Dehydration of CO2-α-cyclodextrin complex powder by desiccant adsorption method and its release properties.

Stability and release properties of CO2-α-cyclodextrin complex powder prepared by solid encapsulation (water activity, aw ≈ 0.95) followed by moisture removal using silica gel and CaCl2 desiccants during post-dehydration were investigated. The results showed that CaCl2 reduced aw much faster than silica gel did under the same conditions. After approximately 60 h, aw of complex powders reduced using silica gel was almost constant at 0.247 (±0.012), while those treated with CaCl2, aw was 0.225 (±0.005) and had not yet reached their lowest value. Moisture adsorption by silica gel and CaCl2 also led to a decrease in the CO2 concentration of complex powder (higher decrease for silica gel adsorption) without affecting the structure and morphology of complex powder. The CO2 release properties of CaCl2-aw-reduced complex powder at different relative humidities (32.73, 52.86, 75.32 and 97.30% RH), liquid environments (water and oil) and packaging methods (normal and vacuum) were also studied.

Preparation of Ibuprofen Microparticles by Antisolvent Precipitation Crystallization Technique: Characterization, Formulation, and In Vitro Performance.

This study demonstrates the preparation and characterization of ibuprofen (IBP) microparticles with some excipients by a controlled crystallization technique with improved dissolution performance. Using the optimum concentrations pluronic F127, hydroxypropyl methyl cellulose, D-mannitol, and l-leucine in aqueous ethanol, the IBP microparticles were prepared. The dissolution tests were performed in phosphate buffer saline using a United States Pharmacopoeia dissolution tester at 37°C. The Raman spectroscopy was used to investigate the interactions and distribution of the IBP with the additives in the microcrystals. The prepared IBP microparticles showed higher dissolution compared to that of the smaller sized original IBP particles. The Raman data revealed that the excipients with a large number of hydroxyl groups distributed around the IBP particle in the crystal enhanced the dissolution of the drug by increasing the drug-solvent interaction presumably through hydrogen bonding. The Raman mapping technique gave an insight into the enhanced dissolution behavior of the prepared IBP microparticles, and such information will be useful for developing pharmaceutical formulations of hydrophobic drugs. The controlled crystallization was a useful technique to prepare complex crystals of IBP microparticles along with other additives to achieve the enhanced dissolution profile.

Encapsulation of CO2 into amorphous alpha-cyclodextrin powder at different moisture contents - Part 1: Encapsulation capacity and stability of inclusion complexes.

This study investigated the effects of water-induced crystallization of amorphous alpha-cyclodextrin (α-CD) powder on CO2 encapsulation at 0.4-1.6 MPa pressure for 1-72 h through the addition of water (to reach to 13, 15 and 17% wet basis, w.b.) into amorphous α-CD powder prior to the encapsulation. The results showed that the α-CD encapsulation capacity was over 1 mol CO2/mol α-CD after pressurizing for longer than 48 h. The encapsulated CO2 concentration by the addition of water was considerably higher (p<0.05) than that of amorphous α-CD powder (5.51% MC, w.b.) without an addition of water and that of crystalline α-CD powders under the same MC and encapsulation conditions. A comparison of CO2 release properties (75% relative humidity, 25 °C) from complexed powders prepared from amorphous and crystalline α-CD powders under the same conditions is also presented.

Encapsulation of CO2 into amorphous alpha-cyclodextrin powder at different moisture contents - Part 2: Characterization of complexed powders and determination of crystalline structure.

This study aims to characterize CO2-α-cyclodextrin (α-CD) inclusion complexes produced from amorphous α-CD powder at moisture contents (MC) close to or higher than the critical level of crystallization (e.g. 13, 15 and 17% MC on wet basis, w.b.) at 0.4 and 1.6MPa pressure for 72h. The results of (13)C NMR, SEM, DSC and X-ray analyses showed that these MC levels were high enough to induce crystallization of CO2-α-CD complexed powders during encapsulation, by which amount of CO2 encapsulated by amorphous α-CD powder was significantly increased. The formation of inclusion complexes were well confirmed by results of FTIR and (13)C NMR analyses through an appearance of a peak associated with CO2 on the FTIR (2334cm(-1)) and NMR (125.3ppm) spectra. Determination of crystal packing patterns of CO2-α-CD complexed powders showed that during crystallization, α-CD molecules were arranged in cage-type structure in which CO2 molecules were entrapped in isolated cavities.

A quantitative review of the transition salt concentration for inhibiting bubble coalescence.

Some salts have been proven to inhibit bubble coalescence above a certain concentration called the transition concentration. The transition concentration of salts has been investigated and determined by using different techniques. Different mechanisms have also been proposed to explain the stabilizing effect of salts on bubble coalescence. However, as yet there is no consensus on a mechanism which can explain the stabilizing effect of all inhibiting salts. This paper critically reviews the experimental techniques and mechanisms for the coalescence of bubbles in saline solutions. The transition concentrations of NaCl, as the most popularly used salt, determined by using different techniques such as bubble swarm, bubble pairs, and thin liquid film micro-interferometry were analyzed and compared. For a consistent comparison, the concept of TC95 was defined as a salt concentration at which the "percentage coalescence" of bubbles reduces by 95% relative to the highest (100% in pure water) and lowest (in high-salt concentration) levels. The results show a linear relationship between the TC95 of NaCl and the reciprocal of the square root of the bubble radius. This relationship holds despite different experimental techniques, salt purities and bubble approach speeds, and highlights the importance of the bubble size in bubble coalescence. The available theoretical models for inhibiting effect of salts have also been reviewed. The failure of these models in predicting the salt transition concentration commands further theoretical development for a better understanding of bubble coalescence in salt solutions.

Encapsulation of CO2 into amorphous and crystalline α-cyclodextrin powders and the characterization of the complexes formed.

Carbon dioxide complexation was undertaken into solid matrices of amorphous and crystalline α-cyclodextrin (α-CD) powders, under various pressures (0.4-1.6 MPa) and time periods (4-96 h). The results show that the encapsulation capacity of crystalline α-CD was significantly lower than that of amorphous α-CD at low pressure and short time (0.4-0.8 MPa and 4-24 h), but was markedly enhanced with an increase of pressure and prolongation of encapsulation time. For each pressure level tested, the time required to reach a near equilibrium encapsulation capacity of the crystalline powder was around 48 h, which was much longer than that of the amorphous one, which only required about 8h. The inclusion complex formation of both types of α-CD powders was confirmed by the appearance of a CO2 peak on the FTIR and NMR spectra. Moreover, inclusion complexes were also characterized by DSC, TGA, SEM and X-ray analyses.

Mass transfer correlations for rotating drum bioreactors.

Evaporative cooling is extremely important for large-scale operation of rotating drum bioreactors (RDBs). Outlet water vapour concentrations were measured for a RDB containing wet wheat bran with the aim of determining the mass transfer coefficient for evaporation from the bran bed to the headspace. Mass transfer was expressed as the mass transfer coefficient times the area for transfer per unit volume of void space in the drum. Values of ka' were determined under combinations of aeration superficial velocities ranging from 0.006 to 0.017 ms(-1) and rotation rates ranging from 0 to 9 rpm. Mass transfer coefficients were evaluated using a variety of residence time distributions (RTDs) for flow in the gas phase including plug flow and well-mixed and a Central Jet RTD based on RTD studies. If plug flow is assumed, the degree of holdup at low effective Peclet (Pe(eff)) numbers gives an apparent under-estimate of ka' compared with empirical correlations. Values of ka' calculated using the Central Jet RTD agree well with values of ka' from literature correlations. There was a linear relationship between ka' and effective Peclet number: ka' = 2.32 x 10(-3)Pe(eff).

Drop penetration into porous powder beds.

The kinetics of drop penetration were studied by filming single drops of several different fluids (water, PEG200, PEG600, and HPC solutions) as they penetrated into loosely packed beds of glass ballotini, lactose, zinc oxide, and titanium dioxide powders. Measured times ranged from 0.45 to 126 s and depended on the powder particle size, viscosity, surface tensions, and contact angle. The experimental drop penetration times were compared to existing theoretical predictions by M. Denesuk et al. (J. Colloid Interface Sci.158, 114, 1993) and S. Middleman ("Modeling Axisymmetric Flows: Dynamics of Films, Jets, and Drops," Academic Press, San Diego, 1995) but did not agree. Loosely packed powder beds tend to have a heterogeneous bed structure containing large macrovoids which do not participate in liquid flow but are included implicitly in the existing approach to estimating powder pore size. A new two-phase model was proposed where the total volume of the macrovoids was assumed to be the difference between the bed porosity and the tap porosity. A new parameter, the effective porosity epsilon(eff), was defined as the tap porosity multiplied by the fraction of pores that terminate at a macrovoid and are effectively blocked pores. The improved drop penetration model was much more successful at estimating the drop penetration time on all powders and the predicted times were generally within an order of magnitude of the experimental results.

Chaotic advection in a 2-D mixed convection flow.

Two-dimensional numerical simulations of particle advection in a channel flow with spatially periodic heating have been carried out. The velocity field is found to be periodic above a critical Rayleigh number of around 18 000 and a Reynolds number of 10. Particle motion becomes chaotic in the lower half plane almost immediately after this critical value is surpassed, as characterized by the power spectral density and Poincare section of the flow. As the Rayleigh number is increased further, particle motion in the entire domain becomes chaotic. (c) 1995 American Institute of Physics.

Use of confocal scanning laser microscopy to measure the concentrations of aerial and penetrative hyphae during growth of Rhizopus oligosporus on a solid surface.

In order to develop a method for use in investigations of spatial biomass distribution in solid-state fermentation systems, confocal scanning laser microscopy was used to determine the concentrations of aerial and penetrative biomass against height and depth above and below the substrate surface, during growth of Rhizopus oligosporus on potato dextrose agar. Penetrative hyphae had penetrated to a depth of 0.445 cm by 64 h and showed rhizoid morphology, in which the maximum biomass concentration, of 4.45 mg dry wt cm(-3), occurred at a depth of 0.075 cm. For aerial biomass the maximum density of 39.54 mg dry wt (-3) occurred at the substrate surface. For both aerial and penetrative biomass, there were two distinct regions in which the biomass concentration decayed exponentially with distance from the surface. For aerial biomass, the first exponential decay region was up to 0.1 cm height. The second region above the height of 0.1 cm corresponded to that in which sporangiophores dominated. This work lays the foundation for deeper studies into what controls the growth of fungal hyphae above and below the surfaces of solid substrates.

Use of confocal microscopy to follow the development of penetrative hyphae during growth of Rhizopus oligosporus in an artificial solid-state fermentation system.

Two methods were compared for determining the concentration of penetrative biomass during growth of Rhizopus oligosporus on an artificial solid substrate consisting of an inert gel and starch as the sole source of carbon and energy. The first method was based on the use of a hand microtome to make sections of approximately 0.2- to 0.4-mm thickness parallel to the substrate surface and the determination of the glucosamine content in each slice. Use of glucosamine measurements to estimate biomass concentrations was shown to be problematic due to the large variations in glucosamine content with mycelial age. The second method was a novel method based on the use of confocal scanning laser microscopy to estimate the fractional volume occupied by the biomass. Although it is not simple to translate fractional volumes into dry weights of hyphae due to the lack of experimentally determined conversion factors, measurement of the fractional volumes in themselves is useful for characterizing fungal penetration into the substrate. Growth of penetrative biomass in the artificial model substrate showed two forms of growth with an indistinct mass in the region close to the substrate surface and a few hyphae penetrating perpendicularly to the surface in regions further away from the substrate surface. The biomass profiles against depth obtained from the confocal microscopy showed two linear regions on log-linear plots, which are possibly related to different oxygen availability at different depths within the substrate. Confocal microscopy has the potential to be a powerful tool in the investigation of fungal growth mechanisms in solid-state fermentation.