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1.
Langmuir ; 31(46): 12727-35, 2015 Nov 24.
Artigo em Inglês | MEDLINE | ID: mdl-26488233

RESUMO

In this work, we describe a method for the production of porous polymer materials in the form of particles characterized by narrow pore size distribution using the principle of shear-induced reactive gelation. Poly(styrene-co-divinylbenzene) primary particles with diameter ranging from 80 to 200 nm are used as building blocks, which are assembled into fractal-like clusters when exposed to high shear rates generated in a microchannel. It was found that independent of the primary particle size, it is possible to modulate the internal structure of formed fractal-like aggregates having fractal dimension ranging from 2.4 to 2.7 by varying the residence time in the microchannel. Thermally induced postpolymerization was used to increase the mechanical resilience of such formed clusters. Primary particle interpenetration was observed by SEM and confirmed by light scattering resulting in an increase of fractal dimension. Nitrogen sorption measurements and mercury porosimetry confirmed formation of a porous material with surface area ranging from 20 to 40 m(2)/g characterized by porosity of 70% and narrow pore size distribution with an average diameter around 700 nm without the presence of any micropores. The strong perfusive character of the synthesized material was confirmed by the existence of a plateau of the height equivalent to a theoretical plate measured at high reduced velocities using a chromatographic column packed with the synthesized microclusters.


Assuntos
Fenômenos Mecânicos , Polímeros/química , Géis , Tamanho da Partícula , Polimerização , Porosidade
2.
J Chromatogr A ; 1386: 13-21, 2015 Mar 20.
Artigo em Inglês | MEDLINE | ID: mdl-25683627

RESUMO

A new strong cation exchanger (SCX) monolithic column was synthesized by at-line surface modification of a cryogel prepared by copolymerization of 2-hydroxyethylmethacrylate (HEMA) and glycidylmethacrylate (GMA). Sodium salt of 3-Mercaptopropane sulfonic acid (3-MPS) was used as the ligand to transform the surface of the monolith into a strong cation exchanger. The obtained material was characterized in terms of elemental analysis, infrared spectroscopy (FTIR), Scanning Electron Microscopy (SEM), Brunauer-Emmett-Teller (BET) N2 adsorption, and used as a stationary phase for strong-cation exchange chromatography of some proteins, such as α-chymotrypsinogen, cytochrome c and lysozyme. Water permeability of the column was calculated according to Darcy's law (2.66×10(-13)m(2)). The performance of the monolithic cryogel column was evaluated on the basis of Height Equivalent to a Theoretical Plate (HETP). Retention behavior of the studied proteins was modeled on the basis of Yamamoto model to understand the role of the ion-exchange mechanism in retention behaviors. The considered proteins were successfully separated, and the obtained chromatogram was compared with that obtained with a non-functionalized cryogel column.


Assuntos
Cromatografia por Troca Iônica , Criogéis/química , Proteínas/química , Ácidos Sulfônicos/química , Adsorção , Resinas de Troca de Cátion/análise , Cátions/química , Quimotripsinogênio/química , Quimotripsinogênio/isolamento & purificação , Citocromos c/química , Citocromos c/isolamento & purificação , Metacrilatos/química , Microscopia Eletrônica de Varredura , Muramidase/química , Muramidase/isolamento & purificação , Proteínas/isolamento & purificação , Espectroscopia de Infravermelho com Transformada de Fourier
3.
J Sep Sci ; 34(16-17): 2159-63, 2011 Aug.
Artigo em Inglês | MEDLINE | ID: mdl-21796787

RESUMO

Polymeric monolithic stationary phases for HPLC can be produced by Reactive Gelation. Unlike the conventional method of using porogens, such novel process consists of a number of separate steps, thus enabling a better control of the quality of the final material. A suspension of polymer nanoparticles in water is produced and subsequently swollen with hydrophobic monomers. The particles are then destabilised (usually by salt addition) to make them aggregate into a large percolating structure, the so-called monolith. Finally, the added monomer can then be polymerised to harden the structure. In this work, a polystyrene latex is used as the base material and functionalised by introduction of epoxide groups on the surface and subsequent reaction to sulphonic acid groups, yielding a SO3(-) density of 0.7 mmol/g dry material. Morphological investigations show 54% porosity made of 300 nm large pores. Van Deemter measurements of a large protein show no practical influence of diffusion limitations on the plate number. Finally, a preliminary separation of a test protein mixture is shown, demonstrating the potential of using ion-exchange chromatography on Reactive Gelation monoliths.


Assuntos
Resinas de Troca de Cátion/química , Cromatografia Líquida de Alta Pressão/instrumentação , Cromatografia por Troca Iônica/instrumentação , Resinas de Troca de Cátion/síntese química , Cromatografia Líquida de Alta Pressão/métodos , Cromatografia por Troca Iônica/métodos , Interações Hidrofóbicas e Hidrofílicas , Polímeros/síntese química , Polímeros/química , Porosidade , Proteínas/química , Proteínas/isolamento & purificação
4.
Parasitol Res ; 105 Suppl 1: S63-74, 2009 Aug.
Artigo em Inglês | MEDLINE | ID: mdl-19575227

RESUMO

The Central Upper-Rhine (Baden-Württemberg, Germany) is one of the warmest regions in Germany and also harbours abundant numbers of mosquitoes. Case reports on presumably autochthonous occurrence of Dirofilaria spp. were reported previously and were a reason for a further investigation into the occurrence of vector-borne pathogens. For this purpose, 44 hunting dogs from the Central Upper-Rhine region were tested between 4(th) and 29(th) June 2007. The blood samples were tested using the Knott's test and IDEXX SNAP 4Dx test. The Knott's test revealed unsheathed microfilaria identified as Dirofilaria repens by PCR in 3 dogs with no history of travelling (6.8%; 95% CI: 2.4-18.2%). The seroprevalence for Anaplasma phagocytophilum was 43.2% (95% CI: 29.7-57.8%), but only 4.5% (95% CI: 1.3-15.1%) for antibodies to Borrelia C6 peptide. Dirofilaria immitis antigen was not detected in any of the samples. A further 288 blood samples from non-hunting companion dogs of the Central Upper-Rhine region were tested negative for heartworm antigen between February and August 2007.


Assuntos
Dirofilaria/classificação , Dirofilaria/isolamento & purificação , Dirofilariose/epidemiologia , Doenças do Cão/epidemiologia , Anaplasma phagocytophilum/imunologia , Animais , Anticorpos Antibacterianos/sangue , Sangue/parasitologia , Borrelia/imunologia , Doenças do Cão/parasitologia , Cães , Alemanha/epidemiologia , Reação em Cadeia da Polimerase/métodos , Prevalência , Kit de Reagentes para Diagnóstico , Estudos Soroepidemiológicos
5.
Biomaterials ; 26(21): 4383-94, 2005 Jul.
Artigo em Inglês | MEDLINE | ID: mdl-15701367

RESUMO

A hydraulic calcium phosphate cement with beta-tricalcium phosphate (TCP) granules embedded in a matrix of dicalcium phosphate dihydrate (DCPD) was implanted in experimentally created defects in sheep. One type of defect consisted of a drill hole in the medial femoral condyle. The other, partial metaphyseal defect was located in the proximal aspect of the tibia plateau and was stabilized using a 3.5 mm T-plate. The bone samples of 2 animals each per group were harvested after 2, 4, 6 and 8 weeks. Samples were evaluated for cement resorption and signs of immediate reaction, such as inflammation, caused by the cement setting in situ. Differences regarding these aspects were assessed for both types of defects using macroscopical, radiological, histological and histomorphometrical evaluations. In both defects the brushite matrix was resorbed faster than the beta-TCP granules. The resorption front was followed directly by a front of new bone formation, in which residual beta-TCP granules were embedded. Cement resorption occurred through (i) extracellular liquid dissolution with cement disintegration and particle formation, and (ii) phagocytosis of the cement particles through macrophages. Signs of inflammation or immunologic response leading to delayed new bone formation were not noticed at any time. Cement degradation and new bone formation occurred slightly faster in the femur defects.


Assuntos
Implantes Absorvíveis , Cimentos Ósseos/uso terapêutico , Fosfatos de Cálcio/uso terapêutico , Fraturas do Fêmur/diagnóstico , Fraturas do Fêmur/terapia , Consolidação da Fratura/fisiologia , Fraturas da Tíbia/diagnóstico , Fraturas da Tíbia/terapia , Animais , Cimentos Ósseos/química , Fosfatos de Cálcio/química , Feminino , Fraturas do Fêmur/fisiopatologia , Implantes Experimentais , Teste de Materiais , Ovinos , Fraturas da Tíbia/fisiopatologia , Resultado do Tratamento
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