Condensation of all-cis-tetraphenylcyclotetrasiloxanetetraol in ammonia: new method for preparation of ladder-like polyphenylsilsesquioxanes

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Development and validation of a reversed‐phase HPLC method for CYP1A2 phenotyping by use of a caffeine metabolite ratio in saliva

CYP1A2 is important for metabolizing various clinically used drugs. Phenotyping of CYP1A2 may prove helpful for drug individualization therapy. Several HPLC methods have been developed for quantification of caffeine metabolites in plasma and urine. Aim of the present study was to develop a valid and simple HPLC method for evaluating CYP1A2 activity during exposure in xenobiotics by the use of human saliva. Caffeine and paraxanthine were isolated from saliva by liquid‐liquid extraction (chlorophorm/isopropanol 85/15v/v). Extracts were analyzed by reversed‐phase HPLC on a C₁₈ column with mobile phase 0.1% acetic acid/methanol/acetonitrile (80/20/2 v/v) and detected at 273nm. Caffeine and paraxanthine elution times were <13min with no interferences from impurities or caffeine metabolites. Detector response was linear (0.10–8.00µg/ml, R²>0.99), recovery was >93% and bias <4.47%. Intra‐ and inter‐day precision was <5.14% (n=6). The limit of quantitation was 0.10µg/ml and the limit of detection was 0.018±0.002µg/mL for paraxanthine and 0.032±0.002µg/ml for caffeine. Paraxanthine/caffeine ratio of 34 healthy volunteers was significantly higher in smokers (p<0.001). Saliva paraxanthine/caffeine ratios and urine metabolite ratios were highly correlated (r=0.85, p<0.001). The method can be used for the monitoring of CYP1A2 activity in clinical practice and in studies relevant to exposure to environmental and pharmacological xenobiotics. Copyright © 2015 John Wiley & Sons, Ltd.     

Formation of porous polymer morphology by microsyneresis during divinylbenzene polymerization

This article describes the investigation of the importance of various reaction conditions on microsyneretic pore formation during polymerization of divinylbenzene (DVB) under so‐called “solvothermal” conditions. To induce microsyneretic pore formation, the most important parameter is an unusually high dilution of monomers with a “good” porogen solvating the polymer chains. High dilution and solvation of the growing poly(DVB) chains promote the prolongation of the polymer chains rather than their interconnection by crosslinking. Consequently, when the polymer gel density reaches the point where syneresis starts, the polymer network is geometrically too extensive to be broken up into precipitating entities and, instead, porogen droplets are formed within the continuous polymer gel. The pore geometry created by microsyneresis offers high surface area in wide mesopores and hence, high capacity for supporting functional groups or reactions with much better accessibility than narrow pores between polymer microspheres produced by macrosyneresis in conventional styrenic polymer supports. © 2015 Wiley Periodicals, Inc. J. Polym. Sci., Part B: Polym. Phys. 2015 , 53, 774–781     

Fatigue life enhancement by irradiation of 12Cr1MoV steel with a Zr<Superscript>+</Superscript> ion beam. Mesoscale deformation and fracture

The structure and properties of 12Cr1MoV steel irradiated with a zirconium ion beam were studied by optical microscopy, scanning electron microscopy, and micro- and nanoindentation. It is shown that the modification covers the entire cross-section of the irradiated specimens to a depth of 1 mm. The data on irradiation-induced structural changes are used to interpret the changes in mechanical properties of the irradiated specimens under static and cyclic loading. Particular attention is given to analysis of strain estimation by the digital image correlation method.     

Synthesis of a disaccharide of phenolic glycolipid from Mycobacterium leprae (PGL-I) and its conjugates with bovine serum albumin

Russian Chemical Bulletin - Terminal disaccharide fragment of phenolic glycolipid from Mycobacterium leprae (PGL-I) was synthesized as a glycoside with 4-(2-aminoethoxy)phenyl aglycon. The obtained...