites (M1 and M2) in human plasma. After extraction with methyl t‐butyl ether, chromatographic separation of analytes in human plasma was performed using a reverse‐phase Luna C₁₈ column with a mobile phase of acetonitrile–10 mm ammonium formate buffer (50:50, v/v) and quantified by ESI‐MS/MS detection in positive ion mode. The flow rate of the mobile phase was 200 μL/min and the retention times of sibutramine, M1, M2 and internal standard (chlorpheniramine) were 1.5, 1.4, 1.3 and 0.9 min, respectively. The calibration curves were linear over the range 0.05–20 ng/mL, for sibutramine, M1 and M2. The lower limit of quantification was 0.05 ng/mL using 500 μL of human plasma. The mean accuracy and the precision in the intra‐ and inter‐day validation for sibutramine, M1 and M2 were acceptable. This LC‐MS/MS method showed improved sensitivity and a short run time for the quantification of sibutramine and its two active metabolites in plasma. The validated method was successfully applied to a pharmacokinetic study in human. Copyright © 2011 John Wiley & Sons, Ltd.     

Efficient Electrocatalytic Reduction of CO2 by Nitrogen-Doped Nanoporous Carbon/Carbon Nanotube Membranes: A Step Towards the Electrochemical CO2 Refinery

Herein we introduce a straightforward, low cost, scalable, and technologically relevant method to manufacture an all-carbon, electroactive, nitrogen-doped nanoporous-carbon/carbon-nanotube composite membrane, dubbed “HNCM/CNT”. The membrane is demonstrated to function as a binder-free, high-performance gas diffusion electrode for the electrocatalytic reduction of CO₂ to formate. The Faradaic efficiency (FE) for the production of formate is 81 %. Furthermore, the robust structural and electrochemical properties of the membrane endow it with excellent long-term stability.     

Synthesis and morphology investigations of a novel alkyne‐functionalized diblock copolymer

We reported the synthesis and morphology of a novel alkyne‐functionalized diblock copolymer (di‐BCP) poly(methyl methacrylate‐random‐propargyl methacrylate)‐block‐poly(4‐bromostyrene). The di‐BCPs were synthesized by atom transfer radical polymerization and postpolymerization deprotection, with good control over molecular weight and polydispersity index. Microphase separation in bulk di‐BCPs was confirmed by thermal analysis, small‐angle X‐ray scattering, and transmission electron microscopy. Microphase‐separated morphologies were also observed in thin films, and the orientation of the microdomains can be conveniently controlled by annealing under different solvents. © 2012 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys, 2012