Structural properties of a family of hydrogen-bonded co-crystals formed between gemfibrozil and hydroxy derivatives of t-butylamine, determined directly from powder X-ray diffraction data

We report the formation and structural properties of co-crystals containing gemfibrozil and hydroxy derivatives of t-butylamine H2NC(CH3)3-n(CH2OH)n, with n=0, 1, 2 and 3. In each case, a 1:1 co-crystal is formed, with transfer of a proton from the carboxylic acid group of gemfibrozil to the amino group of the t-butylamine derivative. All of the co-crystal materials prepared are polycrystalline powders, and do not contain single crystals of suitable size and/or quality for single crystal X-ray diffraction studies. Structure determination of these materials has been carried out directly from powder X-ray diffraction data, using the direct-space Genetic Algorithm technique for structure solution followed by Rietveld refinement. The structural chemistry of this series of co-crystal materials reveals well-defined structural trends within the first three members of the family (n=0, 1, 2), but significantly contrasting structural properties for the member with n=3. © 2007 Elsevier Inc. All rights reserved.

Analysis of powder caking in multicomponent powders using atomic force microscopy to examine particle properties

Atomic force microscopy has been used to study the surface properties of model spray dried powders. Phase imaging, nanoindentation and force modulation microscopy have differentiated between the different surface material properties of the particles, revealing a regular dispersion of soft, oil rich areas distributed across the particles' surface. Humidity and temperature cycling effects on the caking behavior of the particles have also been investigated, with significant morphology changes and onset of caking found to occur within relatively short periods of time.

Effect of thermal and mechanical processing on tensile properties of powder formed 2124 aluminium and 2124 Al-SiC p metal matrix composite

The aging responses of 2124 Al-SiC p metal matrix composite (MMC) and unreinforced matrix alloy are studied and related to variations in tensile properties. The MMC is aged from Wo starting conditions: (i) stretched and naturally aged and (ii) re-solution treated. Accelerated aging occurs in both MMC conditions compared with unreinforced alloy. Tensile strengths and elastic moduli are improved in the MMC compared with the alloy, but ductility is reduced. Stretched MMC exhibits higher strength but lower ductility and modulus than re-solutioned MMC. The re-solutioned MMC fails by microvoid coalescence in low aging conditions, and by void nucleation and shear in high aging conditions. Failure of the stretched MMC initiates at the surface at specimen shoulders, illustrating the increased notch sensitivity of this condition, and propagates via a zigzag shear fracture mode. Zigzag facet size increases on gross aging. Particle fracture occurs during tensile failure, but also before testing as a result of the manufacturing process. © 1995 The Institute of Materials.

Measuring the flow properties of small powder samples using an avalanche tester

The feasibility of using a small-scale avalanche tester to measure the flow properties of pharmaceutical lactose powders was examined. The modes of behaviour observed in larger systems were displayed and showed a clear distinction between angular, free-flowing particles and more spherical particles of similar flow characteristics. Angular Lactohale LH100 particles showed slumping behaviour at a rotational frequency of 0.33Hz which disappeared at higher frequencies. Spherical lactose powder with a similar flow function to LH100 only showed rolling behaviour under the same conditions, as did more cohesive powders LH200 and LH300. Further investigation of the LH100 data using Fast Fourier analysis showed that the slumping frequency was 1/10th of the rotational frequency.

Health-promoting properties of bioactive peptides derived from milk proteins in infant food : a review

Peer reviewed

The effects of formulation and processing on surface characteristics and functional properties of dairy powders

The objectives of this thesis were to (i) study the effect of increasing protein concentration in milk protein concentrate (MPC) powders on surface composition and sorption properties; (ii) examine the effect of increasing protein content on the rehydration properties of MPC; (iii) study the physicochemical properties of spraydried emulsion-containing powders having different water and oil contents; (iv) analyse the effect of protein type on water sorption and diffusivity properties in a protein/lactose dispersion, and; (v) characterise lactose crystallisation and emulsion stability of model infant formula containing intact or hydrolysed whey proteins. Surface composition of MPC powders (protein contents 35 - 86 g / 100 g) indicated that fat and protein were preferentially located on the surface of powders. Low protein powder (35 g / 100 g) exhibited lactose crystallisation, whereas powders with higher protein contents did not, due to their high protein: lactose ratio. Insolubility was evident in high protein MPCs and was primarily related to insolubility of the casein fraction. High temperature (50 °C) was required for dissolution of high protein MPCs (protein content > 60 g / 100 g). The effect of different oil types and spray-drying outlet temperature on the physicochemical properties of the resultant fat-filled powders was investigated and showed that increasing outlet temperature reduced water content, water activity and tapped bulk density, irrespective of oil type, and increased solvent-extractable free fat for all oil types and onset of glass transition (Tg) and crystallisation (Tcr) temperature. Powder dispersions of protein/lactose (0.21:1), containing either intact or hydrolysed whey protein (12 % degree of hydrolysis; DH), were spray-dried at pilot scale. Moisture sorption analysis at 25 °C showed that dispersions containing intact whey protein exhibited lactose crystallisation at a lower relative humidity (RH). Dispersions containing hydrolysed whey protein had significantly higher (P < 0.05) water diffusivity. Finally, a spray-dried model infant formula was produced containing hydrolysed or intact whey as the protein with sunflower oil as the fat source. Reconstituted, hydrolysed formula had a significantly (P < 0.05) higher fat globule size and lower emulsion stability than intact formula. Lactose crystallisation in powders occurred at higher RH for hydrolysed formula. In conclusion, this research has shown the effect of altering the protein type, protein composition, and oil type on the surface composition and physical properties of different dairy powders, and how these variations greatly affect their rehydration characteristics and storage stability.

Enhancing the total phenolic content and antioxidants of lemon pomace aqueous extracts by applying UV-C irradiation on the dried powder

Several studies have shown that UV-C irradiation promotes the bioactive compounds and antioxidants of fresh fruits and vegetables. The aim of this study was to apply UV irradiation in lemon pomace dried powder for enhancing its phenolic content and antioxidant properties, thus more bioactive compounds should be available for extraction and utilization. Lemon pomace dried powder was placed above the UV lamp and treated with dosages of 4, 19, 80 and 185 kJ m-2, while untreated powder was used as a control. UV-C irradiation significantly affected the total phenolic content, total flavonoid content, proanthocyanidins and antioxidant capacity measured by CUPRAC and FRAP of the lemon pomace dried powder, while it did not affect the vitamin C content. UV-C irradiation of 19 kJ m-2 resulted in 19% higher total phenolic content than the control, while UV-C irradiation of 180 kJ m-2 resulted in 28% higher total flavonoid content than the control. The antioxidant capacity was reduced when UV-C irradiation more than 4 kJ m-2 was applied. The results of this study indicate that UV-C treatment has the potential to increase the extraction of bioactive compounds of lemon dried pomace at relatively high dosages.

Foeniculum vulgare Mill. as a natural ingredient to improve cottage cheese antioxidant properties

Food industry is focused on the development of novel functional foods containing health promoting natural ingredients. Natural antioxidants present important health benefits like the prevention of several diseases related to oxidative stress [1,2]. Foeniculum vulgare Mill. (fennel) is a source of those compounds with proved antioxidant potential [3]. Herein, after evaluation of 2,2-diphenyl-1-picrylhydrazyl (DPPH) scavenging activity and reducing power of fennel (provided by Américo Duarte Paixão Lda.) decoction, we propose its incorporation into cottage cheese (produced by Queijos Casa Matias Lda.). Three groups of cottage cheese samples were prepared: control; samples with fennel decoction (incorporated at EC25 value=0.35 mg/mL, previously determined by DPPH assay); and samples with fennel powder (incorporated at 1.75 mg/mL, considering the decoction yield=20%). The samples were submitted to an evaluation of DPPH scavenging activity and reducing power immediately after the incorporations, and after 7 and 14 days of storage, at 4 ºC. The incorporation of fennel improved the antioxidant activity of cottage cheese. Samples incorporated with plant powder revealed higher antioxidant properties than samples incorporated with decoction, either in 0 or 7 days of storage. After 14 days, cottage cheese incorporated with fennel decoction gave the highest DPPH scavenging activity (46.72±0.09 mg/mL). A decrease in the antioxidant potential of the cottage cheese with fennel was observed along the shelf life. Nevertheless, it is important to highlight that the samples still display antioxidant properties. Studies regarding the effects of the incorporation of these natural ingredients on nutritional and chemical composition of cottage cheese are in course

Maltodextrin-incorporated-vacuum-dried honey powder: processing and stability

Honey is rich in sugar content and dominated by fructose and glucose that make honey prone to crystallize during storage. Due to honey composition, the anhydrous glass transition temperature of honey is very low that makes honey difficult to dry alone and drying aid or filler is needed to dry honey. Maltodextrin is a common drying aid material used in drying of sugar-rich food. The present study aims to study the processing of honey powder by vacuum drying method and the impact of drying process and formulation on the stability of honey powder. To achieve the objectives, the series of experiments were done: investigating of maltodextrin DE 10 properties, studying the effect of drying temperature, total solid concentration, DE value, maltodextrin concentration and anti-caking agent on honey powder processing and stability. Maltodextrin provide stable glass compared to lower molecular weight sugars. Dynamic Dew Point Isotherm (DDI) data could be used to determine amorphous content of a system. The area under the first derivative curve from DDI curve is equal to the amount of water needed by amorphous material to crystallize. The drying temperature affected the amorphous content of vacuum-dried honey powder. The higher temperature seemed to result in honey powder with more amorphous component. The ratio of maltodextrin affected more significantly the stability of honey powder compared to the treatments of total solids concentration, DE value and drying temperature. The critical water activity of honey powder was lower than water activity of the equilibrium water content corresponding to BET monolayer water content. Addition of anti-caking agent increased stability and flow-ability of honey powder. Addition of Calcium stearate could inhibit collapse of the honey powder during storage.

Land use change from rainforests to oil palm plantations and food gardens in Papua New Guinea: Effects on soil properties and S fractions

Changes in soil sulfur (S) fractions were assessed in oil palm and food garden land use systems developed on forest vegetation in humid tropical areas of Popondetta in northern Province. The study tested a hypothesis that S in food gardens are limiting nutrient factor and are significantly lower than in plantations and forests. Subsistence food gardens are under long-term slash and burn practice of cropping and such practice is expected to accelerate loss of biomass S from the ecosystem. From each land use, surface soil (0–15 cm) samples were characterised and further pseudocomplete fractionated for S. Conversion of forest to oil palm production decreased (p<0.001) soil pH and electrical conductivity values. The reserve S fraction in soil increased significantly (p<0.05) due to oil palm production ( 28 %) and food gardening activity (∼ 54 %). However, plant available SO42--S was below 15 mg kg^(−1) in the food garden soils and foliar samples of sweet potato crop indicating deficiency of plant available S. Soil organic carbon content (OC) was positively and significantly correlated to total S content (r=0.533; p<0.001) among the land use systems. Thus, crop management practices that affect OC status of the soils would potentially affect the S availability in soils. The possible changes in the chemical nature of mineralisable organic S compounds leading to enhanced mineralisation and leaching losses could be the reasons for the deficiency of S in the food garden soils. The results of this study conclude that long-term subsistence food gardening activity enriched top soils with reserve S or total S content at the expense of soluble S fraction. The subsistence cropping practices such as biomass burning in food gardens and reduced fallow periods are apparently threatening food security of oil palm households. Improved soil OC management strategies such as avoiding burning of fallow vegetation, improved fallows, mulching with fallow biomass, use of manures and S containing fertilisers must be promoted to sustain food security in smallholder oil palm system.

Emerging plant-based proteins: comparison from extraction to functional properties and food application

The increasing demand for alternatives to meat food products, which is linked to ethical and environmental reasons, highlights the necessity of using different protein sources. Plant proteins provide a valid option, thanks to the relative low costs, high availability and wide supply sources. The current process used to produce plant concentrates and isolates is the alkaline extraction followed by isoelectric precipitation. However, despite the high purity of the proteins, it presents some drawbacks. Innovative protein extraction processes are emerging, with the aim of reducing the environmental impact and the costs, as well as improving the functional properties. In this study, the traditional wet protein extraction and another simplified wet process were used to obtain protein-rich extracts out of different plants. The sources considered in the project were de-oiled sunflower and canola, chickpea, lentils, and the camelina meal, an emerging oleaginous seed interesting for its high content of omega 3. The extracts obtained from the two processes were then analysed for their capacities to hold water and fat, to form gel and a stable foam. Results highlighted strong differences concerning the protein content, yield and functionalities. The extracts obtained with the alkaline process confirmed the literature data about the four plant sources (sunflower, canola, chickpea and lentils) and allow to obtain a camelina concentrate with a protein content of 63 % and a protein recovery of 41 %. The second easiest process was not effective to obtain a protein enrichment in oleaginous sources, whereas an enrichment of 10 and 15 % was obtained in chickpea and lentils, respectively. The functional properties were also completely different: the easiest process produced protein ingredients completely water-soluble at pH 7, with a discrete foaming capacity compared to the extracts obtained with alkaline process. These characteristics could make these extracts suitable for the plant milk-analogue products.

Optimization of an innovative T6 heat treatment for the AlSi10Mg alloy processed by Laser-based Powder Bed Fusion: effect on microstructure, mechanical properties, and tribological behavior

Laser-based Powder Bed Fusion (L-PBF) technology is one of the most commonly used metal Additive Manufacturing (AM) techniques to produce highly customized and value-added parts. The AlSi10Mg alloy has received more attention in the L-PBF process due to its good printability, high strength/weight ratio, corrosion resistance, and relatively low cost. However, a deep understanding of the effect of heat treatments on this alloy's metastable microstructure is still required for developing tailored heat treatments for the L-PBF AlSi10Mg alloy to overcome the limits of the as-built condition. Several authors have already investigated the effects of conventional heat treatment on the microstructure and mechanical behavior of the L-PBF AlSi10Mg alloy but often overlooked the peculiarities of the starting supersatured and ultrafine microstructure induced by rapid solidification. For this reason, the effects of innovative T6 heat treatment (T6R) on the microstructure and mechanical behavior of the L-PBF AlSi10Mg alloy were assessed. The short solution soaking time (10 min) and the relatively low temperature (510 °C) reduced the typical porosity growth at high temperatures and led to a homogeneous distribution of fine globular Si particles in the Al matrix. In addition, it increased the amount of Mg and Si in the solid solution available for precipitation hardening during the aging step. The mechanical (at room temperature and 200 °C) and tribological properties of the T6R alloy were evaluated and compared with other solutions, especially with an optimized direct-aged alloy (T5 alloy). Results showed that the innovative T6R alloy exhibits the best mechanical trade-off between strength and ductility, the highest fatigue strength among the analyzed conditions, and interesting tribological behavior. Furthermore, the high-temperature mechanical performances of the heat-treated L-PBF AlSi10Mg alloy make it suitable for structural components operating in mild service conditions at 200 °C.

High-strength steels manufactured via Laser Powder Bed Fusion: effect of post-process heat treatments and surface finishing on microstructure and mechanical properties

Laser Powder Bed Fusion (LPBF) permits the manufacturing of parts with optimized geometry, enabling lightweight design of mechanical components in aerospace and automotive and the production of tools with conformal cooling channels. In order to produce parts with high strength-to-weight ratio, high-strength steels are required. To date, the most diffused high-strength steels for LPBF are hot-work tool steels, maraging and precipitation-hardening stainless steels, featuring different composition, feasibility and properties. Moreover, LPBF parts usually require a proper heat treatment and surface finishing, to develop the desired properties and reduce the high roughness resulting from LPBF. The present PhD thesis investigates the effect of different heat treatments and surface finishing on the microstructure and mechanical properties of a hot-work tool steel and a precipitation-hardening stainless steel manufactured via LPBF. The bibliographic section focuses on the main aspects of LPBF, hot-work tool steels and precipitation-hardening stainless steels. The experimental section is divided in two parts. Part A addresses the effect of different heat treatments and surface finishing on the microstructure, hardness, tensile and fatigue behaviour of a LPBF manufactured hot-work tool steel, to evaluate its feasibility for automotive and racing components. Results indicated the possibility to achieve high hardness and strength, comparable to the conventionally produced steel, but a great sensitivity of fatigue strength on defects and surface roughness resulting from LPBF. Part B investigates the effect of different heat treatments on the microstructure, hardness, tensile and notch-impact behaviour of a LPBF produced precipitation-hardening stainless steel, to assess its feasibility for tooling applications. Results indicated the possibility to achieve high hardness and strength also through a simple Direct Aging, enabling heat treatment simplification by exploiting the microstructural features resulting from LPBF.

Effect Of Spray Drying On The Sensory And Physical Properties Of Hydrolysed Casein Using Gum Arabic As The Carrier.

This study was aimed at spray drying hydrolysed casein using gum Arabic as the carrier agent, in order to decrease the bitter taste. Three formulations with differing proportions of hydrolysed casein: gum Arabic (10:90, 20:80 and 30:70) were prepared and characterized. They were evaluated for their moisture content, water activity, hygroscopicity, dispersibility in water and in oil, particle size and distribution, particle morphology, thermal behaviour (DSC) and bitter taste by a trained sensory panel using a paired-comparison test (free samples vs. spray dried samples). The proportion of hydrolysed casein did not affect the morphology of the microspheres. The spray drying process increased product stability and modified the dissolution time, but had no effect on the ability of the material to dissolve in either water or oil. The sensory tests showed that the spray drying process using gum Arabic as the carrier was efficient in attenuating or masking the bitter taste of the hydrolysed casein.