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31.
A. L. M. Nasser L. P. Mazzolin C. A. Hiruma-Lima L. S. Santos M. N. Eberlin A. R. Monteiro de Souza Brito W. Vilegas 《Chromatographia》2006,64(11-12):695-699
The methanolic extract of the bark of the medicinal plant Qualea parviflora (Vochysiaceae) contains new nor-seco-triterpene and pentacyclic triterpenoids. They were separated in a preparative scale using droplet counter-current chromatography. The optimum solvent used was composed of a mixture of CHCl3/MeOH/H2O (43:37:20, v/v) in the descending mode and led to a successful separation of the new compound 28-nor-17, 22-seco-2α, 3β, 19, 22, 23-pentahydroxy-Δ12-oleanane, besides the known triterpenoids bellericagenin B, bellericaside B and arjunglucoside I . Identification was performed by ESI-MS, 1H NMR and 13C NMR analyses. 相似文献
32.
Hiléia K. S. Souza V. R. da Silveira F. M. M. Borges Dulce M. A. Melo H. Scatena Jr. O. A. de Oliveira A. G. Souza 《Journal of Thermal Analysis and Calorimetry》2007,87(2):433-436
Thermal behavior of rare earth nitrate complexes
with 2-azacyclononanone (AZA) with Ln(NO3)3·3(AZA)
composition (where Ln=Gd, Er and Ho) was
analyzed in kinetic point of view. Kinetic parameters were calculated from
thermogravimetric data. All obtained results were similar. The first decomposition
step was representative to the loss of ligand and the residue was essentially
Ln2O3. Furthermore, a reaction
path was proposed for the thermal decomposition of the Ln(NO3)3·3(AZA). 相似文献
33.
E. M. Araújo Renata Barbosa Amanda D. Oliveira Crislene R. S. Morais T. J. A. deMélo A. G. Souza 《Journal of Thermal Analysis and Calorimetry》2007,87(3):811-814
Polyethylene/montmorillonite clay nanocomposites were obtained via direct
melt intercalation. The clay was organically modified with four different
types of quaternary ammonium salts. The objective of this work is to study
the use of montmorillonite clay in the production of nanocomposites by means
on rheological, mechanical and crystallization properties of nanocomposites
and to compare to the properties of the matrix and PE/unmodified clay nanocomposites.
In general, the tensile test showed that the yield strength and modulus of
the nanocomposites are close to the pure PE. Apparently, the mixture with
Dodigen salt seems to be more stable than the pure PE and PE/unmodified clay. 相似文献
34.
Huenerbein A Sipoli Marques MA Pereira Ados S de Aquino Neto FR 《Journal of chromatography. A》2003,985(1-2):375-386
The Medical Commission of the International Olympic Committee forbids the use of anabolic androgenic steroids and beta2-agonists to improve athletic performance. In this work we have selected examples of anabolic androgenic compounds and their metabolites to evaluate the GC-MS analysis of some trimethylsilyl derivatives. The aim is to set the best GC conditions to improve the detection within the whole range of analyte elution temperatures. The initial column temperature was changed to 105 or 140 degrees C followed by 40 degrees C min(-1) to 200 degrees C and then 15 degrees C min(-1) to 300 degrees C. Using 140 degrees C as the initial oven temperature it was possible to obtain narrower initial analyte distributions for the compounds that elutes at the beginning of the chromatogram as clenbuterol, mabuterol, epimethylenediol and norandrosterone, without loss of derivatized metabolites signal. Later. eluting analytes, such as the stanozolol metabolites, furazabol and oxandrolone were not affected. Temperatures below 140 degrees C. resulted in partial derivatization for some analytes mainly stanozolol related structures. Therefore evaluation of derivatization conditions as occurring in three steps, the vial, vaporization chamber and capillary column, was thoroughly assessed. The new program temperature improves the signal-to-noise ratio for some compounds and shows adequate resolution for endogenous compounds. Some of the difficult key separations necessary for doping control enforcement were also obtained with the proposed method. 相似文献
35.
Rodrigo Cardoso Magno Lorian Cobra Straker Wanderley de Souza Marcia Attias 《Microscopy and microanalysis》2005,11(2):166-174
Toxoplasma gondii, the causative agent of toxoplasmosis, is capable of actively penetrating and multiplying in any nucleated cell of warm-blooded animals. Its survival strategies include escape from fusion of the parasitophorous vacuole with host cell lysosomes and rearrangement of host cell organelles in relation to the parasitophorous vacuole. In this article we report the rearrangement of host cell organelles and elements of the cytoskeleton of LLCMK2 cells, a lineage derived from green monkey kidney epithelial cells, in response to infection by T. gondii tachyzoites. Transmission electron microscopy made on flat embedded monolayers cut horizontally to the apical side of the cells or field emission scanning electron microscopy of monolayers scraped with scotch tape before sputtering showed that association of mitochondria to the vacuole is much less frequent than previously described. On the other hand, all parasitophorous vacuoles were surrounded by elements of the endoplasmic reticulum. These data were complemented by observations by laser scanning microscopy using fluorescent probes from mitochondria and endoplasmic reticulum and reinforced by three-dimensional reconstruction from serial sections observed by transmission electron microscopy and labeling of mitochondria and endoplasmic reticulum by fluorescent probes. 相似文献
36.
Magno Aparecido G. Trindade Glaucia Maria da Silva Valdir Souza Ferreira 《Microchemical Journal》2005,81(2):209-216
This work presents an electroanalytical methodology developed for square-wave voltammetry based in the electrochemical reduction in hanging mercury drop electrode (HMDE), which is simple, fast, reliable and sensitive for determination of moxifloxacin (MOXI) in tablets and spiked urine human samples. The support electrolyte that provided a more defined and intense peak current for MOXI determination was the phosphate buffer 0.04 mol l− 1 pH 8.0. In the best-optimized conditions the drug presented an only peak of reduction at − 1.38 V vs. Ag/AgCl, using an Eacc. of − 0.30 V. An LOD of 0.44 and 3.20 ng ml− 1 and an LOQ of 1.46 and 10.60 ng ml− 1 were found for the pure standard of moxifloxacin and in the presence of matrix, respectively. A good recovery was obtained for assay spiked urine samples and a good quantification of MOXI was achieved in a commercial formulation. The methodology proposed was more sensitive than the spectrofluorimetric and spectrophotometric method with precision and accuracy equivalent. 相似文献
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