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121.
Daniele Di Corcia Veronica Morra Marco Pazzi Marco Vincenti 《Biomedical chromatography : BMC》2010,24(4):358-366
A fast screening protocol was developed and validated for the simultaneous determination of 15 β2‐agonists in human urine (bambuterol, cimbuterol, clenbuterol, fenoterol, formoterol, isoproterenol, mapenterol, metaproterenol, procaterol, ractopamine, ritodrine, salbutamol, salmeterol, terbutaline, tulobuterol). The overall sample processing includes deconjugation with enzyme hydrolysis, liquid–liquid extraction, followed by derivatization of the extract and detection of β2‐agonists trimethylsilyl‐derivatives by fast‐gas chromatography/electron impact–mass spectrometry (fast‐GC/EI‐MS). Sample extraction and derivatization were optimized with the purpose of improving recoveries and reaction yields for a variety of analytes with different structures simultaneously, while keeping the procedure simple and reliable. Validation parameters were determined for each analyte under investigation, including selectivity, linearity, intra‐ and inter‐assay precision, extraction recoveries and signal to noise ratio (S/N) at the lowest calibration level. Fast‐GC/MS sequences, based on the use of short columns, high carrier‐gas velocity and fast temperature ramping, allow considerable reduction of the analysis time (7 min), while maintaining adequate chromatographic resolution. The overall GC cycle time was less than 9 min, allowing a processing rate of 6 samples/h. High MS‐sampling rate, using a benchtop quadrupole mass analyzer, resulted in accurate peak shape definition under both scan and selected ion monitoring modes, and high sensitivity in the latter mode. The method was successfully tested on real samples arising from clinical treatments. Copyright © 2009 John Wiley & Sons, Ltd. 相似文献
122.
123.
Daniele Balducci Simone Contaldi Ilaria Lazzari Gianni Porzi 《Tetrahedron: Asymmetry》2009,20(12):1398-1401
A new, practical and very convenient stereocontrolled synthesis of (S)-2′,6′-dimethyltyrosine [(S)-Dmt] 4 was accomplished in a good yield, starting from the chiral synthon 1,4-N,N-[(S)-phenylethyl]-piperazine-2,5-dione 1. The procedure, which is an extension of our original strategy and occurs with a high level of stereoselectivity (>98%), is simple and inexpensive allowing us to prepare the unnatural α-aminoacid (S)-Dmt also on a multi-gram scale. 相似文献
124.
Piotr Dobrzynski Daniele Fabbri Cristian Torri Janusz Kasperczyk Bozena Kaczmarczyk Malgorzata Pastusiak 《Journal of polymer science. Part A, Polymer chemistry》2009,47(1):247-257
A hydroxylactone ((1R,5S)‐1‐hydroxy‐3,6‐dioxabicyclo [3.2.1] octan‐2‐one, abbreviated as LAC) obtained from catalytic pyrolysis of cellulose was investigated as a monomer in the synthesis of polyesters by ring‐opening polymerization (ROP) with L ‐lactide. Although stannous octoate resulted inactive, ROP initiated by zirconium (IV) acetylacetonate afforded novel copolyesters from LAC and lactide mixtures in the bulk at 110 °C. Copolymers were obtained with different LAC content (from 19 to 45%) with a random microstructure as established by detailed NMR analysis. FTIR spectrometry confirmed the presence in the polymer chain of the OH groups originally present in LAC, which do not react during polymerization due to steric hindrance and inter/intramolecular hydrogen bonding. Reaction with trichloroacetylisocyanide proved that OH groups of the polyesters can be readily derivatized. The application of LAC as a comonomer enables the insertion of the alcohol functionality in polylactide avoiding protection/deprotection steps and potentially expanding the realm of biomaterials affordable from carbohydrate feedstock. © 2008 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 47: 247–257, 2009 相似文献
125.
Daniele Passarella Sergio Riva Gabriele Grieco Francesco Cavallo Begoña Checa Federica Arioli Elena Riva Daniela Comi Bruno Danieli 《Tetrahedron: Asymmetry》2009,20(2):192-197
The convenient synthesis of both enantiomers of the piperidine alkaloids such as dumetorine and epidihydropinidine is described. Pure enantiomers of 2-(2-hydroxy-ethyl)-piperidine-1-carboxylic acid tert-butyl ester are used as a common starting material. The syntheses are based on a RCM reaction and on methylation of the piperidine ring according to Beak–Lee methodology, respectively. 相似文献
126.
Regular polynomials with quaternionic coefficients admit only isolated zeroes and spherical zeroes. In this paper we prove
a factorization theorem for such polynomials. Specifically, we show that every regular polynomial can be written as a product
of degree one binomials and special second degree polynomials with real coefficients. The degree one binomials are determined
(but not uniquely) by the knowledge of the isolated zeroes of the original polynomial, while the second degree factors are
uniquely determined by the spherical zeroes. We also show that the number of zeroes of a polynomial, counted with their multiplicity
as defined in this paper, equals the degree of the polynomial. While some of these results are known in the general setting
of an arbitrary division ring, our proofs are based on the theory of regular functions of a quaternionic variable, and as
such they are elementary in nature and offer explicit constructions in the quaternionic setting.
Partially supported by G.N.S.A.G.A.of the I.N.D.A.M. and by M.I.U.R..
Lecture held by G. Gentili in the Seminario Matematico e Fisico on February 12, 2007.
Received: August 2008 相似文献
127.
Computerized Developments in Design,Generation, Simulation of Meshing,and Stress Analysis of Gear Drives 总被引:4,自引:0,他引:4
Faydor?L.?Litvin Daniele?Vecchiato Eugene?Gurovich Alfonso?FuentesEmail author Ignacio?Gonzalez-Perez Kenichi?Hayasaka Kenji?Yukishima 《Meccanica》2005,40(3):291-323
The paper represents new computerized developments in design, generation, simulation of meshing, and stress analysis of gear drives. The main contents of the paper are: (i) application of a predesigned parabolic function of transmission errors for reduction of noise, (ii) computerized simulation of noise caused by transmission errors, (iii) modification of the basic algorithm of tooth contact analysis, and (iv) application of approaches developed for enhanced design and simulation of meshing of the following gear drives: (a) spiral bevel gear drives, (b) face-gear drives (including an approach for grinding), and (c) modified helical gear drives. The developed theory is illustrated with numerical examples. 相似文献
128.
129.
Daniele Pergolesi Emiliana Fabbri Enrico Traversa 《Electrochemistry communications》2010,12(7):977-980
Anode-supported solid oxide fuel cells (SOFCs) based on thin BaZr0.8Y0.2O3 ? δ (BZY) electrolyte films were fabricated by pulsed laser deposition (PLD) on sintered NiO–BZY composite anodes. After in situ reduction of NiO to Ni, the anode substrates became porous, while retaining good adhesion with the electrolyte. A slurry-coated composite cathode made of La0.6Sr0.4Co0.2Fe0.8O3 ? δ (LSCF) and BaCe0.9Yb0.1O3 ? δ (BCYb), specifically developed for proton conducting electrolytes, was used to assemble fuel cell prototypes. Depositing by PLD 100 nm thick LSCF porous films onto the BZY thin films was essential to improve the cathode/electrolyte adhesion. A power density output of 110 mW/cm2 at 600 °C, the largest reported value for an anode-supported fuel cell based on BZY at this temperature, was achieved. Electrochemical impedance spectroscopy (EIS) measurements were used to investigate the different contributions to the total polarization losses. 相似文献
130.
Li R Zeitler JA Tomerini D Parrott EP Gladden LF Day GM 《Physical chemistry chemical physics : PCCP》2010,12(20):5329-5340
The phonon modes of crystalline benzoic acid have been investigated using terahertz time-domain spectroscopy, rigid molecule atom-atom model potential and plane-wave density functional theory lattice dynamics calculations. The simulation results show good agreement with the measured terahertz spectra and an assignment of the terahertz absorption features of benzoic acid is made with the help of both computational methods. Focussing on the strongest interactions in the crystal, we describe each vibration in terms of distortions of the benzoic acid hydrogen bonded dimers that are present in the crystal structure. The terahertz spectrum is also shown to be highly sensitive to the location of the carboxylic acid hydrogen atoms in the cyclic hydrogen-bonded dimers and we have systematically explored the influence of the observed disorder in the hydrogen atom positions on the lattice dynamics. 相似文献