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101.
Gomes P Wingert NR Paim CS Schapoval EE Steppe M 《Journal of AOAC International》2010,93(6):1829-1835
A stability-indicating HPLC assay method was developed for the quantitative determination of duloxetine (DLX) in a pharmaceutical dosage form in the presence of its degradation products, and kinetic determinations were evaluated in acid conditions and UV-C radiation exposure. Chromatographic separation was achieved by use of an ACE C18 column (250 x 4.0 mm id, 5 microm particle size). The mobile phase was prepared by mixing aqueous 50 mM potassium phosphate buffer (pH 6.0 containing 0.3% triethylamine) and acetonitrile (60 + 40, v/v). DLX was rapidly degraded in an acid medium and in the presence of hydrogen peroxide and UV-C radiation; it was more stable in alkaline medium. The described method was linear over a range of 4.0-14.0 microg/mL for determination of DLX (r = 0.9998). The precision was demonstrated by the RSD of intraday (0.79-1.07%) and interday (0.85%) studies. The mean recovery was found to be 100.56%. The acid degradation of DLX in 0.1 M HCI solution showed an apparent zero-order kinetics (k = 0.177 microg/mL/min), and the photodegradation demonstrated an apparent first-order kinetics (k = 0.082 microg/mL/min). The developed method was found to be simple, specific, robust, linear, precise, and accurate for the determination of DLX in enteric-coated pellets. 相似文献
102.
E. Mateus R.C. Barata Jitka Zrostlíková M.D.R. Gomes da Silva M.R. Paiva 《Journal of chromatography. A》2010,1217(11):1845-1855
The chemical composition of the needles of P. pinea, P. pinaster, P. halepensis, P. nigra, P. brutia, P. patula, P. radiata, P. taeda, P. elliotti, P. kesiya, P. sylvestris and P. eldarica was investigated. Headspace solid-phase microextraction and steam distillation extraction were used to collect the volatile fractions. Samples were analyzed using one-dimensional gas chromatography (1D-GC) and comprehensive two-dimensional gas chromatography (GC × GC) associated with a quadrupole and a time-of-flight mass detectors. Results showed that the analytical capabilities of 1D-GC are partially limited by the separation power of the columns. The higher sensibility and the absence of peak skewing of the time-of-flight mass analyzer, with the use of automated peak finding and deconvolution algorithms, allowed for the detection of trace components with qualitative full spectra and the extraction of true mass spectra from coeluting compounds, promoting their reliable identification and thus significantly improving results obtained by 1D-GC/MS, when using a quadrupole mass analyzer. The use of GC × GC resulted in enhanced separation efficiency and increased signal to noise ratio (sensitivity) of the analytes, maximizing mass spectra quality and improving compound detection and identification. This work shows the use of 1D-GC/ToFMS for the analysis of pine needles volatiles, achieving the detection of 177 compounds, that is more than twice the number previously identified by standard 1D-GC/MS. The analysis by GC × GC for the same sample allowed the detection of 212 compounds. The enantioselective GC × GC analysis performed for all the Pinus spp. under study achieved the detection of 422 different compounds. Cross-over phenomena according to operational conditions are highlighted and discussed. 相似文献
103.
H. Hagemann V. D'Anna S. Gomes G. Renaudin K. Yvon 《Journal of Physics and Chemistry of Solids》2011,72(4):286-289
The structural and vibrational properties of the isostructural compounds Ca2FeH6 and Sr2RuH6 are determined by periodic DFT calculations and compared with their previously published experimental crystal structures as well as new experimental vibrational data. The analysis of the vibrational data is extended to the whole series of alkaline-earth iron and ruthenium hydrides A2TH6 (A=Mg, Ca, Sr; T=Fe, Ru) in order to identify correlations between selected frequencies and the T-H bond length. The bulk moduli of Ca2FeH6 and Sr2RuH6 have also been determined within DFT. Their calculated values prove to compare well with the experimental values reported for Mg2FeH6 and several other compounds of this structure. 相似文献
104.
Adamson P Auty DJ Ayres DS Backhouse C Barr G Bishai M Blake A Bock GJ Boehnlein DJ Bogert D Cavanaugh S Cherdack D Childress S Coelho JA Coleman SJ Corwin L Cronin-Hennessy D Danko IZ de Jong JK Devenish NE Diwan MV Dorman M Escobar CO Evans JJ Falk E Feldman GJ Frohne MV Gallagher HR Gomes RA Goodman MC Gouffon P Graf N Gran R Grant N Grzelak K Habig A Harris D Hartnell J Hatcher R Himmel A Holin A Huang X Hylen J Ilic J Irwin GM Isvan Z Jaffe DE James C Jensen D Kafka T Kasahara SM Koizumi G 《Physical review letters》2011,107(1):011802
Results are reported from a search for active to sterile neutrino oscillations in the MINOS long-baseline experiment, based on the observation of neutral-current neutrino interactions, from an exposure to the NuMI neutrino beam of 7.07×10(20) protons on target. A total of 802 neutral-current event candidates is observed in the Far Detector, compared to an expected number of 754 ± 28(stat) ± 37(syst) for oscillations among three active flavors. The fraction f(s) of disappearing ν(μ) that may transition to ν(s) is found to be less than 22% at the 90% C.L. 相似文献
105.
Adamson P Andreopoulos C Armstrong R Auty DJ Ayres DS Backhouse C Barr G Bishai M Blake A Bock GJ Boehnlein DJ Bogert D Cavanaugh S Cherdack D Childress S Choudhary BC Coelho JA Coleman SJ Corwin L Cronin-Hennessy D Danko IZ de Jong JK Devenish NE Diwan MV Dorman M Escobar CO Evans JJ Falk E Feldman GJ Frohne MV Gallagher HR Gomes RA Goodman MC Gouffon P Graf N Gran R Grant N Grzelak K Habig A Harris D Hartnell J Hatcher R Himmel A Holin A Huang X Hylen J Ilic J Irwin GM Isvan Z Jaffe DE 《Physical review letters》2011,106(18):181801
Measurements of neutrino oscillations using the disappearance of muon neutrinos from the Fermilab NuMI neutrino beam as observed by the two MINOS detectors are reported. New analysis methods have been applied to an enlarged data sample from an exposure of 7.25×10(20) protons on target. A fit to neutrino oscillations yields values of |Δm(2)|=(2.32(-0.08)(+0.12))×10(-3) eV(2) for the atmospheric mass splitting and sin(2)(2θ)>0.90 (90% C.L.) for the mixing angle. Pure neutrino decay and quantum decoherence hypotheses are excluded at 7 and 9 standard deviations, respectively. 相似文献
106.
W. T. Cruz A. R. Gomes C. A. S. Almeida 《The European Physical Journal C - Particles and Fields》2011,71(11):1790
In this work we investigate the issue of fermion localization and resonances in (4,1)-deformed branes constructed with one
scalar field coupled with gravity. Such models provide us branes with internal structures that turns the gravitational interaction
more effective for fermions aside the brane, increasing their lifetime. The coupling between the scalar field and spinors
is a necessary condition for fermions to be localized on such branes. After performing a chiral decomposition of the five-dimensional
spinor we found resonances with both chiralities. The correspondence between the spectra for left and right chirality is guaranteed
and Dirac fermions are realized on the brane. 相似文献
107.
Remedio RN Castellar A Barbosa RA Gomes RJ Caetano FH 《Micron (Oxford, England : 1993)》2011,42(5):484-491
The importance of physical exercise practice in the treatment of diabetes has been reported in many studies recently, but only limited data can be found regarding its benefits on liver morphology and protein content of hepatocytes. In order to assess the changes arising from the development of type I diabetes and the benefits of a training protocol, Wistar rats were divided into four groups: sedentary control (SC), trained control (TC), sedentary diabetic (SD) and trained diabetic (TD). The training protocol consisted of swimming for 60 min a day, 5 days/week, during 8 weeks. Liver samples were collected, processed and analyzed by histochemical and ultrastructural techniques. Biochemical tests were also conducted to examine the protein content and quantity of DNA in the liver. In morphological assessment, the presence of areas of cytoplasmic basophilia observed in control subjects was not visualized in sedentary diabetics. It was related to differences in the amount of mitochondria in the cytosol. The mitochondrial structure has not undergone relevant changes, and the number of rough endoplasmic reticulum cisterns was clearly inferior in sedentary diabetics, suggesting lower protein production. However, the biochemical analysis of protein content indicated no statistical differences between groups. The exercise, in turn, was not responsible for major changes in these characteristics. On the whole, the morphological damages arising from type I diabetes were noteworthy. Nevertheless, regular physical training was not responsible for significant improvements in some respects, making evident the need for combined application of a distinct form of treatment. 相似文献
108.
109.
Frederico Caeiro M. Ivette Gomes Björn Vandewalle 《Methodology and Computing in Applied Probability》2014,16(1):1-29
In this paper, for heavy-tailed models and through the use of probability weighted moments based on the largest observations, we deal essentially with the semi-parametric estimation of the Value-at-Risk at a level p, the size of the loss occurred with a small probability p, as well as the dual problem of estimation of the probability of exceedance of a high level x. These estimation procedures depend crucially on the estimation of the extreme value index, the primary parameter in Statistics of Extremes, also done on the basis of the same weighted moments. Under regular variation conditions on the right-tail of the underlying distribution function F, we prove the consistency and asymptotic normality of the estimators under consideration in this paper, through the usual link of their asymptotic behaviour to the one of the extreme value index estimator they are based on. The performance of these estimators, for finite samples, is illustrated through Monte-Carlo simulations. An adaptive choice of thresholds is put forward. Applications to a real data set in the field of insurance as well as to simulated data are also provided. 相似文献
110.