Unravelling the Chemical Morphology of a Mesoporous Titanium Dioxide Interface by Confocal Raman Microscopy: New Clues for Improving the Efficiency of Dye Solar Cells and Photocatalysts

The presence of anatase and rutile domains on nanocrystalline films of P25 TiO(2), as well as the distinct coordination modes of carboxylates on those phases, were revealed by confocal Raman microscopy, a technique that showed to be suitable for imaging the chemical morphology down to submicrometric size.

Thermal analysis of biodegradable microparticles containing ciprofloxacin hydrochloride obtained by spray drying technique

Thermal analysis has been extensively used to obtain information about drug-polymer interactions and to perform pre-formulation studies of pharmaceutical dosage forms. In this work, biodegradable microparticles of poly(D,L-lactide-co-glycolide) (PLGA) containing ciprofloxacin hydrochloride (CP) in various drug:polymer ratios were obtained by spray drying. The main purpose of this study was to investigate the effect of the spray drying process on the drug-polymer interactions and on the stability of microparticles using differential scanning calorimetry (DSC), thermogravimetry (TG) and derivative thermogravimetry (DTG) and infrared spectroscopy (IR). The results showed that the high levels of encapsulation efficiency were dependant on drug:polymer ratio. DSC and TG/DTG analyses showed that for physical mixtures of the microparticles components the thermal profiles were different from those signals obtained with the pure substances. Thermal analysis data disclosed that physical interaction between CP and PLGA in high temperatures had occurred. The DSC and TG profiles for drug-loaded microparticles were very similar to the physical mixtures of components and it was possible to characterize the thermal properties of microparticles according to drug content. These data indicated that the spray dryer technique does not affect the physicochemical properties of the microparticles. In addition, the results are in agreement with IR data analysis demonstrating that no significant chemical interaction occurs between CP and PLGA in both physical mixtures and microparticles. In conclusion, we have found that the spray drying procedure used in this work can be a secure methodology to produce CP-loaded microparticles. (C) 2007 Elsevier B.V. All rights reserved.

Ex Situ Scanning Electrochemical Microscopy (SECM) Investigation of Bismuth- and Bismuth/Lead Alloy Film-Modified Gold Electrodes in Alkaline Medium

Scanning electrochemical microscopy (SECM) in feedback mode was employed to characterise the reactivity and microscopic peculiarities of bismuth and bismuth/lead alloys plated onto gold disk substrates in 0.1 molL(-1) NaOH solutions. Methyl viologen was used as redox mediator, while a platinum microelectrode was employed as the SECM tip. The metal films were electrodeposited ex situ from NaOH solutions containing either bismuth ions only or both bismuth and lead ions. Approach curves and SECM images indicated that the metal films were conductive and locally reactive with oxygen to provide Bi(3+) and Pb(2+) ions. The occurrence of the latter chemical reactions was verified by local anodic stripping voltammetry (ASV) at the substrate solution interface by using a mercury-coated platinum SECM tip. The latter types of measurements allowed also verifying that lead was not uniformly distributed onto the bismuth film electrode substrate. These findings were confirmed by scanning electron microscopy images. The surface heterogeneity produced during the metal deposition process, however, did not affect the analytical performance of the bismuth coated gold electrode in anodic stripping voltammetry for the determination of lead in alkaline media, even in aerated aqueous solutions. Under the latter conditions, stripping peak currents proportional to lead concentration with a satisfactory reproducibility (within 5% RSD) were obtained.

Investigation of the drying process of linseed oil using FTIR and ToF-SIMS

The drying process of linseed oil, oxidized at 80 oC, has been investigated with rheology measurements, Fourier transformation infrared spectroscopy (FTIR), and time of flight secondary ion mass spectrometry (ToF-SIMS). The drying process can be divided into three main steps: initiation, propagation and termination. ToF-SIMS spectra show that the oxidation is initiated at the linolenic (three double bonds) and linoleic fatty acids (two double bonds). ToF-SIMS spectra reveal peaks that can be assigned to ketones, alcohols and hydroperoxides. In this article it is shown that FTIR in combination with ToF-SIMS are well suited tools for investigations of various fatty acid components and reaction products of linseed oil.

Optimization of osmotic dehydration of papaya followed by air-drying

FERNANDES, Fabiano A. N. et al. Optimization of Osmotic Dehydration of Papaya of followed by air-drying. Food Research Internation, v. 39, p. 492-498, 2006.

Al-based anodic oxide films structure observation using field emission gun scanning electron microscopy

In the present work, the anodic oxide films of Al, Al-Cu 4.5% and Al-Si 6.5% alloys are formed using direct and pulse current. In the case of Al-Cu and Al-Si alloys, the electrolyte used contains sulfuric acid and oxalic acid, meanwhile for Al the electrolyte contains sulfuric acid only. Al-Cu alloy was submitted to a heat treatment in order to decrease the effect of inter metallic phase theta upon the anodic film structure. Fractured samples were observed using a field emission gun scanning electron microscope JSM-6330F at (LME)/Brazilian Synchrotron Light Laboratory (LNLS), Campinas, SP, Brazil. The oxide film images enable evaluation of the pore size and form with a resolution similar to the transmission electron microscope (TEM) resolution. It is also observed that the anodizing process using pulse current produces an irregular structure of pore walls, and by direct cur-rent it is produced a rectilinear pore wall. (c) 2005 Elsevier B.V. All rights reserved.

A scanning electron microscopy study of the seed and post-seminal development in Angelonia salicariifolia Bonpl. (Scrophulariaceae)

The external morphology of seeds and post-germination developmental stages of Angelonia salicariifolia Bonpl. (Scrophulariaceae) were investigated using scanning electron microscopy. Some structural features of the seed exotesta and seedling in Angelonia are presented for the first time and are of potential taxonomic value for this neotropical genus. The seeds are very small (0.9-1.7 mm long and 0.5-0.9 mm wide), ovate, with a reticulate-crested exotesta, reticules arranged uniformly in longitudinal rows, with a high density of microcilia-like projections on the cell wall of the reticule base and on the edge of the crests. The hilum is located beside the micropyle at the narrow end of the seed. Germination is epigeal. During germination the radicle develops, followed by elongation of the hypocotyl and primary root. At this stage dense root hairs develop on the lower part of the hypocotyl. The apical bud-located between the cotyledons-begins to develop after the cotyledons have unfolded. The cotyledons are equal in size, sessile and ovate. The seedlings have two types of trichomes, one characteristic of the cotyledons and first pair of leaves (glandular, sessile, four-celled head with quadrangular shape) and the other characteristic of the hypocotyl and epicotyl (stalked, erect, elongate and three-celled with dome-shaped unicellular head). (C) 2001 Annals of Botany Company.

Identification of new isolates of Bacillus thuringiensis using rep-PCR products and delta-endotoxin electron microscopy

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Preparação e carcterização de complexos multicomponentes contendo ciclodextrinas e benznidazol

The benznidazole (BNZ) is the only alternative for Chagas disease treatment in Brazil. This drug has low solubility, which restricts its dissolution rate. Thus, the present work aimed to study the BNZ interactions in binary systems with beta cyclodextrin (β-CD) and hydroxypropyl-beta cyclodextrin (HP-β-CD), in order to increase the apparent aqueous solubility of drug. The influence of seven hydrophilic polymers, triethanolamine (TEA) and 1-methyl-2- pyrrolidone (NMP) in benznidazole apparent aqueous solubility, as well as the formation of inclusion complexes was also investigated. The interactions in solution were predicted and investigated using phase solubility diagram methodology, nuclear magnetic resonance of protons (RMN) and molecular modeling. Complexes were obtained in solid phase by spray drying and physicochemical characterization included the UV-Vis spectrophotometric spectroscopy in the infrared region, scanning electron microscopy, X-ray diffraction and dissolution drug test from the different systems. The increment on apparent aqueous solubility of drug was achieved with a linear type (AL) in presence of both cyclodextrins at different pH values. The hydrophilic polymers and 1-methyl-2-pyrrolidone contributes to the formation of inclusion complexes, while the triethanolamine decreased the complex stability constant (Kc). The log-linear model applied for solubility diagrams revealed that both triethanolamine and 1-methyl-2-pyrrolidone showed an action cosolvent (both solvents) and complexing (1-methyl-2-pyrrolidone). The best results were obtained with complexes involving 1-methyl-2-pyrrolidone and hydroxypropylbeta- cyclodextrin, with an increased of benznidazole solubility in 27.9 and 9.4 times, respectively. The complexes effectiveness was proven by dissolution tests, in which the ternary complexes and physical mixtures involving 1-methyl- 2-pyrrolidone and both cyclodextrins investigated showed better results, showing the potential use as novel pharmaceutical ingredient, that leads to increased benznidazole bioavailability

Micropartículas de poli (ácido láctico)/ poloxámero obtids por spray drying para liberação modificada de metotrexatro

New drug delivery systems have been used to increase chemotherapy efficacy due the possible drug resistance of cancer cells. Poly (lactic acid) (PLA) microparticles are able to reduce toxicity and prolong methotrexate (MTX) release. In addition, the use of PLA/poloxamer polymer blends can improve drug release due to changes in the interaction of particles with biological surfaces. The aim of this study was developing spray dried biodegradable MTX-loaded microparticles and evaluate PLA interactions with different kinds of Pluronic® (PLUF127 and PLUF68) in order to modulate drug release. The variables included different drug:polymer (1:10, 1:4.5, 1:3) and polymer:copolymer ratios (25:75, 50:50, 75:25). The precision and accuracy of spray drying method was confirmed assessing drug loading into particles (75.0- 101.3%). The MTX/PLA microparticles showed spherical shape with an apparently smooth surface, which was dependent on the PLU ratio used into blends particles. XRD and thermal analysis demonstrated that the drug was homogeneously dispersed into polymer matrix, whereas the miscibility among components was dependent on the used polymer:copolymer ratio. No new drug- polymer bond was identified by FTIR analysis. The in vitro performance of MTX-loaded PLA microparticles demonstrated an extended-release profile fitted using Korsmeyer- Peppas kinetic model. The PLU accelerated drug release rate possible due PLU leached in the matrix. Nevertheless, drug release studies carried out in cell culture demonstrated the ability of PLU modulating drug release from blend microparticles. This effect was confirmed by cytotoxicity observed according to the amount of drug released as a function of time. Thus, studied PLU was able to improve the performance of spray dried MTX-loaded PLA microparticles, which can be successfully used as carries for modulated drug delivery with potential in vivo application

Transmission electron microscopy for characterization of acrosomal damage after Percoll gradient centrifugation of cryopreserved bovine spermatozoa

The objective of this study was to characterize acrosomal ultrastructure following discontinuous Percoll gradient centrifugation of cryopreserved bovine sperm. Semen was collected from six bulls of different breeds and three ejaculates per bull were evaluated. Frozen semen samples were thawed and the acrosomal region of sperm cells was evaluated by transmission electron microscopy (TEM) before (n = 18) and after (n = 18) Percoll centrifugation. The evaluation of 20 sperm heads from each of the 36 samples analyzed ensured that a large number of cells were investigated. The data were subjected to analysis of variance at a level of significance of 5%. Percoll centrifugation reduced the percentage of sperm exhibiting normal acrosomes (from 61.77 to 30.24%), reduced the percentage of sperm presenting atypical acrosome reactions (from 28.38 to 4.84%) and increased the percentage of sperm exhibiting damage in the acrosome (from 6.14 to 64.26%). The percentage of sperm with typical acrosome reactions was not significantly different before (3.70%) and after (0.67%) centrifugation. TEM distinguished four different types of acrosomal status and enabled ultrastructural characterization of acrosomal injuries. The percentage of sperm exhibiting normal acrosomes decreased and damage in the acrosome was the most frequent acrosomal injury with the Percoll gradient centrifugation protocol utilized.

Use of scanning electron microscopy for the evaluation of intestinal epithelium integrity

Propõe-se, neste trabalho, o uso de microscopia eletrônica de varredura para avaliar perda de epitélio intestinal da mucosa intestinal de pintos machos e fêmeas submetidos a prolongado jejum pós-eclosão de água e ração. Dois segmentos do duodeno, jejuno e íleo por ave foram coletados e processados pelo método de rotina para microscopia eletrônica de varredura. Seis diferentes graus de perda de epitélio intestinal foram determinados: grau 0, vilos normais, sem extrusão; grau 1, vilos com pequenos pontos de extrusão; grau 2, vilos com perda de epitélio no ápice; grau 3, vilos com perda de epitélio na região apical; grau 4, vilos com perda de epitélio em sua metade superior; grau 5: vilos sem epitélio; grau 6: vilo quebrado. As três regiões intestinais das fêmeas apresentaram aproximadamente 90% de seus vilos normais (graus 0 e 1), enquanto nos machos ocorreu 38% de vilos normais no duodeno e jejuno e 85% no íleo. Além disso, machos apresentaram graus mais acentuados de perda de epitélio (graus 3, 4, 5 e 6) que as fêmeas (grau 3). Os dados indicaram que a mucosa intestinal de pintos machos é mais sensível a prolongado jejum pós-eclosão que a de pintos fêmeas. A microscopia eletrônica de varredura pode ser usada como um método de rotina seguro para a caracterização e quantificação de perda de epitélio intestinal.

Observation of the embryonic development in Pseudoplatystoma coruscans (Siluriformes: Pimelodidae) under light and scanning electron microscopy

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Early development of Astronotus ocellatus under stereomicroscopy and scanning electron microscopy

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)