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171.
Rossella Gottardo Daniela Sorio Giulia Soldati Marco Ballotari Nadia Maria Porpiglia Franco Tagliaro 《Electrophoresis》2021,42(4):450-459
The continuous introduction in the market of new psychoactive drugs (NPS) represents a well-known international emergency. Indeed, the European Monitoring Centre for Drugs and Drug Addiction and the United Nations Office on Drugs and Crime are paying great attention to the spread of NPS. In addition to the traditional analytical approaches based on GC-MS and HPLC-MS, also CE coupled with MS has proved to be a precious tool for the toxicological screening of biosamples. On these grounds, the aim of the present work was to test the application of CE-HRMS as a new screening tool for the rapid detection of these novel drugs in urine. Separations were performed in an uncoated fused-silica capillary with id of 75 μm with a total length of 100 cm, by applying a constant voltage of 15 kV. The QTOF-MS was implemented with an electrospray ion source operating in positive ionization full scan mode in the range of 100–1000 m/z. Under these conditions, different NPS has been tested, including eight cathinones, five phenethylamine, and seven tryptamines. The method was validated after optimization of the following analytical parameters: BGE composition and pH, separation voltage, sheath liquid composition, and flow rate and ESI source settings. The applicability of the method was successfully tested by analyzing a series of real urine samples obtained from drug users. 相似文献
172.
Nara Singh BS Liu Z Wadsworth R Grawe H Brock TS Boutachkov P Braun N Blazhev A Górska M Pietri S Rudolph D Domingo-Pardo C Steer SJ Ataç A Bettermann L Cáceres L Eppinger K Engert T Faestermann T Farinon F Finke F Geibel K Gerl J Gernhäuser R Goel N Gottardo A Grębosz J Hinke C Hoischen R Ilie G Iwasaki H Jolie J Kaşkaş A Kojouharov I Krücken R Kurz N Merchán E Nociforo C Nyberg J Pfützner M Prochazka A Podolyák Z Regan PH Reiter P Rinta-Antila S Scholl C Schaffner H Söderström PA Warr N 《Physical review letters》2011,107(17):172502
A β-decaying high-spin isomer in (96)Cd, with a half-life T(1/2)=0.29(-0.10)(+0.11) s, has been established in a stopped beam rare isotope spectroscopic investigations at GSI (RISING) experiment. The nuclei were produced using the fragmentation of a primary beam of (124)Xe on a (9)Be target. From the half-life and the observed γ decays in the daughter nucleus, (96)Ag, we conclude that the β-decaying state is the long predicted 16(+) "spin-gap" isomer. Shell-model calculations, using the Gross-Frenkel interaction and the πν(p(1/2),g(9/2)) model space, show that the isoscalar component of the neutron-proton interaction is essential to explain the origin of the isomer. Core excitations across the N=Z=50 gaps and the Gamow-Teller strength, B(GT) distributions have been studied via large-scale shell-model calculations using the πν(g,d,s) model space to compare with the experimental B(GT) value obtained from the half-life of the isomer. 相似文献
173.
174.
In recent years, 3D printing of carbon-based conductive filaments has received growing attention for assembling electrodes to be used in a wide variety of electroanalytical devices and applications. Despite the large amount of work present in literature concerning the development of three-dimensional (3D) conductive structures, its potential as dry deposition method for assembling two-dimensional (2D) electrodes to be used in planar configuration is still largely unexplored. In fact, the possibility to rapidly change the geometry of the electrochemical circuits, associated with the reduction of waste and the absence of solvents, which are instead important components of ink and paste formulations, makes this strategy a valid green and efficient alternative to other deposition approaches such as screen-printing technology. We report here a rapid and solvent-free method for assembling fully 3D printed flexible planar electroanalytical platforms (3DEPs) to be used with microliters of liquid. At the same time, a novel protocol for the surface pre-treatment of 3D printed electrodes based on ultrasonication in aqueous NaOH solution followed by electrochemical activation using the same medium, is presented. In addition, the same procedure has proved to be efficient for cleaning the electrode surface after electrochemical passivation, thus confirming the validity of both time-efficient and environmentally-friendly assembling and activation/cleaning procedures developed which allow efficient and reusable electrodes to be produced. Finally, 3DEPs were tested by a proof-of-concept quantification of a commonly used food dye (Brilliant Blue, E-133) in commercial solutions used for homemade food coloring. 相似文献
175.
Collie GW Promontorio R Hampel SM Micco M Neidle S Parkinson GN 《Journal of the American Chemical Society》2012,134(5):2723-2731
The folding of the single-stranded 3' end of the human telomere into G-quadruplex arrangements inhibits the overhang from hybridizing with the RNA template of telomerase and halts telomere maintenance in cancer cells. The ability to thermally stabilize human telomeric DNA as a four-stranded G-quadruplex structure by developing selective small molecule compounds is a therapeutic path to regulating telomerase activity and thereby selectively inhibit cancer cell growth. The development of compounds with the necessary selectivity and affinity to target parallel-stranded G-quadruplex structures has proved particularly challenging to date, relying heavily upon limited structural data. We report here on a structure-based approach to the design of quadruplex-binding ligands to enhance affinity and selectivity for human telomeric DNA. Crystal structures have been determined of complexes between a 22-mer intramolecular human telomeric quadruplex and two potent tetra-substituted naphthalene diimide compounds, functionalized with positively charged N-methyl-piperazine side-chains. These compounds promote parallel-stranded quadruplex topology, binding exclusively to the 3' surface of each quadruplex. There are significant differences between the complexes in terms of ligand mobility and in the interactions with quadruplex grooves. One of the two ligands is markedly less mobile in the crystal complex and is more quadruplex-stabilizing, forming multiple electrostatic/hydrogen bond contacts with quadruplex phosphate groups. The data presented here provides a structural rationale for the biophysical (effects on quadruplex thermal stabilization) and biological data (inhibition of proliferation in cancer cell lines and evidence of in vivo antitumor activity) on compounds in this series and, thus, for the concept of telomere targeting with DNA quadruplex-binding small molecules. 相似文献
176.
Herbert Oberacher Florian Pitterl Eleni Siapi Barry R. Steele Thomas Letzel Sylvia Grosse Bernhard Poschner Franco Tagliaro Rossella Gottardo Silvi A. Chacko Jonathan L. Josephs 《Journal of mass spectrometry : JMS》2012,47(2):263-270
Mass spectral libraries represent versatile tools for the identification of small bioorganic molecules. Libraries based on electron impact spectra are rated robust and transferable. Tandem mass spectral libraries are often considered to work properly only on the instrument that has been used to build the library. An exception from that rule is the ‘Wiley Registry of Tandem Mass Spectral Data, MSforID’. In various studies with data sets from different kinds of tandem mass spectrometric instruments, the outstanding sensitivity and robustness of this tandem mass spectral library search approach was demonstrated. The instrumental platforms tested, however, mainly included various tandem‐in‐space instruments. Herein, the results of a multicenter study with a focus on upfront and tandem‐in‐time fragmentation are presented. Five laboratories participated and provided fragment ion mass spectra from the following types of mass spectrometers: time‐of‐flight (TOF), quadrupole–hexapole–TOF, linear ion trap (LIT), 3‐D ion trap and LIT–Orbitrap. A total number of 1231 fragment ion mass spectra were collected from 20 test compounds (amiloride, buphenin, cinchocaine, cyclizine, desipramine, dihydroergotamine, dyxirazine, dosulepin, ergotamine, ethambutol, etofylline, mefruside, metoclopramide, phenazone, phentermine, phenytoin, sulfamethoxazole, sulfamoxole, sulthiame and tetracycline) on seven electrospray ionization instruments using 18 different instrumental configurations for fragmentation. For 1222 spectra (99.3%), the correct compound was retrieved as the best matching compound. Classified matches (matches with ‘relative average match probability’ >40.0) were obtained for 1207 spectra (98.1%). This high percentage of correct identifications clearly supports the hypothesis that the tandem mass spectral library approach tested is a robust and universal identification tool. Copyright © 2012 John Wiley & Sons, Ltd. 相似文献
177.
We prove, using the random-cluster model, a strict inequality between site percolation and magnetization in the region of
phase transition for the d-dimensional Ising model, thus improving a result of [5]. We extend this result also at the case of two plane lattices
(slabs) and give a characterization of phase transition in this case. The general case of N slabs, with N an arbitrary positive integer, is partially solved and it is used to show that this characterization holds in the case of
three slabs with periodic boundary conditions.
AMS classification: 60K35, 82B20, 82A25 相似文献
178.
Rossella Dorati 《Polymer Degradation and Stability》2010,95(4):694-701
The aim of the study was to examine the relationship between the structural features of PLGA 3-D scaffolds and their degradation performances. PLGA 3-D scaffolds were fabricated by solvent casting and particulate leaching using salt and sucrose particles as porogen and they were characterized in terms of structure, physico-chemical and mechanical properties. The in vitro degradation study was performed at 37 °C in PBS for 28 days and it included the determination of Mw, Mn, PI, water uptake, mass loss and pH changes of the degradation buffer. It was found that the preparation method scaffolds, in particular the choice of the porogen type and was responsible for the three-dimensional structure (pore size, porosity, apparent density and, mechanical properties) of the scaffold and for physico-chemical PLGA polymer modifications (polymer degradation reactions, polymer chain rearrangement, Tg changes). Scaffolds with high porosity (83.8-89.4%) and an interconnected network were obtained. 相似文献
179.
180.
Christine Gottardo Stephen Fratpietro Alan N. Hughes Mark Stradiotto 《Heteroatom Chemistry》2000,11(3):182-186
The stable 7‐phosphanorbornadiene derivative, 2,3‐benzo‐1,4,5,6,7‐pentaphenyl‐7‐phosphabicyclo[2.2.1]hepta‐2,5‐diene‐7‐oxide ( 1 ) was synthesized in 45% yield via the Diels‐Alder reaction of pentaphenylphosphole oxide and benzyne. The reaction occurs specifically to give a single isomer, which was characterized by use of X‐ray crystallography and 31P NMR spectroscopy. © 2000 John Wiley & Sons, Inc. Heteroatom Chem 11:182–186, 2000 相似文献