Rapid and Simple Method to Determine Tamoxifen and Its Major Metabolites in Human Liver Microsomes by High Performance Liquid Chromatography with Fluorescence Detection

Abstract

Sensitive and reproducible analyses were developed for assaying tamoxifen, desmethyltamoxifen, didesmethyltamoxifen and hydroxytamoxifen in human liver microsomes by high performance liquid chromatography (H.P.L.C.) following protein precipitation. Detection was by fluorimetry of phenanthrene derivatives formed by on-stream U.V. irradiation with a photochemical reactor enhanced detection (P.H.R.E.D.) for post-column irradiation of the H.P.L.C. stream. The method is highly sensitive (1 ng/ml). A C8,5 μm column (4.6 x 150 mm) was used, with a mobile phase of acetonitrile / 100 mM ammonium acetate (1:1) pH 5. Precipitation of the microsomal protein was carried out by adding methanol and concentrated chloric acid to the reaction mixture, and extraction efficiencies were approximately 100 % for tamoxifen and its metabolites. The assay has been optimised for the identification and quantitation of the 4-hydroxylated metabolite, as well as the two metabolites formed by N-oxidative demethylation of the side chain. The latter catalytic activity involves cytochrome P450 3A enzymes.     

Discontinuous Galerkin methods for the Navier–Stokes equations using solenoidal approximations

An interior penalty method and a compact discontinuous Galerkin method are proposed and compared for the solution of the steady incompressible Navier–Stokes equations. Both compact formulations can be easily applied using high‐order piecewise divergence‐free approximations, leading to two uncoupled problems: one associated with velocity and hybrid pressure, and the other one only concerned with the computation of pressures in the elements interior. Numerical examples compare the efficiency and the accuracy of both proposed methods. Copyright © 2009 John Wiley & Sons, Ltd.     

UV‐curable bismaleimides containing poly(dimethylsiloxane): Use as hydrophobic agent

The synthesis and characterization of poly(dimethylsiloxanes) bearing maleimides end‐groups (PDMSM) were carried out through imidization of maleic anhydride with three poly(dimethylsiloxanes) diamines of different molecular weights. Self‐photopolymerization of PDMSM was studied by Real‐Time Fourier Transform infrared spectroscopy (RT‐FTIR) and was possible even without photoinitiator (Darocur 1173). The reaction was found to proceed within seconds upon exposure to ultraviolet (UV) radiation to generate highly crosslinked polymer networks. The results indicated that these polymerizations were less sensitive to oxygen inhibition than the radical processes carried out on conventional UV‐curable acrylate resins. The thermal and mechanical properties of these resulting materials were studied starting from PDMS precursors with different molecular weights. These materials exhibit a low glass transition temperature (相似文献   

High‐density polyethylene/expanded graphite nanocomposites produced by polymerization‐filling technique using an industrial heterogeneous catalyst

High‐density polyethylene nanocomposites with different expanded graphite (EG) contents (0.34–1.80 wt %) were prepared by polymerization‐filling technique using an industrial heterogeneous catalyst ( cat K ), and characterized using a range techniques: melting flow index (MFI), thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), dynamic mechanical analysis (DMA), and transmission electron microscopy (TEM). The MFI data showed that EG acts as a plasticizer decreasing melt viscosity in comparison to neat HDPE produced exclusively by cat K . DSC results showed that EG nucleated the HDPE crystallization as established by the increased crystallization temperature, and the degree of crystallinity. HDPE/EG nanocomposites displayed a significant improvement in the flexural (increased from 1458 to 1831 MPa), and storage modulus (increased from 122 to 1627 MPa) at only 1.80 wt % EG content. TEM images confirmed a homogeneous distribution of EG into the polymer matrix with the presence of dispersed, intercalated and aggregated EG nanofillers. © 2016 Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2016 , 55, 1260–1267     

Synthesis of a benzoxazine with precisely two phenolic OH linkages and the properties of its high‐performance copolymers

A phenolic OH‐containing benzoxazine ( F‐ap ), which cannot be directly synthesized from the condensation of bisphenol F, aminophenol, and formaldehyde by traditional procedures, has been successfully prepared in our alternative synthetic approach. F‐ap was prepared by three steps including (a) condensation of 4‐aminophenol and 5,5'‐methylenebis(2‐hydroxybenzaldehyde) (1) , (b) reduction of the resulting imine linkage by sodium borohydride, and (c) ring closure condensation by formaldehyde. The key starting material, (1) , was prepared from 2‐hydroxybenzaldehyde and s‐trioxane in the presence of sulfuric acid. F‐ap is structurally similar to bis(3,4‐dihydro‐2H‐3‐phenyl‐1,3‐benzoxazinyl)methane ( F‐a, a commercial benzoxazine based on bisphenol F/aniline/formaldehyde) except for two phenolic OHs. The phenolic OHs can provide reaction sites with epoxy and 1,1'‐(methylenedi‐p‐phenylene)bismaleimide (BMI). The structure–property relationships between the thermosets of F‐ap /epoxy, F‐a /epoxy, F‐ap /BMI, and F‐a /BMI were discussed. Experimental data showed that thermosets based on F‐ap /epoxy and F‐ap /BMI provided much better thermal properties than those based on F‐a /epoxy and F‐a /BMI. © 2013 Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2013, 51, 2686–2694     

High pressure studies of viscosity effects on isomerization

Abstract

The viscosity dependence of the isomerization process with comparatively low potential barrier was studied as a model of one-dimensional barrier crossing.

We found that the ground-state isomerization of DODCI fails to fit the Kramers equation. We analyzed this non-Kramers behavior by means of an approach of frequency dependent friction.     

High pressure neutron-scattering experiments on phospholipid model biomembranes

Abstract

By use of neutron small-angle scattering (SANS) the structural properties of saturated and unsaturated phosphatidylcholine model biomembrane systems have been investigated in the temperature range from 0°C to 70°C and at pressures up to 3.5 kbar. The effect of chemical constitution of the hydrocarbon chains of the lipids and the effect of cholesterol on the thermotropic and barotropic phase behaviour is discussed.     

Phase transition of samarium under high pressure

Abstract

The DAC X-ray power photograph method was employed for studing the phase transition of samarium up to 26.3 GPa. The experimental results show that the dhcp and fcc high pressure phase of Sm appeared at about 4.0 and 12.5 GPa and room temperature respectively. The dhcp phase was kept until 19.6 GPa. A model for Sm-type -? dhcp -? fcc phase transition is provided in this paper.