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第二届全国治疗药物监测学术年会

作者： Alexander Louie Robert Shi robin k.kelley Drug Studies Unit Department of Bioengineering & Therapeutic SciencesUniversity of CaliforniaSan FranciscoCA 94143USA. Helen Diller Family Comprehensive Cancer Center University of CaliforniaSan Francisco

A simple,fast and sensitive LC-MS/MS method was developed and validated for the simultaneous determination of the concentrations of temsirolimus and its major metabolite, sirolimus,in human whole *** blood sample(100μL)after adding temsirolimus-d7 and sirolimus-d3 internal standards was precipitated with 0.200 mL of methanol/0.300 M zinc sulfate (70/30,v/v)and then analyzed by a Shimatzu LC system coupled to a Sciex API-5000mass *** chromatographic separation was carried out on a BDS Hypersil C8 column(50 x 3.0 mm,5μrn)at 50℃with a mobile phase composed of methanol/water/formic acid(72/28/0.1) (v/v/v)containing 2.50 mM ammonium *** spectrometric detection was performed using electrospray positive ionization with multiple reactionsmonitoring *** method was validated from 0.250 ngmLto 100 ngmLfor temsirolimus and 0.100 ngmLto 40.0 ngmL for *** lower limits of quantitation were 0.25ngmLfor temsirolimus and 0.1 ngmL for *** precisions(CV%)of intra-day and inter-day for spiked quality control(QC) samples were less than 10.4%and 9.56%,*** accuracies as determined by the relative error for QC samples were less than 12.1%for intra-dayand 7.33%for *** significant matrix effect was *** method has been successfully applied to analyze the clinical pharmacokinetic study *** assay reproducibility was also demonstrated by using incurred samples.

关键词： Temsirolimus sirolimus human blood hepatocellular carcinoma LC-MS/MS

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Zinc-assisted synthesis of imidazolium-tetrazolate bi-heterocyclic zwitterions with variable alkyl bridge length

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Science China Chemistry 2012年第8期55卷 1620-1626页

作者： DRAB David M. SHAMSHINA Julia L. SMIGLAk Marcin COJOCARU O. Andreea kelley Steven P. ROGERS robin D. Center for Green Manufacturing and Department of Chemistry The University of Alabama Tuscaloosa AL 35487 USA

Zinc halide-complexed alkyl-bridged bi-heterocycles were obtained as zwitterions from the Click reaction of a series of N-cyanoalkyl-N-alkylimidazolium halide ionic liquids with sodium azide. Reaction optimization sho... 详细信息

关键词： Click chemistry ionic liquids heterocycle coordination chemistry

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Reactivity of N-cyanoalkyl-substituted imidazolium halide salts by simple elution through an azide anion exchange resin

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Science China Chemistry 2012年第8期55卷 1683-1687页

作者： DRAB David M. kelley Steven P. SHAMSHINA Julia L. SMIGLAk Marcin COJOCARU O. Andreea GURAU Gabriela ROGERS robin D. Center for Green Manufacturing and Department of Chemistry The University of Alabama Tuscaloosa AL 35487 USA

Certain N-cyanoalkyl-functionalized imidazolium halide salts unexpectedly undergo nitrile hydrolysis to amides, as well as dipolar cycloaddition to tetrazoles when eluted on azide anion exchanged resin.

关键词： multi-heterocycles ionic liquids azide exchange column nitrile cycloaddition tetrazoles imidazolium halide

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