Preparation and characterization of chloroaluminum phthalocyanine-loaded solid lipid nanoparticles by thermal analysis and powder X-ray diffraction techniques

Solid lipid nanoparticles (SLN) without drug and SLN loaded with chloroaluminum phthalocyanine (AlClPc) were prepared by solvent diffusion method in aqueous system and characterized by thermal analyses and X-ray diffraction (XRD) in this study. Determination of particle size, zeta potential (ZP), and encapsulation efficiency were also evaluated. SLN containing AlClPc of nanometer size with high encapsulation efficiency and ZP were obtained. The results indicated that the size of SLN loaded with AlClPc is larger than that of the inert particle, but ZP is not changed significantly with incorporation of the drug. In differential scanning calorimetry (DSC) curves, it was observed that the melting point of stearic acid (SA) isolated and in SLN occurred at 55 and 64 degrees C, respectively, suggesting the presence of different polymorphs. DSC also shows that the crystallinity state of SLN was much less than that of SA isolated. The incorporation of drug in SLN may have been favored by this lower crystallinity degree of the samples. XRD techniques corroborated with the thermal analytic techniques, suggesting the polymorphic modifications of stearic acid.

Influence of milk type and addition of passion fruit peel powder on fermentation kinetics, texture profile and bacterial viability in probiotic yoghurts

The effect of the addition of passion fruit peel powder (PFPP) on the fermentation kinetics and texture parameters, post-acidification and bacteria counts of probiotic yoghurts made with two milk types were evaluated during 28 days of storage at 4 degrees C. Milks were fermented by Streptococcus thermophilus and Lactobacillus delbrueckii subsp. bulgaricus (CY340), and one strain of probiotic bacteria: Lactobacillus acidophilus (L10 and NCFM), Bifidobacterium animalis subsp. lactis (8104 and HN019). The addition of PFPP reduced significantly fermentation time of skim milk co-fermented by the strains L10, NCFM and HN019. At the end of 28-day shelf-life, counts of B. lactis Bl04 were about 1 Log CFU mL(-1) higher in whole yoghurt fermented with PFPP regarding its control but, in general, the addition of PFPP had less influence on counts than the milk type itself. The titratable acidity in yoghurts with PFPP was significantly higher than in their respective controls, and in skim yoghurts higher than in the whole ones. The PFPP increased firmness, consistency (except for the NCFM strain of L acidophilus) and cohesiveness of all skim yoghurts. The results point out the suitability of using passion fruit by-product in the formulation of both skim and whole probiotic yoghurts. (C) 2012 Elsevier Ltd. All rights reserved.

Enterobacteria Isolation in Ostrich Eggs (Struthio camelus)

This study was conducted to determine the presence of enterobacteria in the eggs of ostriches reared on a farm with a history of reproductive failure. Ninety samples from twenty eggs were submitted to bacteriological tests. The results showed Enterobacteria growth in 100% of the eggs. The microorganisms isolated were Hafnia alvei in 50% (10/20), Serratia spp. in 20% (4/20), Escherichia coli in 15% (3/20), and Citrobacter freundii in 15% (3/20). All eggs presented poor eggshell quality, which favored enterobacteria contamination. Hafnia alvei was present only in the internal egg structures (albumen and yolk sac), suggesting the possibility of vertical infection.

Dual function of egg-covering in the Kentish plover Charadrius alexandrinus

Many bird species take recesses during incubation, and while the nests are unattended, the eggs may both be vulnerable to predation and reach suboptimal temperatures for embryo development. Perhaps to avoid these negative possibilities, some birds cover their eggs with materials when they depart from nests. We examined experimentally, using the ground-nesting Kentish plover as model species, whether egg-covering allows egg temperatures to remain within optimal limits for embryogenesis in unattended nests, thus reducing the requirements of contact incubation, and simultaneously maintain the eggs' camouflage. There was a negative relationship between nest attendance and ambient temperature, but only during mid-morning, the period of the day when egg-covering was most frequent. Indeed, during mid-morning egg-covering not only served to better camouflage the eggs, but also to maintain egg temperatures within optimal thermal thresholds for embryogenesis while the nests remained unattended. During other periods of the day, covered eggs in unattended nests overheated (e.g., afternoon) or did not reach the optimal temperature for embryogenesis (e.g., early morning). During periods in which eggs may be uncovered to alleviate overheating, unattended nests may be easier to locate by predators, because the eggs are less well camouflaged. Therefore, camouflage and appropriate thermal environment are inseparable functions of egg-covering in the ground-nesting Kentish plover.

Concurrent crack and powder cocaine users from Sao Paulo: Do they represent a different group?

Abstract Background Cocaine abuse is a serious and socially damaging illegal drug problem. Different routes of administration are associated with a specific progression of use, different degrees of abuse liability, propensity for dependence and treatment response. There have been relatively few studies comparing different cocaine users groups and no studies into the characterization of the group of individuals reporting concurrent use of powder cocaine and crack cocaine. Methods Six hundred and ninety-nine cocaine users were assessed during the period August 1997 to October 1998 in one outpatient and six inpatient clinics located in the São Paulo, Brazil. Patients were interviewed using a structured questionnaire schedule in Portuguese, designed specifically for the Brazilian population. The statistical analyses were performed using either ANOVA or a chi-squared test and focusing on their preferred form of use/route of administration and other variables. Results For 83% of the variables tested in this study, the Dual Users subgroup (using both powder and crack cocaine) demonstrated statistical differences from the single drug user subgroups. Those differences include the initiation of cocaine, the abuse of other illicit drugs, and rates of criminal history. Conclusion These data suggest cocaine-dependent individuals who report use of both powder and crack cocaine are an at least partially, distinct subgroup. However, further studies will be necessary to confirm this and to determine if they also show a different treatment response.

Adição de carotenóides naturais e artificiais na alimentação de galinhas poedeiras: efeitos na qualidade de ovos frescos e armazenados

A pesquisa teve como objetivo avaliar os atributos de qualidade e de durabilidade dos ovos de duas diferentes linhagens de poedeiras, com dietas contendo aditivos artificiais ou naturais, em diferentes períodos de armazenamento. Foram quantificadas durante o armazenamento as variáveis perda de peso, pH da gema e albúmen, gravidade específica, índice de gema (IG) e foi realizada também classificação por peso e Unidade Haugh (UH). Os resultados foram avaliados segundo teste de Tukey (P≤0,05). As linhagens diferiram quanto à classificação extra dos ovos, com maior porcentagem para a Isa Brown. Os ovos obtidos das poedeiras Carijó apresentaram maior porcentagem de gema (Carijó 30,66 e Isa-Brown 24,55). O tempo de armazenamento fez com que a porcentagem de gema aumentasse nas duas linhagens (Carijó 30,66 tempo zero para 34,85 depois de 36 dias; e Isa- Brown de 24,55 para 27,48). As dietas com aditivos artificiais ou naturais não influenciaram a porcentagem de clara (% Clara 58,72 Controle; 59,52 Aditivo; 60,11 Urucum 1,5%; 59,43 e de gema %Gema 27,64 Controle; 27,90 Aditivo; 27,21 Urucum 1,5%; 27,66 Urucum 2%). O pH da clara diferiu entre os tratamentos no tempo inicial e aos 36 dias de armazenamento, mas o pH da gema não diferiu durante todo o armazenamento. O índice de gema diferiu nos tempos de armazenamento, mas não diferiu considerando os tratamentos. Em dietas com aditivos artificiais ou naturais, as linhagens e os tempos de armazenamento influenciam na qualidade e durabilidade dos ovos.

On Ti-18Si-6B and Ti-7.5Si-22.5B powder alloys prepared by high-energy ball milling and sintering

Recently, a new ternary phase was discovered in the Ti-Si-B system, located near the Ti6Si2B composition. The present study concerns the preparation of titanium alloys that contain such phase mixed with α-titanium and other intermetallic phases. High-purity powders were initially processed in a planetary ball-mill under argon atmosphere with Ti-18Si-6B and Ti-7.5Si-22.5B at. (%) initial compositions. Variation of parameters such as rotary speed, time, and ball diameters were adopted. The as-milled powders were pressureless sintered and hot pressed. Both the as-milled and sintered materials were characterized by X-ray diffraction, scanning electron microscopy and energy-dispersive spectrometry. Sintered samples have presented equilibrium structures formed mainly by the α-Ti+Ti6Si2B+Ti5Si3+TiB phases. Silicon and boron peaks disappear throughout the milling processes, as observed in the powder diffraction data. Furthermore, an iron contamination of up to 10 at. (%) is measured by X-ray spectroscopy analysis on some regions of the sintered samples. Density, hardness and tribological results for these two compositions are also presented here.

Enterobacteria isolation in ostrich eggs (Struthio Camelus)

This study was conducted to determine the presence of enterobacteria in the eggs of ostriches reared on a farm with a history of reproductive failure. Ninety samples from twenty eggs were submitted to bacteriological tests. The results showed Enterobacteria growth in 100% of the eggs. The microorganisms isolated were Hafnia alvei in 50% (10/20), Serratia spp. in 20% (4/20), Escherichia coli in 15% (3/20), and Citrobacter freundii in 15% (3/20). All eggs presented poor eggshell quality, which favored enterobacteria contamination. Hafnia alvei was present only in the internal egg structures (albumen and yolk sac), suggesting the possibility of vertical infection.

Photoluminescence of core-shell nanoparticles made from yttrium stabilized zirconia powder grain coated with alumina

A YSZ@Al2O3 nanocomposite was obtained by Al2O3 coating on the surface of yttrium stabilized zirconia via a polymeric precursor method. The resulting core–shell structures were characterized by X-ray diffraction, scanning electron microscopy, transmission electronic microscopy and PL spectra. The TEM micrographs clearly show a homogeneous Al2O3 shell around the ZrO2 core. The observed PL is related to surface–interface defects. Such novel technologies can, in principle, explore materials which are not available in the bulk single crystal form but their figure-of-merit is dramatically dependent on the surface–interface defect states.

Studies of Inorganic Layer and Framework Structures Using Time-, Temperature- and Pressure-Resolved Powder Diffraction Techniques

This thesis is concerned with in-situ time-, temperature- and pressure-resolved synchrotron X-ray powder diffraction investigations of a variety of inorganic compounds with twodimensional layer structures and three-dimensional framework structures. In particular, phase stability, reaction kinetics, thermal expansion and compressibility at non-ambient conditions has been studied for 1) Phosphates with composition MIV(HPO4)2·nH2O (MIV = Ti, Zr); 2) Pyrophosphates and pyrovanadates with composition MIVX2O7 (MIV = Ti, Zr and X = P, V); 3) Molybdates with composition ZrMo2O8. The results are compiled in seven published papers and two manuscripts. Reaction kinetics for the hydrothermal synthesis of α-Ti(HPO4)2·H2O and intercalation of alkane diamines in α-Zr(HPO4)2·H2O was studied using time-resolved experiments. In the high-temperature transformation of γ-Ti(PO4)(H2PO4)·2H2O to TiP2O7 three intermediate phases, γ'-Ti(PO4)(H2PO4)·(2-x)H2O, β-Ti(PO4)(H2PO4) and Ti(PO4)(H2P2O7)0.5 were found to crystallise at 323, 373 and 748 K, respectively. A new tetragonal three-dimensional phosphate phase called τ-Zr(HPO4)2 was prepared, and subsequently its structure was determined and refined using the Rietveld method. In the high-temperature transformation from τ-Zr(HPO4)2 to cubic α-ZrP2O7 two new orthorhombic intermediate phases were found. The first intermediate phase, ρ-Zr(HPO4)2, forms at 598 K, and the second phase, β-ZrP2O7, at 688 K. Their respective structures were solved using direct methods and refined using the Rietveld method. In-situ high-pressure studies of τ-Zr(HPO4)2 revealed two new phases, tetragonal ν-Zr(HPO4)2 and orthorhombic ω-Zr(HPO4)2 that crystallise at 1.1 and 8.2 GPa. The structure of ν-Zr(HPO4)2 was solved and refined using the Rietveld method. The high-pressure properties of the pyrophosphates ZrP2O7 and TiP2O7, and the pyrovanadate ZrV2O7 were studied up to 40 GPa. Both pyrophosphates display smooth compression up to the highest pressures, while ZrV2O7 has a phase transformation at 1.38 GPa from cubic to pseudo-tetragonal β-ZrV2O7 and becomes X-ray amorphous at pressures above 4 GPa. In-situ high-pressure studies of trigonal α-ZrMo2O8 revealed the existence of two new phases, monoclinic δ-ZrMo2O8 and triclinic ε-ZrMo2O8 that crystallises at 1.1 and 2.5 GPa, respectively. The structure of δ-ZrMo2O8 was solved by direct methods and refined using the Rietveld method.

Combined levels of carotenoids and vitamin E in diets for gilthead seabream broodstocks (Sparus aurata L.): effect on the quality of egg spawning and composition

Watanabe et al. (1991 a,b) state that, vitamin E and carotenoids perform an essential role on the quality of egg spawning. Vitamin E is one of the main nutrients for the reproduction of fish (Izquierdo et al., 2001), and it has been proved that its inclusion in diets for broodstocks favors the quality of egg spawning in several species of fish (Watanabe and Takashima,1977; Takeuchi et al., 1981; Watanabe et al., 1985, 1991 a,b; Sutjaritvongsanon, 1987; Watanabe, 1990; Schimittou, 1993; Mushiake et al., 1993; Dube, 1996; Shiranee and Natarajan, 1996; Izquierdo et al., 2001; Morehead et al., 2001; Fernández- Palacios et al., 2005). On the other hand, the carotenoids which also perform an antioxidizing function (including the protection of lipids from oxidation), have been involved in the reproductive processes of marine organisms: crustaceans (Liñan-Cabello et al., 2002), marine fish (Watanabe y Kiron, 1995; Verakunpiriya et al., 1997 a,b; Vassallo-Agius et al., 2001 a,b,c, 2002; Watanabe and Vassallo-Agius 2003) and fresh water fish (Ahmadi et al., 2006). The results of this study suggest that the recommended levels of n-3 HUFA in diets for gilthead sea bream broodstocks could be increased up to 3,5 % when supplemented jointly with carotenoids from paprika oleoresin and vitamin E, thus favoring the quality of spawning.

Dose-dependent effect of a single GnRHa injection on the spawning of meagre ("Argyrosomus regius") broodstock reared in captivity

[EN]The present study aimed to determine the spawning efficacy, egg quality and quantity of captive breed meagre induced with a single gonadotrophin-releasing hormone agonist (GnRHa) injection of 0, 1, 5, 10, 15, 20, 25, 30, 40 or 50 μg kg–1 to determine a recommended optimum dose to induce spawning. The doses 10, 15 and 20 μg kg–1 gave eggs with the highest quality (measured as: percentage of viability, floating, fertilisation and hatch) and quantity (measured as: total number of eggs, number of viable eggs, number of floating eggs, number of hatched larvae and number of larvae that reabsorbed the yolk sac). All egg quantity parameters were described by Gaussian regression analysis with R2 = 0.89 or R2 = 0.88. The Gaussian regression analysis identified that the optimal dose used was 15 μg kg–1. The regression analysis highlighted that this comprehensive study examined doses that ranged from low doses insufficient to stimulate a high spawning response (significantly lower egg quantities, p < 0.05) compared to 15 μg kg–1 through to high doses that stimulated the spawning of significantly lower egg quantities and eggs with significantly lower quality (egg viability). In addition, the latency period (time from hormone application to spawning) decreased with increasing doses to give a regression (R2 = 0.93), which suggests that higher doses accelerated oocyte development that in turn reduced egg quality and quantity. The identification of an optimal dose for the spawning of meagre, which has high aquaculture potential, represents an important advance for the Mediterranean aquaculture industry.

Bioactive and toxic compounds in different foodstuffs: analytical techniques and sensory analysis

Foods that provide medical and health benefits or have a role in disease risk prevention are termed functional foods. The functionality of functional foods is derived from bioactive compounds that are extranutritional constituents present in small quantities in food. Bioactive components include a range of chemical compounds with varying structures such as carotenoids, flavonoids, plant sterols, omega-3 fatty acids (n-3), allyl and diallyl sulfides, indoles (benzopyrroles), and phenolic acids. The increasing consumer interest in natural bioactive compounds has brought about a rise in demand for these kinds of compounds and, in parallel, an increasing number of scientific studies have this type of substance as main topic. The principal aim of this PhD research project was the study of different bioactive and toxic compounds in several natural matrices. To achieve this goal, chromatographic, spectroscopic and sensorial analysis were performed. This manuscript reports the main results obtained in the six activities briefly summarized as follows: • SECTION I: the influence of conventional packaging on lipid oxidation of pasta was evaluated in egg spaghetti. • SECTION II: the effect of the storage at different temperatures of virgin olive oil was monitored by peroxide value, fatty acid activity, OSI test and sensory analysis. • SECTION III: the glucosinolate and phenolic content of 37 rocket salad accessions were evaluated, comparing Eruca sativa and Diplotaxis tenuifolia species. Sensory analysis and the influence of the phenolic and glucosinolate composition on sensory attributes of rocket salads has been also studied. • SECTION IV: ten buckwheat honeys were characterised on the basis of their pollen, physicochemical, phenolic and volatile composition. • SECTION V: the polyphenolic fraction, anthocyanins and other polar compounds, the antioxidant capacity and the anty-hyperlipemic action of the aqueous extract of Hibiscus sabdariffa were achieved. • SECTION VI: the optimization of a normal phase high pressure liquid chromatography–fluorescence detection method for the quantitation of flavanols and procyanidins in cocoa powder and chocolate samples was performed.

Mechanical microcontacts of powder particles studied with the quartz crystal microbalance

Within this work, a particle-polymer surface system is studied with respect to the particle-surface interactions. The latter are governed by micromechanics and are an important aspect for a wide range of industrial applications. Here, a new methodology is developed for understanding the adhesion process and measure the relevant forces, based on the quartz crystal microbalance, QCM. rnThe potential of the QCM technique for studying particle-surface interactions and reflect the adhesion process is evaluated by carrying out experiments with a custom-made setup, consisting of the QCM with a 160 nm thick film of polystyrene (PS) spin-coated onto the quartz and of glass particles, of different diameters (5-20µm), deposited onto the polymer surface. Shifts in the QCM resonance frequency are monitored as a function of the oscillation amplitude. The induced frequency shifts of the 3rd overtone are found to decrease or increase, depending on the particle-surface coupling type and the applied oscillation (frequency and amplitude). For strong coupling the 3rd harmonic decreased, corresponding to an “added mass” on the quartz surface. However, positive frequency shifts are observed in some cases and are attributed to weak-coupling between particle and surface. Higher overtones, i.e. the 5th and 7th, were utilized in order to derive additional information about the interactions taking place. For small particles, the shift for specific overtones can increase after annealing, while for large particle diameters annealing causes a negative frequency shift. The lower overtones correspond to a generally strong-coupling regime with mainly negative frequency shifts observed, while the 7th appears to be sensitive to the contact break-down and the recorded shifts are positive.rnDuring oscillation, the motion of the particles and the induced frequency shift of the QCM are governed by a balance between inertial forces and contact forces. The adherence of the particles can be increased by annealing the PS film at 150°C, which led to the formation of a PS meniscus. For the interpretation, the Hertz, Johnson-Kendall-Roberts, Derjaguin-Müller-Toporov and the Mindlin theory of partial slip are considered. The Mindlin approach is utilized to describe partial slip. When partial slip takes place induced by an oscillating load, a part of the contact ruptures. This results in a decrease of the effective contact stiffness. Additionally, there are long-term memory effects due to the consolidation which along with the QCM vibrations induce a coupling increase. However, the latter can also break the contact, lead to detachment and even surface damage and deformation due to inertia. For strong coupling the particles appear to move with the vibrations and simply act as added effective mass leading to a decrease of the resonance frequency, in agreement with the Sauerbrey equation that is commonly used to calculate the added mass on a QCM). When the system enters the weak-coupling regime the particles are not able to follow the fast movement of the QCM surface. Hence, they effectively act as adding a “spring” with an additional coupling constant and increase the resonance frequency. The frequency shift, however, is not a unique function of the coupling constant. Furthermore, the critical oscillation amplitude is determined, above which particle detach. No movement is detected at much lower amplitudes, while for intermediate values, lateral particle displacement is observed. rnIn order to validate the QCM results and study the particle effects on the surface, atomic force microscopy, AFM, is additionally utilized, to image surfaces and measure surface forces. By studying the surface of the polymer film after excitation and particle removal, AFM imaging helped in detecting three different meniscus types for the contact area: the “full contact”, the “asymmetrical” and a third one including a “homocentric smaller meniscus”. The different meniscus forms result in varying bond intensity between particles and polymer film, which could explain the deviation between number of particles per surface area measured by imaging and the values provided by the QCM - frequency shift analysis. The asymmetric and the homocentric contact types are suggested to be responsible for the positive frequency shifts observed for all three measured overtones, i.e. for the weak-coupling regime, while the “full contact” type resulted in a negative frequency shift, by effectively contributing to the mass increase of the quartz..rnThe interplay between inertia and contact forces for the particle-surface system leads to strong- or weak-coupling, with the particle affecting in three mentioned ways the polymer surface. This is manifested in the frequency shifts of the QCM system harmonics which are used to differentiate between the two interaction types and reflect the overall state of adhesion for particles of different size.rn