Plasmon dispersion in a multilayer solid torus in terms of three-term vector recurrence relations and matrix continued fractions

DOE PAGES

Garapati, K. V.; Bagherian, M.; Passian, A.; ...

2018-01-03

Toroidal confinement, which has played a crucial role in magnetized plasmas and Tokamak physics, is emerging as an effective means to obtain useful electronic and optical response in solids. In particular, excitation of surface plasmons in metal nanorings by photons or electrons finds important applications due to the engendered field distribution and electromagnetic energy confinement. However, in contrast to the case of a plasma, often the solid nanorings are multilayered and/or embedded in a medium. The non-simply connected geometry of the torus results in surface modes that are not linearly independent. A three-term difference equation was recently shown to arisemore » when seeking the nonretarded plasmon dispersion relations for a stratified solid torus (Garapati et al 2017 Phys. Rev. B 95 165422). The reported generalized plasmon dispersion relations are here investigated in terms of the involved matrix continued fractions and their convergence properties including the determinant forms of the dispersion relations obtained for computing the plasmon eigenmodes. We also present the intricacies of the derivation and properties of the Green's function employed to solve the three term amplitude equation that determines the response of the toroidal structure to arbitrary external excitations.« less

Plasmon dispersion in a multilayer solid torus in terms of three-term vector recurrence relations and matrix continued fractions

DOE Office of Scientific and Technical Information (OSTI.GOV)

Garapati, K. V.; Bagherian, M.; Passian, A.

Toroidal confinement, which has played a crucial role in magnetized plasmas and Tokamak physics, is emerging as an effective means to obtain useful electronic and optical response in solids. In particular, excitation of surface plasmons in metal nanorings by photons or electrons finds important applications due to the engendered field distribution and electromagnetic energy confinement. However, in contrast to the case of a plasma, often the solid nanorings are multilayered and/or embedded in a medium. The non-simply connected geometry of the torus results in surface modes that are not linearly independent. A three-term difference equation was recently shown to arisemore » when seeking the nonretarded plasmon dispersion relations for a stratified solid torus (Garapati et al 2017 Phys. Rev. B 95 165422). The reported generalized plasmon dispersion relations are here investigated in terms of the involved matrix continued fractions and their convergence properties including the determinant forms of the dispersion relations obtained for computing the plasmon eigenmodes. We also present the intricacies of the derivation and properties of the Green's function employed to solve the three term amplitude equation that determines the response of the toroidal structure to arbitrary external excitations.« less

Enhanced solubility of piperine using hydrophilic carrier-based potent solid dispersion systems.

PubMed

Thenmozhi, Kathavarayan; Yoo, Young Je

2017-09-01

Piperine alkaloid, an important constituent of black pepper, exhibits numerous therapeutic properties, whereas its usage as a drug is limited due to its poor solubility in aqueous medium, which leads to poor bioavailability. Herein, a new method has been developed to improve the solubility of this drug based on the development of solid dispersions with improved dissolution rate using hydrophilic carriers such as sorbitol (Sor), polyethylene glycol (PEG) and polyvinyl pyrrolidone K30 (PVP) by solvent method. Physical mixtures of piperine and carriers were also prepared for comparison. The physicochemical properties of the prepared solid dispersions were examined using SEM, TEM, DSC, XRD and FT-IR. In vitro dissolution profile of the solid dispersions was recorded and compared with that of the pure piperine and physical mixtures. The effect of these carriers on the aqueous solubility of piperine has been investigated. The solid dispersions of piperine with Sor, PEG and PVP exhibited superior performance for the dissolution of piperine with a drug release of 70%, 76% and 89%, respectively after 2 h compared to physical mixtures and pure piperine, which could be due to its transformation from crystalline to amorphous form as well as the attachment of hydrophilic carriers to the surface of poorly water-soluble piperine. Results suggest that the piperine solid dispersions prepared with improved in vitro release exhibit potential advantage in delivering poorly water-soluble piperine as an oral supplement.

Comparison of a solid SMEDDS and solid dispersion for enhanced stability and bioavailability of clopidogrel napadisilate.

PubMed

Kim, Dong Wuk; Kwon, Min Seok; Yousaf, Abid Mehmood; Balakrishnan, Prabagar; Park, Jong Hyuck; Kim, Dong Shik; Lee, Beom-Jin; Park, Young Joon; Yong, Chul Soon; Kim, Jong Oh; Choi, Han-Gon

2014-12-19

The intention of this study was to compare the physicochemical properties, stability and bioavailability of a clopidogrel napadisilate (CN)-loaded solid dispersion (SD) and solid self-microemulsifying drug delivery system (solid SMEDDS). SD was prepared by a surface attached method using different ratios of Cremophor RH60 (surfactant) and HPMC (polymer), optimized based on their drug solubility. Liquid SMEDDS was composed of oil (peceol), a surfactant (Cremophor RH60) and a co-surfactant (Transcutol HP). A pseudo-ternary phase diagram was constructed to identify the emulsifying domain, and the optimized liquid SMEDDS was spray dried with an inert solid carrier (silicon dioxide), producing the solid SMEDDS. The physicochemical properties, solubility, dissolution, stability and pharmacokinetics were assessed and compared to clopidogrel napadisilate (CN) and bisulfate (CB) powders. In solid SMEDDS, liquid SMEDDS was absorbed or coated inside the pores of silicon dioxide. In SD, hydrophilic polymer and surfactants were adhered onto drug surface. The drug was in crystalline and molecularly dispersed form in SD and solid SMEDDS, respectively. Solid SMEDDS and SD greatly increased the solubility of CN but gave lower drug solubility compared to CB powder. These preparations significantly improved the dissolution of CN, but the latter more increased than the former. Stability under accelerated condition showed that they were more stable compared to CB powder, and SD was more stable than solid SMEDDS. They significantly increased the oral bioavailability of CN powder. Furthermore, SD showed significantly improved oral bioavailability compared to solid SMEDDS and CB powder. Thus, SD with excellent stability and bioavailability is recommended as an alternative for the clopidogrel-based oral formulation. Copyright © 2014 Elsevier Ltd. All rights reserved.

Colloidal approach to dispersion and enhanced deaggregation of aqueous ferrite suspensions

NASA Astrophysics Data System (ADS)

Mandanas, Michael Patrick M.

The role of solution and surface chemistry on deaggregation of calcined ferrites during attrition (stirred-media) milling of aqueous suspensions were investigated. Suspensions of commercially calcined Fe2O 3 powder (d50 ˜ 5.0 mum) were milled at different solid loadings and suspension pH. The drift of suspension pH, from pH 2.5 to pH 7.0, during solid loading experiments accounted for the observed reagglomeration with milling time. The observed deaggregation rates during pH stat milling, in the acidic region, can be related to (i) elevated solubility and (ii) enhanced dispersion via surface charge. Proton adsorption density during pH stat milling at different pH values is also comparable to existing potentiometric titration plots and can be related to deaggregation rates. A passivation-dispersion approach for dispersing manganese zinc ferrite (MnxZn(1 - x)Fe2O4) powder is presented. Addition of oxalic acid can help control dissolution reactions from particle surfaces and is subsequently dispersed with polyethyleneimine (PEI). Fully dissociated oxalic acid (pK1 = 1.2, pK2 = 4.3) solutions reacted with MnxZn(1 - x)Fe 2O4 leads to the formation of a uniform negative charge on the particle surface, resulting from the sparingly soluble salt formed on the surface. The resulting rheological data for passivation/dispersion of relatively high solid MnxZn(1 - x)Fe2O 4 suspensions (˜80 w/o, (˜40 v/o)) demonstrate improved colloid stability with improved rheological properties. Using the passivation dispersion scheme developed, deaggregation of commercially calcined MnxZn(1 - x)Fe2O4 powders during attrition milling was investigated. Reagglomeration is apparent when using a typical treatment, 2 w/w of a sulfonated based naphthalene condensate, during deaggregation of the calcined MnxZn(1 - x)Fe 2O4. However, is not observed for select oxalate/PEI treatments. The determined ideal treatment is 2 w/w oxalate and 3 w/w PEI based on the particle size and rheological characteristics of the suspensions during milling. (Abstract shortened by UMI.)

Dielectric dispersion of porous media as a fractal phenomenon

NASA Astrophysics Data System (ADS)

Thevanayagam, S.

1997-09-01

It is postulated that porous media is made up of fractal solid skeleton structure and fractal pore surface. The model thus developed satisfies measured anomalous dielectric behavior of three distinctly different porous media: kaolin, montmorillonite, and shaly sand rock. It is shown that the underlying mechanism behind dielectric dispersion in the kHz range to high MHz range is indeed Maxwell-Wagner mechanism but modified to take into account the multiphase nature of the porous media as opposed to the traditional two-phase Maxwell-Wagner charge accumulation effect. The conductivity of the surface water associated with the solid surface and charge accumulation across the surface irregularities, asperity, and bridging between particles at the micro-scale-level pores are shown to contribute to this modified Maxwell-Wagner mechanism. The latter is dominant at low frequencies. The surface water thickness is calculated to be about 2-6 nm for a variety of porous media.

Active motility in bimodular bacterial aggregates

NASA Astrophysics Data System (ADS)

Zeng, Yu; Liu, Bin

2017-11-01

Dispersal capability is essential for microorganisms to achieve long-distance translocation, thus crucial for their abundance in various environments. In general, active dispersals are attributed to the movements of self-powered planktonic cells, while sessile cells that live a colonial life often disperse passively through flow entrainments. Here, we report another means of active dispersal employed by aggregates of sessile cells. The spherical rosette colonies of the bacterium Caulobacter crescentus are aggregates of sessile stalked cells, of which a small proportion undergo cell division, grow active flagella and effect whole-rosette motility. We show that these rosettes actively disperse both in bulk water and near the solid-liquid interface. In particular, the proximity of a self-powered rosette to the solid surface promotes a rolling movement, leading to its persistent transportation along the solid boundary. The active dispersal of these rosettes demonstrated a novel mode of colonial transportation that is based on the division of labor between sessile and motile cells. The authors thank the support of National Science Foundation CREST: Center for Cellular and Biomolecular Machines at UC Merced (NSF-HRD-1547848).

Waveguiding by a locally resonant metasurface

NASA Astrophysics Data System (ADS)

Maznev, A. A.; Gusev, V. E.

2015-09-01

Dispersion relations for acoustic and electromagnetic waves guided by resonant inclusions located at the surface of an elastic solid or an interface between two media are analyzed theoretically within the effective medium approximation. Oscillators on the surface of an elastic half-space are shown to give rise to a Love-type surface acoustic wave only existing below the oscillator frequency. A simple dispersion relation governing this system is shown to also hold for electromagnetic waves guided by Lorentz oscillators at an interface between two media with equal dielectric constants. Different kinds of behavior of the dispersion of the resonantly guided mode are identified, depending on whether the bulk wave in the absence of oscillators can propagate along the surface or interface.

Dispersion of acoustic surface waves by velocity gradients

NASA Astrophysics Data System (ADS)

Kwon, S. D.; Kim, H. C.

1987-10-01

The perturbation theory of Auld [Acoustic Fields and Waves in Solids (Wiley, New York, 1973), Vol. II, p. 294], which describes the effect of a subsurface gradient on the velocity dispersion of surface waves, has been modified to a simpler form by an approximation using a newly defined velocity gradient for the case of isotropic materials. The modified theory is applied to nitrogen implantation in AISI 4140 steel with a velocity gradient of Gaussian profile, and compared with dispersion data obtained by the ultrasonic right-angle technique in the frequency range from 2.4 to 14.8 MHz. The good agreement between experiments and our theory suggests that the compound layer in the subsurface region plays a dominant role in causing the dispersion of acoustic surface waves.

Formulation and process design for a solid dosage form containing a spray-dried amorphous dispersion of ibipinabant.

PubMed

Leane, Michael M; Sinclair, Wayne; Qian, Feng; Haddadin, Raja; Brown, Alan; Tobyn, Mike; Dennis, Andrew B

2013-01-01

Amorphous forms of poorly soluble drugs are more frequently being incorporated into solid dispersions for administration and extensive research has led to a reasonable understanding of how these dispersions, although still kinetically unstable, improve stability relative to the pure amorphous form. There remains however a paucity of literature describing the effects on such solid dispersions of subsequent processing into solid dosage forms such as tablets. This paper addresses this area by looking at the effects of the addition of common excipients and different manufacturing routes on the stability of a spray-dried dispersion (SDD) of the cannabinoid CB-1 antagonist, ibipinabant. A marked difference in physical stability of tablets was seen with the different fillers with microcrystalline cellulose (MCC) giving the best stability profile. It was found that minimising the number of compression steps led to improved formulation stability with a direct compression process giving the best results. Increased levels of crystallinity were seen in coated tablets most likely due to the exposure of the amorphous matrix to moisture and heat during the coating process. DSIMS analysis of the SDD particles indicated increased levels of polymer on the surface.

Hypercrosslinked particles for the extraction of sweeteners using dispersive solid-phase extraction from environmental samples.

PubMed

Lakade, Sameer S; Zhou, Qing; Li, Aimin; Borrull, Francesc; Fontanals, Núria; Marcé, Rosa M

2018-04-01

This work presents a new extraction material, namely, Q-100, based on hypercrosslinked magnetic particles, which was tested in dispersive solid-phase extraction for a group of sweeteners from environmental samples. The hypercrosslinked Q-100 magnetic particles had the advantage of suitable pore size distribution and high surface area, and showed good retention behavior toward sweeteners. Different dispersive solid-phase extraction parameters such as amount of magnetic particles or extraction time were optimized. Under optimum conditions, Q-100 showed suitable apparent recovery, ranging in the case of river water sample from 21 to 88% for all the sweeteners, except for alitame (12%). The validated method based on dispersive solid-phase extraction using Q-100 followed by liquid chromatography with tandem mass spectrometry provided good linearity and limits of quantification between 0.01 and 0.1 μg/L. The method was applied to analyze samples from river water and effluent wastewater, and four sweeteners (acesulfame, saccharin, cyclamate, and sucralose) were found in both types of sample. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Enhancement of solubility and bioavailability of ambrisentan by solid dispersion using Daucus carota as a drug carrier: formulation, characterization, in vitro, and in vivo study.

PubMed

Deshmane, Subhash; Deshmane, Snehal; Shelke, Santosh; Biyani, Kailash

2018-06-01

Ambrisentan is an US FDA approved drug, it is the second oral endothelin A receptor antagonist known for the treatment of pulmonary arterial hypertension, but its oral administration is limited due to its poor water solubility. Hence, the objective of the investigation was focused on enhancement of solubility and bioavailability of ambrisentan by solid dispersion technique using natural Daucus carota extract as drug carrier. Drug carrier was evaluated for solubility, swelling index, viscosity, angle of repose, hydration capacity, and acute toxicity test (LD 50 ). Ambrisentan was studied for the saturation solubility, phase solubility, and Gibbs free energy change. Compatibility of drug and the natural carrier was confirmed by DSC, FTIR, and XRD. Solid dispersions were evaluated for drug content, solubility, morphology, in vitro, and in vivo study. Screening of the natural carrier showed the desirable properties like water solubility, less swelling index, less viscosity, and acute toxicity study revealed no any clinical symptoms of toxicity. Drug and carrier interaction study confirmed the compatibility to consider its use in the formulation. Formed particles were found to be spherical with smooth surface. In vitro studies revealed higher drug release from the solid dispersion than that of the physical mixture. Bioavailability study confirms the increased absorption and bioavailability by oral administration of solid dispersion. Hence, it can be concluded that the natural Daucus carota extract can be the better alternative source for the preparation of solid dispersion and/or other dosage forms for improving solubility and bioavailability.

Colossal super saturation of oxygen at the iron-aluminum interfaces fabricated using solid state welding

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sridharan, Niyanth; Isheim, D.; Seidman, David N.

Solid state joining is achieved in three steps, (i) interface asperity deformation, (ii) oxide dispersion, followed by (iii) atomic contact and bonding. Atomically clean metallic surfaces without an oxide layer bond spontaneously. Despite its importance the oxide dispersion mechanism is not well studied. In this work the first ever atom probe study of iron-aluminum solid state welds show that the oxygen concentration at the interface is 20 at.%. This is significantly lower than any equilibrium oxide concentration. Here, we therefore propose that the high-strain rate deformation at the interfaces renders the oxide unstable resulting in the observed concentration of oxygen.

Colossal super saturation of oxygen at the iron-aluminum interfaces fabricated using solid state welding

DOE PAGES

Sridharan, Niyanth; Isheim, D.; Seidman, David N.; ...

2016-12-14

Solid state joining is achieved in three steps, (i) interface asperity deformation, (ii) oxide dispersion, followed by (iii) atomic contact and bonding. Atomically clean metallic surfaces without an oxide layer bond spontaneously. Despite its importance the oxide dispersion mechanism is not well studied. In this work the first ever atom probe study of iron-aluminum solid state welds show that the oxygen concentration at the interface is 20 at.%. This is significantly lower than any equilibrium oxide concentration. Here, we therefore propose that the high-strain rate deformation at the interfaces renders the oxide unstable resulting in the observed concentration of oxygen.

All-solid-state flexible supercapacitors based on highly dispersed polypyrrole nanowire and reduced graphene oxide composites.

PubMed

Yu, Chenfei; Ma, Peipei; Zhou, Xi; Wang, Anqi; Qian, Tao; Wu, Shishan; Chen, Qiang

2014-10-22

Highly dispersed polypyrrole nanowires are decorated on reduced graphene oxide sheets using a facile in situ synthesis route. The prepared composites exhibit high dispersibility, large effective surface area, and high electric conductivity. All-solid-state flexible supercapacitors are assembled based on the prepared composites, which show excellent electrochemical performances with a specific capacitance of 434.7 F g(-1) at a current density of 1 A g(-1). The as-fabricated supercapacitor also exhibits excellent cycling stability (88.1% capacitance retention after 5000 cycles) and exceptional mechanical flexibility. In addition, outstanding power and energy densities were obtained, demonstrating the significant potential of prepared material for flexible and portable energy storage devices.

Compact solid source of hydrogen gas

DOEpatents

Kravitz, Stanley H.; Hecht, Andrew M.; Sylwester, Alan P.; Bell, Nelson S.

2004-06-08

A compact solid source of hydrogen gas, where the gas is generated by contacting water with micro-disperse particles of sodium borohydride in the presence of a catalyst, such as cobalt or ruthenium. The micro-disperse particles can have a substantially uniform diameter of 1-10 microns, and preferably about 3-5 microns. Ruthenium or cobalt catalytic nanoparticles can be incorporated in the micro-disperse particles of sodium borohydride, which allows a rapid and complete reaction to occur without the problems associated with caking and scaling of the surface by the reactant product sodium metaborate. A closed loop water management system can be used to recycle wastewater from a PEM fuel cell to supply water for reacting with the micro-disperse particles of sodium borohydride in a compact hydrogen gas generator. Capillary forces can wick water from a water reservoir into a packed bed of micro-disperse fuel particles, eliminating the need for using an active pump.

Electrostatic stabilization of multi-walled carbon nanotubes dispersed in nonaqueous media.

PubMed

Damasceno, João Paulo V; Zarbin, Aldo J G

2018-06-04

Dispersing carbon nanotubes is an easy and low-cost way to manipulate these solids and allows the preparation of more complex materials or devices, so it is fundamental for further uses that these dispersions have controlled properties and high colloidal stability. In this work we report the spontaneous electrical charge build-up in pristine multi-walled carbon nanotubes dispersed in common organic solvents such as chloroform and tetrahydrofuran and the achievement of dispersions stable for long periods without adding passivant agents or functional groups on nanotubes surface. Results from electrokinetics, homo- and heterocoagulation provided macroscopic evidences that carbon nanotubes acquire electric charges after dispersion in some organic liquids and we confirmed this process by measuring in situ Raman spectra of the nanotubes dispersions with higher surface electric potentials. We also show that the signal of electric potential of the dispersions can be predicted by the acid-base behaviour of the dispersing medium, corroborating previously reports for other dispersions of carbon nanomaterials. Copyright © 2018 Elsevier Inc. All rights reserved.

Improving Powder Tableting Performance through Materials Engineering

NASA Astrophysics Data System (ADS)

Osei-Yeboah, Frederick

Adequate mechanical strength is a critical requirement to the successful development of a tablet product. Before tablet compression, powders are often engineered by various processes including wet granulation and surface coating, which may improve or adversely affect the powder tableting performance. Such effects, commonly, result from a change in either particle mechanical properties or particulate (size, shape) properties. In this work, tableting performance is interpreted based on the qualitative bonding-area and bonding-strength (BABS) model. The tabletability of the microcrystalline cellulose (MCC) granules deteriorates rapidly with increasing amount of granulating water and eventually leads to over-granulation at high water level. Granule surface smoothing, size enlargement, granule densification and shape rounding are the dominant factors leading to the tabletability reduction of plastic MCC. Incorporation of increasing amounts of brittle excipients, such as lactose or dibasic calcium phosphate reduces the rate of tabletability reduction by promoting more granule fragmentation, introducing more surface area available for bonding. When a sufficient amount of brittle excipients is used, the over-granulation phenomenon can be eliminated. Surface coating of incompressible MCC pellets with highly bonding polymer leads to sufficient surface deformation and adhesion to enable direct compression of the pellets into tablets of adequate mechanical strength. This improvement is enhanced by the presence of moisture, which plasticizes the polymer to allow the development of a larger bonding area between coated pellets. The relationship between mechanical properties and tableting behavior is systematically investigated in polymeric composites using celecoxib-polyvinylpyrrolidone vinyl acetate solid dispersions. Mechanical properties such as indentation hardness of the solid dispersions were measured using nanoindentation. Incorporation of celecoxib up to 60% by weight hardens the polymers, which reduces bonding area but increases bonding strength. On the other hand, moisture softens the solid dispersions and facilitates deformation under pressure to improve tablet mechanical strength. In summary, insights into the deteriorated tabletability of wet granulated powders have been developed and strategies for improving tabletability have been demonstrated. Also, the relationship between particle mechanical properties and tableting performance has been examined using solid dispersions. The BABS model has been further developed to enable its widespread application in interpreting complex tableting behavior.

Contact angle of sessile drops in Lennard-Jones systems.

PubMed

Becker, Stefan; Urbassek, Herbert M; Horsch, Martin; Hasse, Hans

2014-11-18

Molecular dynamics simulations are used for studying the contact angle of nanoscale sessile drops on a planar solid wall in a system interacting via the truncated and shifted Lennard-Jones potential. The entire range between total wetting and dewetting is investigated by varying the solid-fluid dispersive interaction energy. The temperature is varied between the triple point and the critical temperature. A correlation is obtained for the contact angle in dependence of the temperature and the dispersive interaction energy. Size effects are studied by varying the number of fluid particles at otherwise constant conditions, using up to 150,000 particles. For particle numbers below 10,000, a decrease of the contact angle is found. This is attributed to a dependence of the solid-liquid surface tension on the droplet size. A convergence to a constant contact angle is observed for larger system sizes. The influence of the wall model is studied by varying the density of the wall. The effective solid-fluid dispersive interaction energy at a contact angle of θ = 90° is found to be independent of temperature and to decrease linearly with the solid density. A correlation is developed that describes the contact angle as a function of the dispersive interaction, the temperature, and the solid density. The density profile of the sessile drop and the surrounding vapor phase is described by a correlation combining a sigmoidal function and an oscillation term.

Efficient sample preparation method based on solvent-assisted dispersive solid-phase extraction for the trace detection of butachlor in urine and waste water samples.

PubMed

Aladaghlo, Zolfaghar; Fakhari, Alireza; Behbahani, Mohammad

2016-10-01

In this work, an efficient sample preparation method termed solvent-assisted dispersive solid-phase extraction was applied. The used sample preparation method was based on the dispersion of the sorbent (benzophenone) into the aqueous sample to maximize the interaction surface. In this approach, the dispersion of the sorbent at a very low milligram level was achieved by inserting a solution of the sorbent and disperser solvent into the aqueous sample. The cloudy solution created from the dispersion of the sorbent in the bulk aqueous sample. After pre-concentration of the butachlor, the cloudy solution was centrifuged and butachlor in the sediment phase dissolved in ethanol and determined by gas chromatography with flame ionization detection. Under the optimized conditions (solution pH = 7.0, sorbent: benzophenone, 2%, disperser solvent: ethanol, 500 μL, centrifuged at 4000 rpm for 3 min), the method detection limit for butachlor was 2, 3 and 3 μg/L for distilled water, waste water, and urine sample, respectively. Furthermore, the preconcentration factor was 198.8, 175.0, and 174.2 in distilled water, waste water, and urine sample, respectively. Solvent-assisted dispersive solid-phase extraction was successfully used for the trace monitoring of butachlor in urine and waste water samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Vortex-Assisted Dispersive Micro-Solid Phase Extraction Using CTAB-Modified Zeolite NaY Sorbent Coupled with HPLC for the Determination of Carbamate Insecticides.

PubMed

Salisaeng, Pawina; Arnnok, Prapha; Patdhanagul, Nopbhasinthu; Burakham, Rodjana

2016-03-16

A vortex-assisted dispersive micro-solid phase extraction (VA-D-μ-SPE) based on cetyltrimethylammonium bromide (CTAB)-modified zeolite NaY was developed for preconcentration of carbamate pesticides in fruits, vegetables, and natural surface water prior to analysis by high performance liquid chromatography with photodiode array detection. The small amounts of solid sorbent were dispersed in a sample solution, and extraction occurred by adsorption in a short time, which was accelerated by vortex agitation. Finally, the sorbents were filtered from the solution, and the analytes were subsequently desorbed using an appropriate solvent. Parameters affecting the VA-D-μ-SPE performance including sorbent amount, sample volume, desorption solvent ,and vortex time were optimized. Under the optimum condition, linear dynamic ranges were achieved between 0.004-24.000 mg kg(-1) (R(2) > 0.9946). The limits of detection (LODs) ranged from 0.004-4.000 mg kg(-1). The applicability of the developed procedure was successfully evaluated by the determination of the carbamate residues in fruits (dragon fruit, rambutan, and watermelon), vegetables (cabbage, cauliflower, and cucumber), and natural surface water.

Development And Testing Of A New Protocol For Evaluating The Effectiveness Of Oil Spill Surface Washing Agents

EPA Science Inventory

As defined by the National Oil and Hazardous Substances Pollution Contingency Plan (NCP), a surface washing agent (SWA) is a product that removes oil from solid surfaces, such as beaches, rocks, and concrete, through a detergency mechanism and that does not involve dispersing or ...

Formulation and optimization of spray-dried amlodipine solid dispersion for enhanced oral absorption.

PubMed

Jang, Dong-Jin; Sim, Taeyong; Oh, Euichaul

2013-07-01

To enhance the oral absorption of photosensitive amlodipine free base, which exhibits a slow dissolution rate and low permeability characteristics, an amorphous solid dispersion system was formulated and characterized. The solid dispersion was prepared by dispersing the amlodipine free base in excess dextrin (1:10 by weight) using a spray-drying technique in the presence of a minimum amount (0.9% w/w) of SLS as an absorption enhancer. The dextrin-based solid dispersion of amlodipine (Amlo-SD) was evaluated in term of formulation, characterization and in vivo absorption study, as well as the spray-drying process was also optimized. The Amlo-SD particles were spherical with a smooth surface and an average particle size of 12.9 μm. Amlodipine was dispersed in an amorphous state and its content remained uniform in the Amlo-SD. The physicochemical stability of the Amlo-SD was maintained at room temperature for 6 months and the photostability was considerably improved. The dissolution of the Amlo-SD was much faster than that of amlodipine at pH 1.2 and 6.8. Amlo-SD produced significantly higher plasma concentrations of amlodipine in rats than amlodipine alone. Amlo-SD with and without SLS provided 2.8- and 2.0-fold increase in AUC, respectively: the difference seems to be attributed to a permeability enhancement effect by SLS. The Amlo-SD with SLS system is a potential formulation option for amlodipine.

Surface plasmon oscillations in a semi-bounded semiconductor plasma

NASA Astrophysics Data System (ADS)

M, SHAHMANSOURI; A, P. MISRA

2018-02-01

We study the dispersion properties of surface plasmon (SP) oscillations in a semi-bounded semiconductor plasma with the effects of the Coulomb exchange (CE) force associated with the spin polarization of electrons and holes as well as the effects of the Fermi degenerate pressure and the quantum Bohm potential. Starting from a quantum hydrodynamic model coupled to the Poisson equation, we derive the general dispersion relation for surface plasma waves. Previous results in this context are recovered. The dispersion properties of the surface waves are analyzed in some particular cases of interest and the relative influence of the quantum forces on these waves are also studied for a nano-sized GaAs semiconductor plasma. It is found that the CE effects significantly modify the behaviors of the SP waves. The present results are applicable to understand the propagation characteristics of surface waves in solid density plasmas.

A stable solid acid material: Sulfated ZrO2 dispersed on alumina nanotubes

NASA Astrophysics Data System (ADS)

Feng, Yu; Jiaqi, Chen; Xu, Wang; Rui-Feng, Li

2017-02-01

A tubular solid acid catalyst was designed by loading sulfated zirconia into γ-Al2O3 nanotubes using the method of stepwise deposition. The XRD, N2 adsorption-desorption characterization demonstrated that introducing alumina nanotube and SO4 2- anions have played an important role in stabilizing the metastable tetragonal ZrO2 phase, and the sulfated zirconia on the surface of the γ-Al2O3 nanotube has high dispersion and stability. The catalyst reused repeatedly possesses large amounts of acid sites and good acidity, exhibiting high catalytic activity and stability for isopropylbenzene cracking.

Moisture-Induced Amorphous Phase Separation of Amorphous Solid Dispersions: Molecular Mechanism, Microstructure, and Its Impact on Dissolution Performance.

PubMed

Chen, Huijun; Pui, Yipshu; Liu, Chengyu; Chen, Zhen; Su, Ching-Chiang; Hageman, Michael; Hussain, Munir; Haskell, Roy; Stefanski, Kevin; Foster, Kimberly; Gudmundsson, Olafur; Qian, Feng

2018-01-01

Amorphous phase separation (APS) is commonly observed in amorphous solid dispersions (ASD) when exposed to moisture. The objective of this study was to investigate: (1) the phase behavior of amorphous solid dispersions composed of a poorly water-soluble drug with extremely low crystallization propensity, BMS-817399, and PVP, following exposure to different relative humidity (RH), and (2) the impact of phase separation on the intrinsic dissolution rate of amorphous solid dispersion. Drug-polymer interaction was confirmed in ASDs at different drug loading using infrared (IR) spectroscopy and water vapor sorption analysis. It was found that the drug-polymer interaction could persist at low RH (≤75% RH) but was disrupted after exposure to high RH, with the advent of phase separation. Surface morphology and composition of 40/60 ASD at micro-/nano-scale before and after exposure to 95% RH were also compared. It was found that hydrophobic drug enriched on the surface of ASD after APS. However, for the 40/60 ASD system, the intrinsic dissolution rate of amorphous drug was hardly affected by the phase behavior of ASD, which may be partially attributed to the low crystallization tendency of amorphous BMS-817399 and enriched drug amount on the surface of ASD. Intrinsic dissolution rate of PVP decreased resulting from APS, leading to a lower concentration in the dissolution medium, but supersaturation maintenance was not anticipated to be altered after phase separation due to the limited ability of PVP to inhibit drug precipitation and prolong the supersaturation of drug in solution. This study indicated that for compounds with low crystallization propensity and high hydrophobicity, the risk of moisture-induced APS is high but such phase separation may not have profound impact on the drug dissolution performance of ASDs. Therefore, application of ASD technology on slow crystallizers could incur low risks not only in physical stability but also in dissolution performance. Copyright © 2018 American Pharmacists Association®. Published by Elsevier Inc. All rights reserved.

FFT-SOLUTION®

EPA Pesticide Factsheets

Technical product bulletin: this dispersant for oil spill cleanups should be applied as droplets. Manufacturer recommends that spray tips on booms be changed into solid tubing for injection of product 3 to 5 feet below water surface.

The influence of spray-drying parameters on phase behavior, drug distribution, and in vitro release of injectable microspheres for sustained release.

PubMed

Meeus, Joke; Lenaerts, Maité; Scurr, David J; Amssoms, Katie; Davies, Martyn C; Roberts, Clive J; Van Den Mooter, Guy

2015-04-01

For ternary solid dispersions, it is indispensable to characterize their structure, phase behavior, and the spatial distribution of the dispersed drug as this might influence the release profile and/or stability of these formulations. This study shows how formulation (feed concentration) and process (feed rate, inlet air temperature, and atomizing air pressure) parameters can influence the characteristics of ternary spray-dried solid dispersions. The microspheres considered here consist of a poly(lactic-co-glycolic acid) (PLGA) surface layer and an underlying polyvinylpyrrolidone (PVP) phase. A poorly soluble active pharmaceutical ingredient (API) was molecularly dispersed in this matrix. Differences were observed in component miscibility, phase heterogeneity, particle size, morphology, as well as API surface coverage for selected spray-drying parameters. Observed differences are likely because of changes in the droplet generation, evaporation, and thus particle formation processes. However, varying particle characteristics did not influence the drug release of the formulations studied, indicating the robustness of this approach to produce particles of consistent drug release characteristics. This is likely because of the fact that the release is dominated by diffusion from the PVP layer through pores in the PLGA surface layer and that observed differences in the latter have no influence on the release. © 2015 Wiley Periodicals, Inc. and the American Pharmacists Association.

Development and evaluation of gastroretentive raft forming systems incorporating curcumin-Eudragit® EPO solid dispersions for gastric ulcer treatment.

PubMed

Kerdsakundee, Nattha; Mahattanadul, Sirima; Wiwattanapatapee, Ruedeekorn

2015-08-01

Novel raft forming systems incorporating curcumin-Eudragit® EPO solid dispersions were developed to prolong the gastric residence time and provide for a controlled release therapy of curcumin to treat gastric ulcers. The solid dispersions of curcumin with Eudragit® EPO were prepared by the solvent evaporation method at various ratios to improve the solubility and the dissolution of curcumin. The optimum weight ratio of 1:5 for curcumin to Eudragit® EPO was used to incorporate into the raft forming systems. The raft forming formulations were composed of curcumin-Eudragit® EPO solid dispersions, sodium alginate as a gelling polymer and calcium carbonate for generating divalent Ca(2+) ions and carbon dioxide to form a floating raft. All formulations formed a gelled raft in 1min and sustained buoyancy on the 0.1N hydrochloric acid (pH 1.2) surface with a 60-85% release of curcumin within 8h. The curative effect on the acetic acid-induced chronic gastric ulcer in rats was determined. The curcumin raft forming formulations at 40mg/kg once daily showed a superior curative effect on the gastric ulcer in terms of the ulcer index and healing index than the standard antisecretory agent: lansoprazole (1mg/kg, twice daily) and a curcumin suspension (40mg/kg, twice daily). These studies demonstrated that the new raft forming systems containing curcumin solid dispersions are promising carriers for a stomach-specific delivery of poorly soluble lipophilic compounds. Copyright © 2015 Elsevier B.V. All rights reserved.

Improved Vemurafenib Dissolution and Pharmacokinetics as an Amorphous Solid Dispersion Produced by KinetiSol® Processing.

PubMed

Ellenberger, Daniel J; Miller, Dave A; Kucera, Sandra U; Williams, Robert O

2018-03-14

Vemurafenib is a poorly soluble, low permeability drug that has a demonstrated need for a solubility-enhanced formulation. However, conventional approaches for amorphous solid dispersion production are challenging due to the physiochemical properties of the compound. A suitable and novel method for creating an amorphous solid dispersion, known as solvent-controlled coprecipitation, was developed to make a material known as microprecipitated bulk powder (MBP). However, this approach has limitations in its processing and formulation space. In this study, it was hypothesized that vemurafenib can be processed by KinetiSol into the same amorphous formulation as MBP. The KinetiSol process utilizes high shear to rapidly process amorphous solid dispersions containing vemurafenib. Analysis of the material demonstrated that KinetiSol produced amorphous, single-phase material with acceptable chemical purity and stability. Values obtained were congruent to analysis conducted on the comparator material. However, the materials differed in particle morphology as the KinetiSol material was dense, smooth, and uniform while the MBP comparator was porous in structure and exhibited high surface area. The particles produced by KinetiSol had improved in-vitro dissolution and pharmacokinetic performance for vemurafenib compared to MBP due to slower drug nucleation and recrystallization which resulted in superior supersaturation maintenance during drug release. In the in-vivo rat pharmacokinetic study, both amorphous solid dispersions produced by KinetiSol exhibited mean AUC values at least two-fold that of MBP when dosed as a suspension. It was concluded that the KinetiSol process produced superior dosage forms containing vemurafenib with the potential for substantial reduction in patient pill burden.

[Study on solid dispersion of precipitated calcium carbonate-based oleanolic acid].

PubMed

Yan, Hong-mei; Zhang, Zhen-hai; Jia, Xiao-bin; Jiang, Yan-rong; Sun, E

2015-05-01

Oleanolic acid-precipitated calcium carbonate solid dispersion was prepared by using solvent evaporation method. The microscopic structure and physicochemical properties of solid dispersion were analyzed using differential scanning calorimetry and scanning electron microscopy (SEM). And its in vitro release also was investigated. The properties of the precipitated calcium carbonate was studied which was as a carrier of oleanolic acid solid dispersion. Differential scanning calorimetry analysis suggested that oleanolic acid may be present in solid dispersion as amorphous substance. The in vitro release determination results of oleanolic acid-precipitated calcium carbonate (1: 5) solid dispersion showed accumulated dissolution rate of.oleanolic acid was up to 90% at 45 min. Accelerating experiment showed that content and in vitro dissolution of oleanolic acid solid dispersion did not change after storing over 6 months. The results indicated that in vitro dissolution of oleanolic acid was improved greatly by the solid dispersion with precipitated calcium carbonate as a carrier. The solid dispersion is a stabilizing system which has actual applied value.

[Effect of stability and dissolution of realgar nano-particles using solid dispersion technology].

PubMed

Guo, Teng; Shi, Feng; Yang, Gang; Feng, Nian-Ping

2013-09-01

To improve the stability and dissolution of realgar nano-particles by solid dispersion. Using polyethylene glycol 6000 and poloxamer-188 as carriers, the solid dispersions were prepare by melting method. XRD, microscopic inspection were used to determine the status of realgar nano-particles in solid dispersions. The content and stability test of As(2)0(3) were determined by DDC-Ag method. Hydride generation atomic absorption spectrometry was used to determine the content of Arsenic and investigated the in vitro dissolution behavior of solid dispersions. The results of XRD and microscopic inspection showed that realgar nano-particles in solid dispersions were amorphous. The dissolution amount and rate of Arsenic from realgar nano-particles of all solid dispersions were increased significantly, the reunion of realgar nano-particles and content of As(2)0(3) were reduced for the formation of solid dispersions. The solid dispersion of realgar nano-particles with poloxamer-188 as carriers could obviously improve stability, dissolution and solubility.

Unraveling the Structure of Mn-Promoted Co/TiO2 Fischer-Tropsch Catalysts by In Situ X-Ray Absorption Spectroscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Grandjean, Didier; Morales, Fernando; Mens, Ad

2007-02-02

Combination of in situ X-ray absorption spectroscopy (XAFS) at the Co and Mn K-edges with electron microscopy (STEM-EELS) has allowed to unravel the complex structure of a series of unpromoted and Mn promoted TiO2-supported cobalt Fischer-Tropsch catalysts prepared by homogeneous deposition precipitation (HDP), both in their calcined and reduced states. After calcination the catalysts are generally composed of large Co3O4 aggregates (13-20 nm) and a MnO2-type phase that is either dispersed on the TiO2 surface or, for the major part, covering the Co3O4 particles. Additionally Mn is also forming a spinel-type Co3-xMnxO4 solid solution at the surface of the Co3O4more » particles. In pure Co or when small amount of this spinel-type phase are formed during calcination, reduction in H2 at 350 deg. C produces Co0 particles of variable sizes (3.5-15 nm) otherwise Co reduction is limited to the Co2+ state. Manganese that exists entirely in a Mn2+ state in the reduced catalysts is forming (1) a highly dispersed Ti2MnO4-type phase at the TiO2 surface, (2) a less dispersed MnO phase close to the cobalt particles that coexists with (3) a rock salt-type Mn1-xCoxO solid solution. Similarly, large amount of spinel solid solution in the calcined state favors the formation of Mn1-xCoxO-type solid solution during reduction showing that one of the main roles of the Mn promoter is to limit Co reducibility.« less

Mathematical Modeling of Torsional Surface Wave Propagation in a Non-Homogeneous Transverse Isotropic Elastic Solid Semi-Infinite Medium Under a Layer

NASA Astrophysics Data System (ADS)

Sethi, M.; Sharma, A.; Vasishth, A.

2017-05-01

The present paper deals with the mathematical modeling of the propagation of torsional surface waves in a non-homogeneous transverse isotropic elastic half-space under a rigid layer. Both rigidities and density of the half-space are assumed to vary inversely linearly with depth. Separation of variable method has been used to get the analytical solutions for the dispersion equation of the torsional surface waves. Also, the effects of nonhomogeneities on the phase velocity of torsional surface waves have been shown graphically. Also, dispersion equations have been derived for some particular cases, which are in complete agreement with some classical results.

Thermal shock resistance ceramic insulator

DOEpatents

Morgan, Chester S.; Johnson, William R.

1980-01-01

Thermal shock resistant cermet insulators containing 0.1-20 volume % metal present as a dispersed phase. The insulators are prepared by a process comprising the steps of (a) providing a first solid phase mixture of a ceramic powder and a metal precursor; (b) heating the first solid phase mixture above the minimum decomposition temperature of the metal precursor for no longer than 30 minutes and to a temperature sufficiently above the decomposition temperature to cause the selective decomposition of the metal precursor to the metal to provide a second solid phase mixture comprising particles of ceramic having discrete metal particles adhering to their surfaces, said metal particles having a mean diameter no more than 1/2 the mean diameter of the ceramic particles, and (c) densifying the second solid phase mixture to provide a cermet insulator having 0.1-20 volume % metal present as a dispersed phase.

Coating solid dispersions on microneedles via a molten dip coating method: development and in vitro evaluation for transdermal delivery of a water insoluble drug

PubMed Central

Ma, Yunzhe; Gill, Harvinder S.

2014-01-01

This study demonstrates for the first time the ability to coat solid dispersions on microneedles as a means to deliver water-insoluble drugs through the skin. Polyethylene glycol (PEG) was selected as the hydrophilic matrix, and lidocaine base was selected as the model hydrophobic drug to create the solid dispersion. First, thermal characterization and viscosity measurements of the PEG-lidocaine mixture at different mass fractions were performed. The results show that lidocaine can remain stable at temperatures up to ~130 °C, and that viscosity of the PEG-lidocaine molten solution increases as the mass fraction of lidocaine decreases. Differential scanning calorimetry demonstrated that at lidocaine mass fraction less than or equal to 50%, lidocaine is well dispersed in the PEG-lidocaine mixture. Uniform coatings were obtained on microneedle surfaces. In vitro dissolution studies in porcine skin showed that microneedles coated with PEG-lidocaine dispersions resulted in significantly higher delivery of lidocaine in just 3 min compared to 1 h topical application of 0.15 g EMLA®, a commercial lidocaine-prilocaine cream. In conclusion, the molten coating process we introduce here offers a practical approach to coat water-insoluble drugs on microneedles for transdermal delivery. PMID:25213295

Facile solid-state synthesis of highly dispersed Cu nanospheres anchored on coal-based activated carbons as an efficient heterogeneous catalyst for the reduction of 4-nitrophenol

NASA Astrophysics Data System (ADS)

Wang, Shan; Gao, Shasha; Tang, Yakun; Wang, Lei; Jia, Dianzeng; Liu, Lang

2018-04-01

Coal-based activated carbons (AC) were acted as the support, Cu/AC catalysts were synthesized by a facile solid-state reaction combined with subsequent heat treatment. In Cu/AC composites, highly dispersed Cu nanospheres were anchored on AC. The catalytic activity for 4-nitrophenol (4-NP) was investigated, the effects of activation temperature and copper loading on the catalytic performance were studied. The catalysts exhibited very high catalytic activity and moderate chemical stability due to the unique characteristics of the particle-assembled nanostructures, the high surface area and the porous structure of coal-based AC and the good dispersion of metal particles. Design and preparation of non-noble metal composite catalysts provide a new direction for improving the added value of coal.

A novel osmotic pump-based controlled delivery system consisting of pH-modulated solid dispersion for poorly soluble drug flurbiprofen: in vitro and in vivo evaluation.

PubMed

Li, Shujuan; Wang, Xiaoyu; Wang, Yingying; Zhao, Qianqian; Zhang, Lina; Yang, Xinggang; Liu, Dandan; Pan, Weisan

2015-01-01

In this study, a novel controlled release osmotic pump capsule consisting of pH-modulated solid dispersion for poorly soluble drug flurbiprofen (FP) was developed to improve the solubility and oral bioavailability of FP and to minimize the fluctuation of plasma concentration. The pH-modulated solid dispersion containing FP, Kollidon® 12 PF and Na2CO3 at a weight ratio of 1/4.5/0.02 was prepared using the solvent evaporation method. The osmotic pump capsule was assembled by semi-permeable capsule shell of cellulose acetate (CA) prepared by the perfusion method. Then, the solid dispersion, penetration enhancer, and suspending agents were tableted and filled into the capsule. Central composite design-response surface methodology was used to evaluate the influence of factors on the responses. A second-order polynomial model and a multiple linear model were fitted to correlation coefficient of drug release profile and ultimate cumulative release in 12 h, respectively. The actual response values were in good accordance with the predicted ones. The optimized formulation showed a complete drug delivery and zero-order release rate. Beagle dogs were used to be conducted in the pharmacokinetic study. The in vivo study indicated that the relative bioavailability of the novel osmotic pump system was 133.99% compared with the commercial preparation. The novel controlled delivery system with combination of pH-modulated solid dispersion and osmotic pump system is not only a promising strategy to improve the solubility and oral bioavailability of poorly soluble ionizable drugs but also an effective way to reduce dosing frequency and minimize the plasma fluctuation.

Solid lipid dispersions: potential delivery system for functional ingredients in foods.

PubMed

Asumadu-Mensah, Aboagyewa; Smith, Kevin W; Ribeiro, Henelyta S

2013-07-01

Structured solid lipid (SL) systems have the advantages of long-term physical stability, low surfactant concentrations, and may exhibit controlled release of active ingredients. In this research work, the potential use of high-melting SLs for the production of the above structured SL carrier systems was investigated. Dispersions containing either SL or blend of solid lipid and oil (SL+O) were produced by a hot melt high-pressure homogenization method. Experiments involved the use of 3 different SLs for the disperse phase: stearic acid, candelilla wax and carnauba wax. Sunflower oil was incorporated in the disperse phase for the production of the dispersions containing lipid and oil. In order to evaluate the practical aspects of structured particles, analytical techniques were used including: static light scattering to measure particle sizes, transmission electron microscopy (TEM) for investigating particle morphology and differential scanning calorimetry (DSC) to investigate the crystallization behavior of lipids in bulk and in dispersions. Results showed different mean particle sizes depending on the type of lipid used in the disperse phase. Particle sizes for the 3 lipids were: stearic acid (SL: 195 ± 2.5 nm; SL+O: 138 ± 6.0 nm); candelilla wax (SL: 178 ± 1.7 nm; SL+O: 144 ± 0.6 nm); carnauba wax (SL: 303 ± 1.5 nm; SL+O: 295 ± 5.0 nm). TEM results gave an insight into the practical morphology, showing plate-like and needle-like structures. DSC investigations also revealed that SL dispersions melted and crystallized at lower temperatures than the bulk. This decrease can be explained by the small particle sizes of the dispersion, the high-specific surface area, and the presence of a surfactant. © 2013 Institute of Food Technologists®

Development of an analytical method for crystalline content determination in amorphous solid dispersions produced by hot-melt extrusion using transmission Raman spectroscopy: A feasibility study.

PubMed

Netchacovitch, L; Dumont, E; Cailletaud, J; Thiry, J; De Bleye, C; Sacré, P-Y; Boiret, M; Evrard, B; Hubert, Ph; Ziemons, E

2017-09-15

The development of a quantitative method determining the crystalline percentage in an amorphous solid dispersion is of great interest in the pharmaceutical field. Indeed, the crystalline Active Pharmaceutical Ingredient transformation into its amorphous state is increasingly used as it enhances the solubility and bioavailability of Biopharmaceutical Classification System class II drugs. One way to produce amorphous solid dispersions is the Hot-Melt Extrusion (HME) process. This study reported the development and the comparison of the analytical performances of two techniques, based on backscattering and transmission Raman spectroscopy, determining the crystalline remaining content in amorphous solid dispersions produced by HME. Principal Component Analysis (PCA) and Partial Least Squares (PLS) regression were performed on preprocessed data and tended towards the same conclusions: for the backscattering Raman results, the use of the DuoScan™ mode improved the PCA and PLS results, due to a larger analyzed sampling volume. For the transmission Raman results, the determination of low crystalline percentages was possible and the best regression model was obtained using this technique. Indeed, the latter acquired spectra through the whole sample volume, in contrast with the previous surface analyses performed using the backscattering mode. This study consequently highlighted the importance of the analyzed sampling volume. Copyright © 2017 Elsevier B.V. All rights reserved.

Nonadditivity of van der Waals forces on liquid surfaces

NASA Astrophysics Data System (ADS)

Venkataram, Prashanth S.; Whitton, Jeremy D.; Rodriguez, Alejandro W.

2016-09-01

We present an approach for modeling nanoscale wetting and dewetting of textured solid surfaces that exploits recently developed, sophisticated techniques for computing exact long-range dispersive van der Waals (vdW) or (more generally) Casimir forces in arbitrary geometries. We apply these techniques to solve the variational formulation of the Young-Laplace equation and predict the equilibrium shapes of liquid-vacuum interfaces near solid gratings. We show that commonly employed methods of computing vdW interactions based on additive Hamaker or Derjaguin approximations, which neglect important electromagnetic boundary effects, can result in large discrepancies in the shapes and behaviors of liquid surfaces compared to exact methods.

[Preparation and in vitro dissolution of magnolol solid dispersion].

PubMed

Tang, Lan; Qiu, Shuai-Bo; Wu, Lan; Lv, Long-Fei; Lv, Hui-Xia; Shan, Wei-Guang

2016-02-01

In this study, solid dispersion system of magnolol in croscarmellose sodium was prepared by using the solvent evaporation method, in order to increase the drug dissolution. And its dissolution behavior, stability and physical characteristics were studied. The solid dispersion was prepared with magnolol and croscarmellose sodium, with the proportion of 1∶5, the in vitro dissolution of magnolol solid dispersion was up to 80.66% at 120 min, which was 6.9 times of magnolol. The results of DSC (differential scanning calorimetry), IR (infra-red) spectrum and SEM (scanning electron microscopy) showed that magnolol existed in solid dispersion in an amorphous form. After an accelerated stability test for six months, the drug dissolution and content in magnolol solid dispersion showed no significant change. So the solid dispersion prepared with croscarmellose sodium as the carrier can remarkably improve the stability and dissolution of magnolol. Copyright© by the Chinese Pharmaceutical Association.

Propagation of SH waves in an infinite/semi-infinite piezoelectric/piezomagnetic periodically layered structure.

PubMed

Pang, Yu; Liu, Yu-Shan; Liu, Jin-Xi; Feng, Wen-Jie

2016-04-01

In this paper, SH bulk/surface waves propagating in the corresponding infinite/semi-infinite piezoelectric (PE)/piezomagnetic (PM) and PM/PE periodically layered composites are investigated by two methods, the stiffness matrix method and the transfer matrix method. For a semi-infinite PE/PM or PM/PE medium, the free surface is parallel to the layer interface. Both PE and PM materials are assumed to be transversely isotropic solids. Dispersion equations are derived by the stiffness/transfer matrix methods, respectively. The effects of electric-magnetic (ME) boundary conditions at the free surface and the layer thickness ratios on dispersion curves are considered in detail. Numerical examples show that the results calculated by the two methods are the same. The dispersion curves of SH surface waves are below the bulk bands or inside the frequency gaps. The ratio of the layer thickness has an important effect not only on the bulk bands but also on the dispersion curves of SH surface waves. Electric and magnetic boundary conditions, respectively, determine the dispersion curves of SH surface waves for the PE/PM and PM/PE semi-infinite structures. The band structures of SH bulk waves are consistent for the PE/PM and PM/PE structures, however, the dispersive behaviors of SH surface waves are indeed different for the two composites. The realization of the above-mentioned characteristics of SH waves will make it possible to design PE/PM acoustic wave devices with periodical structures and achieve the better performance. Copyright © 2016 Elsevier B.V. All rights reserved.

Evaluation of the physicochemical characteristics of crospovidone that influence solid dispersion preparation.

PubMed

Nakanishi, Sayaka; Fujii, Makiko; Sugamura, Yuka; Suzuki, Ayako; Shibata, Yusuke; Koizumi, Naoya; Watanabe, Yoshiteru

2011-07-15

A solid dispersion (SD) powder of indomethacin (IM) with crospovidone (CrosPVP) shows useful characteristics for manufacturing dosage forms. Four types of commercial CroPVP, Polyplasdone XL (XL) used as the initial carrier, Polyplasdone XL10 and INF-10 manufactured by milling XL, and Kollidon CL (CL) marketed by another company, were compared. The limit of the IM-CrosPVP weight ratio with which an SD can be prepared (maximum IM content) was calculated on the basis of the heat of fusion of physical mixtures of IM and CrosPVP with various weight ratios. When Polyplasdones were used, the maximum IM content increased with the specific surface area of the CrosPVP. When CL was used, however, it was about half of that obtained with XL, even though the difference between XL and CL was not observed in the physicochemical characteristics (particle size, specific surface area, flowability, glass transition temperature, IR spectra, and solid state NMR spectra). As determined by pore size distribution measurement, the volume of pore of which size is larger than the particle size of IM was less in CL than in XL. Therefore, the effective surface area of CrosPVP that comes in contact with IM is important for the preparation of the SD. Copyright © 2011 Elsevier B.V. All rights reserved.

Effect of hydroxypropylcellulose and Tween 80 on physicochemical properties and bioavailability of ezetimibe-loaded solid dispersion.

PubMed

Rashid, Rehmana; Kim, Dong Wuk; Din, Fakhar Ud; Mustapha, Omer; Yousaf, Abid Mehmood; Park, Jong Hyuck; Kim, Jong Oh; Yong, Chul Soon; Choi, Han-Gon

2015-10-05

The purpose of this research was to evaluate the effect of the HPC (hydroxypropylcellulose) and Tween 80 on the physicochemical properties and oral bioavailability of ezetimibe-loaded solid dispersions. The binary solid dispersions were prepared with drug and various amounts of HPC. Likewise, ternary solid dispersions were prepared with different ratios of drug, HPC and Tween 80. Both types of solid dispersions were prepared using the solvent evaporation method. Their aqueous solubility, physicochemical properties, dissolution and oral bioavailability were investigated in comparison with the drug powder. All the solid dispersions significantly improved the drug solubility and dissolution. As the amount of HPC increased in the binary solid dispersions to 10-fold, the drug solubility and dissolution were increased accordingly. However, further increase in HPC did not result in significant differences among them. Similarly, up to 0.1-fold, Tween 80 increased the drug solubility in the ternary solid dispersions followed by no significant change. However, Tween 80 hardly affected the drug dissolution. The physicochemical analysis proved that the drug in binary and ternary solid dispersion was existed in the amorphous form. The particle-size measurements of these formulations were also not significantly different from each other, which showed that Tween 80 had no impact on physicochemical properties. The ezetimibe-loaded binary and ternary solid dispersions gave 1.6- and 1.8-fold increased oral bioavailability in rats, respectively, as compared to the drug powder; however, these values were not significantly different from each other. Thus, HPC greatly affected the solubility, dissolution and oral bioavailability of drug, but Tween 80 hardly did. Furthermore, this ezetimibe-loaded binary solid dispersion prepared only with HPC would be suggested as a potential formulation for oral administration of ezetimibe. Copyright © 2015 Elsevier Ltd. All rights reserved.

In vitro and in vivo studies on a novel solid dispersion of repaglinide using polyvinylpyrrolidone as the carrier.

PubMed

Yin, Li-Fang; Huang, Shi-Jing; Zhu, Chun-Li; Zhang, Shu-Hui; Zhang, Qiang; Chen, Xi-Jing; Liu, Qing-Wang

2012-11-01

In order to improve the dissolution and absorption of the water insoluble drug repaglinide, a solid dispersion was developed by solvent method using polyvinylpyrrolidone K30 (PVP K30) as the hydrophilic carrier for the first time. Studies indicated that both solubility and the dissolution rate of repaglinide were significantly increased in the solid dispersion system compared with that of repaglinide raw material or physical mixtures. The repaglinide solid dispersions with PVP K30 solid state was characterized by polarizing microscopy, differential scanning calorimetry (DSC), X-ray diffraction (XRD), and Fourier transform infrared spectroscopy (FT-IR). DSC and XRD studies indicated that repaglinide existed in an amorphous form in the solid dispersion. FT-IR analysis demonstrated the presence of intermolecular hydrogen bonding between repaglinide and PVP K30 in the solid dispersion. In the in situ gastrointestinal perfusion experiment, solid dispersion was shown to remarkably enhance the absorption of repaglinide in stomach and all segments of intestine. In vivo pharmacokinetic study in rats showed that immediate and complete release of repaglinide from the solid dispersion resulted in rapid absorption that significantly increased the bioavailability and the maximum plasma concentration over repaglinide raw material. These results demonstrated PVP K30 was an appropriate carrier for solid dispersion of repaglinide, with increased dissolution and oral absorption.

Development of novel sibutramine base-loaded solid dispersion with gelatin and HPMC: physicochemical characterization and pharmacokinetics in beagle dogs.

PubMed

Lim, Hyun-Tae; Balakrishnan, Prabagar; Oh, Dong Hoon; Joe, Kwan Hyung; Kim, Young Ran; Hwang, Doo Hyung; Lee, Yong-Bok; Yong, Chul Soon; Choi, Han-Gon

2010-09-15

To develop a novel sibutramine base-loaded solid dispersion with enhanced solubility and bioavailability, various solid dispersions were prepared using a spray drying technique with hydrophilic polymers such as gelatin, HPMC and citric acid. Their solubility, thermal characteristics and crystallinity were investigated. The dissolution and pharmacokinetics of the sibutramine base-loaded solid dispersion were then compared with a sibutramine hydrochloride monohydrate-loaded commercial product (Reductil). The solid dispersions prepared with gelatin gave higher drug solubility than those prepared without gelatin, irrespective of the amount of polymer. The sibutramine base-loaded solid dispersions containing hydrophilic polymer and citric acid showed higher drug solubility compared to sibutramine base and sibutramine hydrochloride monohydrate. Among the formulations tested, the solid dispersion composed of sibutramine base/gelatin/HPMC/citric acid at the weight ratio of 1/0.8/0.2/0.5 gave the highest solubility of 5.03+/-0.24 mg/ml. Our DSC and powder X-ray diffraction results showed that the drug was present in an altered amorphous form in this solid dispersion. The difference factor (f(1)) values between solid dispersion and commercial product were 2.82, 6.65 and 6.31 at pH 1.2, 4.0 and 6.8, respectively. Furthermore, they had the similarity factor (f(2)) value of 65.68, 53.43 and 58.97 at pH 1.2, 4.0 and 6.8, respectively. Our results suggested that the solid dispersion and commercial product produced a similar correlation of dissolution profiles at all pH ranges. The AUC, C(max) and T(max) of the parent drug and metabolite I and II from the solid dispersion were not significantly different from those of the commercial product, suggesting that the solid dispersion might be bioequivalent to the commercial product in beagle dogs. Thus, the sibutramine base-loaded solid dispersion prepared with gelatin, HPMC and citric acid is a promising candidate for improving the solubility and bioavailability of the poorly water-soluble sibutramine base. Crown Copyright 2010. Published by Elsevier B.V. All rights reserved.

Improving the dissolution rate of poorly water soluble drug by solid dispersion and solid solution: pros and cons.

PubMed

Chokshi, Rina J; Zia, Hossein; Sandhu, Harpreet K; Shah, Navnit H; Malick, Waseem A

2007-01-01

The solid dispersions with poloxamer 188 (P188) and solid solutions with polyvinylpyrrolidone K30 (PVPK30) were evaluated and compared in an effort to improve aqueous solubility and bioavailability of a model hydrophobic drug. All preparations were characterized by differential scanning calorimetry, powder X-ray diffraction, intrinsic dissolution rates, and contact angle measurements. Accelerated stability studies also were conducted to determine the effects of aging on the stability of various formulations. The selected solid dispersion and solid solution formulations were further evaluated in beagle dogs for in vivo testing. Solid dispersions were characterized to show that the drug retains its crystallinity and forms a two-phase system. Solid solutions were characterized to be an amorphous monophasic system with transition of crystalline drug to amorphous state. The evaluation of the intrinsic dissolution rates of various preparations indicated that the solid solutions have higher initial dissolution rates compared with solid dispersions. However, after storage at accelerated conditions, the dissolution rates of solid solutions were lower due to partial reversion to crystalline form. The drug in solid dispersion showed better bioavailability in comparison to solid solution. Therefore, considering physical stability and in vivo study results, the solid dispersion was the most suitable choice to improve dissolution rates and hence the bioavailability of the poorly water soluble drug.

Thunder-induced ground motions: 2. Site characterization

NASA Astrophysics Data System (ADS)

Lin, Ting-L.; Langston, Charles A.

2009-04-01

Thunder-induced ground motion, near-surface refraction, and Rayleigh wave dispersion measurements were used to constrain near-surface velocity structure at an unconsolidated sediment site. We employed near-surface seismic refraction measurements to first define ranges for site structure parameters. Air-coupled and hammer-generated Rayleigh wave dispersion curves were used to further constrain the site structure by a grid search technique. The acoustic-to-seismic coupling is modeled as an incident plane P wave in a fluid half-space impinging into a solid layered half-space. We found that the infrasound-induced ground motions constrained substrate velocities and the average thickness and velocities of the near-surface layer. The addition of higher-frequency near-surface Rayleigh waves produced tighter constraints on the near-surface velocities. This suggests that natural or controlled airborne pressure sources can be used to investigate the near-surface site structures for earthquake shaking hazard studies.

Lattice Waves, Spin Waves, and Neutron Scattering

DOE R&D Accomplishments Database

Brockhouse, Bertram N.

1962-03-01

Use of neutron inelastic scattering to study the forces between atoms in solids is treated. One-phonon processes and lattice vibrations are discussed, and experiments that verified the existence of the quantum of lattice vibrations, the phonon, are reviewed. Dispersion curves, phonon frequencies and absorption, and models for dispersion calculations are discussed. Experiments on the crystal dynamics of metals are examined. Dispersion curves are presented and analyzed; theory of lattice dynamics is considered; effects of Fermi surfaces on dispersion curves; electron-phonon interactions, electronic structure influence on lattice vibrations, and phonon lifetimes are explored. The dispersion relation of spin waves in crystals and experiments in which dispersion curves for spin waves in Co-Fe alloy and magnons in magnetite were obtained and the reality of the magnon was demonstrated are discussed. (D.C.W)

Development of megestrol acetate solid dispersion nanoparticles for enhanced oral delivery by using a supercritical antisolvent process.

PubMed

Ha, Eun-Sol; Kim, Jeong-Soo; Baek, In-Hwan; Yoo, Jin-Wook; Jung, Yunjin; Moon, Hyung Ryong; Kim, Min-Soo

2015-01-01

In the present study, solid dispersion nanoparticles with a hydrophilic polymer and surfactant were developed using the supercritical antisolvent (SAS) process to improve the dissolution and oral absorption of megestrol acetate. The physicochemical properties of the megestrol acetate solid dispersion nanoparticles were characterized using scanning electron microscopy, differential scanning calorimetry, powder X-ray diffraction, and a particle-size analyzer. The dissolution and oral bioavailability of the nanoparticles were also evaluated in rats. The mean particle size of all solid dispersion nanoparticles that were prepared was <500 nm. Powder X-ray diffraction and differential scanning calorimetry measurements showed that megestrol acetate was present in an amorphous or molecular dispersion state within the solid dispersion nanoparticles. Hydroxypropylmethyl cellulose (HPMC) solid dispersion nanoparticles significantly increased the maximum dissolution when compared with polyvinylpyrrolidone K30 solid dispersion nanoparticles. The extent and rate of dissolution of megestrol acetate increased after the addition of a surfactant into the HPMC solid dispersion nanoparticles. The most effective surfactant was Ryoto sugar ester L1695, followed by D-α-tocopheryl polyethylene glycol 1000 succinate. In this study, the solid dispersion nanoparticles with a drug:HPMC:Ryoto sugar ester L1695 ratio of 1:2:1 showed >95% rapid dissolution within 30 minutes, in addition to good oral bioavailability, with approximately 4.0- and 5.5-fold higher area under the curve (0-24 hours) and maximum concentration, respectively, than raw megestrol acetate powder. These results suggest that the preparation of megestrol acetate solid dispersion nanoparticles using the supercritical antisolvent process is a promising approach to improve the dissolution and absorption properties of megestrol acetate.

Stabilization and Amorphization of Lovastatin Using Different Types of Silica.

PubMed

Khanfar, Mai; Al-Nimry, Suhair

2017-08-01

Lovastatin (LOV), an antihyperlipidimic agent, is characterized by low solubility/poor dissolution and, thus, low bioavailability (<5%). A beneficial effect on its bioavailability could result from improving its dissolution. One of the most common methods used to enhance dissolution is the preparation of solid dispersions. Solid dispersions of LOV and silica with different surface areas were prepared. The effects of the type of silica, ratio of drug/silica, incubation period with silica, and the effect of surface area were all studied. Characterization of the prepared formulae for possible interaction between drug and polymer was carried out using differential scanning calorimetery, Fourier transform infrared spectroscopy, powder X-ray diffraction, surface area determination, and scanning electron microscopy. The dissolution profiles of all prepared formulae were constructed and evaluated. It was found that the formula made of LOV and Sylysia 350 FCP in a ratio of 1:5 after an incubation period of 48 h resulted in the best release, and it was stable after 3 months storage at 75% RH and 40°C.

Development and in-vivo assessment of the bioavailability of oridonin solid dispersions by the gas anti-solvent technique.

PubMed

Li, Songming; Liu, Ying; Liu, Tao; Zhao, Ling; Zhao, Jihui; Feng, Nianping

2011-06-15

We developed solid dispersions, using the gas anti-solvent technique (GAS), to improve the oral bioavailability of the poorly water-soluble active component oridonin. The solubility of oridonin in supercritical carbon dioxide was measured under various pressures and temperatures. To prepare oridonin solid dispersions using the GAS technique, ethanol was used as the solvent, CO(2) was used as the anti-solvent and the hydrophilic polymer polyvinylpyrrolidone K17 (PVP K17) was used as the drug carrier matrix. Characterization of the obtained preparations was undertaken using scanning electron microscopy (SEM), X-ray diffraction (XRD) analyses and a drug release study. Oridonin solid dispersions were formed and oridonin was present in an amorphous form in these dispersions. Oridonin solid dispersions significantly increased the drug dissolution rate compared with that of oridonin powder, primarily through drug amorphization. Compared with the physical mixture of oridonin and PVP K17, oridonin solid dispersions gave higher values of AUC and C(max), and the absorption of oridonin from solid dispersions resulted in 26.4-fold improvement in bioavailability. The present study illustrated the feasibility of applying the GAS technique to prepare oridonin solid dispersions, and of using them for the delivery of oridonin via the oral route. Copyright © 2011 Elsevier B.V. All rights reserved.

Improving the chemical stability of amorphous solid dispersion with cocrystal technique by hot melt extrusion.

PubMed

Liu, Xu; Lu, Ming; Guo, Zhefei; Huang, Lin; Feng, Xin; Wu, Chuanbin

2012-03-01

To explore in-situ forming cocrystal as a single-step, efficient method to significantly depress the processing temperature and thus minimize the thermal degradation of heat-sensitive drug in preparation of solid dispersions by melting method (MM) and hot melt extrusion (HME). Carbamazepine (CBZ)-nicotinamide (NIC) cocrystal solid dispersions were prepared with polymer carriers PVP/VA, SOLUPLUS and HPMC by MM and/or HME. The formation of cocrystal was investigated by differential scanning calorimetry and hot stage polarized optical microscopy. State of CBZ in solid dispersion was characterized by X-ray powder diffraction and optical microscopy. Interactions between CBZ, NIC and polymers were investigated by FTIR. Dissolution behaviors of solid dispersions were compared with that of pure CBZ. CBZ-NIC cocrystal with melting point of 160°C was formed in polymer carriers during heating process, and the preparation temperature of amorphous CBZ solid dispersion was therefore depressed to 160°C. The dissolution rate of CBZ-NIC cocrystal solid dispersion was significantly increased. By in-situ forming cocrystal, chemically stable amorphous solid dispersions were prepared by MM and HME at a depressed processing temperature. This method provides an attractive opportunity for HME of heat-sensitive drugs.

Application of spherical silicate to prepare solid dispersion dosage forms with aqueous polymers.

PubMed

Nagane, Kentaro; Kimura, Susumu; Ukai, Koji; Takahashi, Chisato; Ogawa, Noriko; Yamamoto, Hiromitsu

2015-09-30

The objective of this study is to prepare and characterize solid dispersions of nifedipine (NP) using porous spherical silicate micro beads (MB) that were approximately 100 μm in diameter with vinylpyrrolidone/vinyl acetate copolymer (PVP/VA) and a Wurster-type fluidized bed granulator. Compared with previously reported solid dispersion using only MB, the supersaturation of NP dissolved from the proposed system of MB and PVP/VA was maintained during dissolution tests. The proposed system produced a solid dispersion product coated on MB, and morphology was maintained after the coating process to prepare solid dispersion; therefore, the powder characteristics, such as flowability of the proposed solid dispersion product, was tremendously preferable to that of the conventional spray-dried solid dispersions of NP with PVP/VA, expecting to make the consequent manufacturing processes easy for development. Another advantage in the terms of manufacturing is its simple process to prepare solid dispersion by spraying the drug and polymer that were dissolved in an organic solvent onto a MB in a Wurster-type fluidized bed granulator, thus, simplifying the optimization and scale-up with ease. Copyright © 2015 Elsevier B.V. All rights reserved.

Development of novel ibuprofen-loaded solid dispersion with enhanced bioavailability using cycloamylose.

PubMed

Baek, Hyung Hee; Kim, Dae-Hwan; Kwon, So Young; Rho, Shin-Joung; Kim, Dong-Wuk; Choi, Han-Gon; Kim, Yong-Ro; Yong, Chul Soon

2012-03-01

To develop a novel ibuprofen-loaded solid dispersion with enhanced bioavailability using cycloamylose, it was prepared using spray-drying techniques with cycloamylose at a weight ratio of 1:1. The effect of cycloamylose on aqueous solubility of ibuprofen was investigated. The physicochemical properties of solid dispersions were investigated using scanning electron microscopy (SEM), differential scanning calorimetry (DSC), and X-ray diffraction. The dissolution and bioavailability in rats were evaluated compared with ibuprofen powder. This ibuprofen-loaded solid dispersion improved about 14-fold drug solubility. Ibuprofen was present in an unchanged crystalline state, and cycloamylose played the simple role of a solubilizing agent in this solid dispersion. Moreover, the dispersion gave 2-fold higher AUC (area under the drug concentration-time curve) value compared with a ibuprofen powder, indicating that it improved the oral bioavailability of ibuprofen in rats. Thus, the solid dispersion may be useful to deliver ibuprofen with enhanced bioavailability without crystalline change.

Solid Lubrication by Multiwalled Carbon Nanotubes in Air and in Vacuum for Space and Aeronautics Applications

NASA Technical Reports Server (NTRS)

Miyoshi, Kazuhisa; Street, Kenneth W., Jr.; Andraws, Rodney; Jacques, David; VanderWal, Randy L.; Sayir, Ali

2005-01-01

To evaluate recently developed aligned multiwalled carbon nanotubes (MWNTs) and dispersed MWNTs for solid lubrication applications, unidirectional sliding friction experiments were conducted with 440 C stainless steel balls and hemispherical alumina-yttria stabilized zirconia pins in sliding contact with the MWNTs deposited on quartz disks in air and in vacuum. The results indicate that MWNTs have superior solid lubrication friction properties and endurance lives in air and vacuum under dry conditions. The coefficient of friction of the dispersed MWNTs is close to 0.05 and 0.009 in air and in vacuum, respectively, showing good dry lubricating ability. The wear life of MWNTs exceeds 1 million passes in both air and vacuum showing good durability. In general, the low coefficient of friction can be attributed to the combination of the transferred, agglomerated patches of MWNTs on the counterpart ball or pin surfaces and the presence of tubular MWNTs at interfaces.

Refined potentials for rare gas atom adsorption on rare gas and alkali-halide surfaces

NASA Technical Reports Server (NTRS)

Wilson, J. W.; Heinbockel, J. H.; Outlaw, R. A.

1985-01-01

The utilization of models of interatomic potential for physical interaction to estimate the long range attractive potential for rare gases and ions is discussed. The long range attractive force is calculated in terms of the atomic dispersion properties. A data base of atomic dispersion parameters for rare gas atoms, alkali ion, and halogen ions is applied to the study of the repulsive core; the procedure for evaluating the repulsive core of ion interactions is described. The interaction of rare gas atoms on ideal rare gas solid and alkali-halide surfaces is analyzed; zero coverage absorption potentials are derived.

Comparison of HPMC based polymers performance as carriers for manufacture of solid dispersions using the melt extruder.

PubMed

Ghosh, Indrajit; Snyder, Jennifer; Vippagunta, Radha; Alvine, Marilyn; Vakil, Ronak; Tong, Wei-Qin; Vippagunta, Sudha

2011-10-31

Preparation of amorphous solid dispersions using hot-melt extrusion process for poorly water soluble compounds which degrade on melting remains a challenge due to exposure to high temperatures. The aim of this study was to develop a physically and chemically stable amorphous solid dispersion of a poorly water-soluble compound, NVS981, which is highly thermal sensitive and degrades upon melting at 165 °C. Hydroxypropyl Methyl Cellulose (HPMC) based polymers; HPMC 3cps, HPMC phthalate (HPMCP) and HPMC acetyl succinate (HPMCAS) were selected as carriers to prepare solid dispersions using hot melt extrusion because of their relatively low glass transition temperatures. The solid dispersions were compared for their ease of manufacturing, physical stability such as recrystallization potential, phase separation, molecular mobility and enhancement of drug dissolution. Two different drug loads of 20 and 50% (w/w) were studied in each polymer system. It was interesting to note that solid dispersions with 50% (w/w) drug load were easier to process in the melt extruder compared to 20% (w/w) drug load in all three carriers, which was attributed to the plasticizing behavior of the drug substance. Upon storage at accelerated stability conditions, no phase separation was observed in HPMC 3cps and HPMCAS solid dispersions at the lower and higher drug load, whereas for HPMCP, phase separation was observed at higher drug load after 3 months. The pharmaceutical performance of these solid dispersions was evaluated by studying drug dissolution in pH 6.8 phosphate buffer. Drug release from solid dispersion prepared from polymers used for enteric coating, i.e. HPMCP and HPMCAS was faster compared with the water soluble polymer HPMC 3cps. In conclusion, of the 3 polymers studied for preparing solid dispersions of thermally sensitive compound using hot melt extrusion, HPMCAS was found to be the most promising as it was easily processible and provided stable solid dispersions with enhanced dissolution. Copyright © 2011 Elsevier B.V. All rights reserved.

Mathematical model to analyze the dissolution behavior of metastable crystals or amorphous drug accompanied with a solid-liquid interface reaction.

PubMed

Hirai, Daiki; Iwao, Yasunori; Kimura, Shin-Ichiro; Noguchi, Shuji; Itai, Shigeru

2017-04-30

Metastable crystals and the amorphous state of poorly water-soluble drugs in solid dispersions (SDs), are subject to a solid-liquid interface reaction upon exposure to a solvent. The dissolution behavior during the solid-liquid interface reaction often shows that the concentration of drugs is supersaturated, with a high initial drug concentration compared with the solubility of stable crystals but finally approaching the latter solubility with time. However, a method for measuring the precipitation rate of stable crystals and/or the potential solubility of metastable crystals or amorphous drugs has not been established. In this study, a novel mathematical model that can represent the dissolution behavior of the solid-liquid interface reaction for metastable crystals or amorphous drug was developed and its validity was evaluated. The theory for this model was based on the Noyes-Whitney equation and assumes that the precipitation of stable crystals at the solid-liquid interface occurs through a first-order reaction. Moreover, two models were developed, one assuming that the surface area of the drug remains constant because of the presence of excess drug in the bulk and the other that the surface area changes in time-dependency because of agglomeration of the drug. SDs of Ibuprofen (IB)/polyvinylpyrrolidone (PVP) were prepared and their dissolution behaviors under non-sink conditions were fitted by the models to evaluate improvements in solubility. The model assuming time-dependent surface area showed good agreement with experimental values. Furthermore, by applying the model to the dissolution profile, parameters such as the precipitation rate and the potential solubility of the amorphous drug were successfully calculated. In addition, it was shown that the improvement in solubility with supersaturation was able to be evaluated quantitatively using this model. Therefore, this mathematical model would be a useful tool to quantitatively determine the supersaturation concentration of a metastable drug from solid dispersions. Copyright © 2017 Elsevier B.V. All rights reserved.

Spread of pathogens through rain drop impact

NASA Astrophysics Data System (ADS)

Kim, Seungho; Gruszewski, Hope; Gidley, Todd; Schmale, David G., III; Jung, Sunghwan

2017-11-01

Rain drop impact can disperse micron-sized pathogenic particles over long distances. In this study, we aim to elucidate mechanisms for disease dispersal when a rain drop impacts a particle-laden solid surface. Three different dispersal types were observed depending on whether the dispersed glass particles were dry or wet. For a dry particle dispersal, the movement of contact line made the particles initially jump off the surface with relatively high velocity. Then, air vortex was formed due to the air current entrained along with the falling drop, and advected the particles with relatively low velocity. For a wet particle dispersal, the contact line of a spreading liquid became unstable due to the presence of the particles on the substrate. This caused splashing at the contact line and ejected liquid droplets carrying the particles. Finally, we released a drop onto wheat plants infected with the rust fungus, Puccinia triticina, and found that nearly all of the satellite droplets from a single drop contained at least one rust spore. Also, we visualized such novel dispersal dynamics with a high-speed camera and characterized their features by scaling models. This research was partially supported by National Science Foundation Grant CBET-1604424.

Molecular implications of drug-polymer solubility in understanding the destabilization of solid dispersions by milling.

PubMed

Yang, Ziyi; Nollenberger, Kathrin; Albers, Jessica; Qi, Sheng

2014-07-07

The solubility of drugs in polymer matrixes has been recognized as one of the key factors governing the physical stability of solid dispersions. This study has explored the implications of drug solubility on the destabilization that occurs on milling, which is often used as an additional process for hot melt extruded (HME) solid dispersions. The theoretical drug solubility in the polymer was first predicted using various theoretical and experimental approaches. The destabilization effects of high-energy mechanical milling on the solid dispersions with drug loadings below and above the predicted solubility were then investigated using a range of thermal, microscopic, and spectroscopic techniques. Four model drug-polymer combinations were studied. The HME formulations with drug loading below the predicted solid solubility (undersaturated and true molecular dispersion) showed good stability against milling. In contrast, milling destabilized supersaturated HME dispersions via increasing molecular mobility and creating phase-separated, amorphous, drug-rich domains. However, these additional amorphous drug-rich domains created by milling show good stability under ambient conditions, though crystallization can be accelerated by additional heating. These results highlighted that the processing method used to prepare the solid dispersions may play a role in facilitating the stabilization of amorphous drug in supersaturated solid dispersions. The degree of supersaturation of the drug in the polymer showed significant impact on the destabilization behavior of milling on solid dispersions. An improved understanding of the destabilization behavior of solid dispersions upon milling can provide new insights into the processing related apparent solubility of drugs in polymers.

Preparation and characterization of azithromycin--Aerosil 200 solid dispersions with enhanced physical stability.

PubMed

Li, Xuechao; Peng, Huanhuan; Tian, Bin; Gou, Jingxin; Yao, Qing; Tao, Xiaoguang; He, Haibing; Zhang, Yu; Tang, Xing; Cai, Cuifang

2015-01-01

The main purpose of this study was to investigate the feasibility of azithromycin (AZI)--Aerosil 200 solid dispersions specifically with high stability under accelerated condition (40 °C/75% RH). Ball milling (BM) and hot-melt extrusion (HME) were used to prepare AZI solid dispersions. The physical properties of solid dispersions were evaluated by differential scanning calorimetry (DSC), scanning electron microscopy (SEM), powder X-ray diffraction (PXRD), Fourier transform infrared spectroscopy (FT-IR) and thermogravimetric analysis (TGA). For solid dispersions prepared with both methods, no crystalline of AZI was detected (except for AZI: Aerosil 200=75:25) by DSC or PXRD, indicating the amorphous state of AZI in solid dispersions. The FT-IR results demonstrated the loss of crystallization water and the formation of hydrogen bonds between Aerosil 200 and AZI during the preparation of solid dispersions. After 4 weeks storage under accelerated condition, the degree of crystallinity of AZI increased in solid dispersions prepared by BM, whereas for solid dispersions containing AZI, Aerosil 200 and glyceryl behenate (GB) prepared by HME, no crystalline of AZI was identified. This high stability can be attributed to the hydrophobic properties of GB and the presence of hydrogen bonds. Based on the above results, it is inferred the protection of hydrogen bonds between AZI and Aerosil 200 formed during preparation process effectively inhibited the recrystallization of AZI and improved the physical stability of amorphous AZI in the presence of Aerosil 200. Copyright © 2015 Elsevier B.V. All rights reserved.

Fusion processing of itraconazole solid dispersions by kinetisol dispersing: a comparative study to hot melt extrusion.

PubMed

DiNunzio, James C; Brough, Chris; Miller, Dave A; Williams, Robert O; McGinity, James W

2010-03-01

KinetiSol Dispersing (KSD) is a novel high energy manufacturing process investigated here for the production of pharmaceutical solid dispersions. Solid dispersions of itraconazole (ITZ) and hypromellose were produced by KSD and compared to identical formulations produced by hot melt extrusion (HME). Materials were characterized for solid state properties by modulated differential scanning calorimetry and X-ray diffraction. Dissolution behavior was studied under supersaturated conditions. Oral bioavailability was determined using a Sprague-Dawley rat model. Results showed that KSD was able to produce amorphous solid dispersions in under 15 s while production by HME required over 300 s. Dispersions produced by KSD exhibited single phase solid state behavior indicated by a single glass transition temperature (T(g)) whereas compositions produced by HME exhibited two T(g)s. Increased dissolution rates for compositions manufactured by KSD were also observed compared to HME processed material. Near complete supersaturation was observed for solid dispersions produced by either manufacturing processes. Oral bioavailability from both processes showed enhanced AUC compared to crystalline ITZ. Based on the results presented from this study, KSD was shown to be a viable manufacturing process for the production of pharmaceutical solid dispersions, providing benefits over conventional techniques including: enhanced mixing for improved homogeneity and reduced processing times. 2009 Wiley-Liss, Inc. and the American Pharmacists Association

To evaluate the change in release from solid dispersion using sodium lauryl sulfate and model drug sulfathiazole.

PubMed

Dave, Rutesh H; Patel, Hardikkumar H; Donahue, Edward; Patel, Ashwinkumar D

2013-10-01

The solubility of drugs remains one of the most challenging aspects of formulation development. There are numerous ways to improve the solubility of drugs amongst which the most promising strategy is solid dispersion. Different ratios of sulfathiazole: PVP-K29/32: sodium lauryl sulfate (SLS) were prepared (1:1:0.1, 1:1:0.5, 1:1:1) and various methods were employed to characterize the prepared solid dispersions, namely modulated differential scanning calorimeter, X-ray powder diffraction, Fourier Transformed Infrared Spectroscopy and dissolution studies. Lack of crystallinity was observed in internal and external systems suggesting a loss of crystallinity, whereas the physical mixtures showed a characteristic peak of sulfathiazole. In vitro dissolution results clearly showed that the incorporation of a relatively small amount of surfactants (5, 20 or 33% w/w) into a solid dispersion can improve its dissolution rates compared to binary solid dispersion (SD) alone and pure sulfathiazole. In all ratios solid dispersion internal shows a higher dissolution rate compared to a physical mixture and solid dispersion external which suggests that the way that the surfactant is incorporated into the solid dispersion plays an important role in changing the solubility of a drug. The solubilization mechanism is mainly responsible for this higher dissolution rate when we incorporate the SLS in SD.

Orally Disintegrating Tablets Containing Melt Extruded Amorphous Solid Dispersion of Tacrolimus for Dissolution Enhancement.

PubMed

Ponnammal, Poovizhi; Kanaujia, Parijat; Yani, Yin; Ng, Wai Kiong; Tan, Reginald B H

2018-03-16

In order to improve the aqueous solubility and dissolution of Tacrolimus (TAC), amorphous solid dispersions of TAC were prepared by hot melt extrusion with three hydrophilic polymers, Polyvinylpyrrolidone vinyl acetate (PVP VA64), Soluplus ® and Hydroxypropyl Cellulose (HPC), at a drug loading of 10% w / w . Molecular modeling was used to determine the miscibility of the drug with the carrier polymers by calculating the Hansen Solubility Parameters. Powder X-ray diffraction and differential scanning calorimetry (DSC) studies of powdered solid dispersions revealed the conversion of crystalline TAC to amorphous form. Fourier transform Infrared (FTIR) spectroscopy results indicated formation of hydrogen bond between TAC and polymers leading to stabilization of TAC in amorphous form. The extrudates were found to be stable under accelerated storage conditions for 3 months with no re-crystallization, indicating that hot melt extrusion is suitable for producing stable amorphous solid dispersions of TAC in PVP VA64, Soluplus ® and HPC. Stable solid dispersions of amorphous TAC exhibited higher dissolution rate, with the solid dispersions releasing more than 80% drug in 15 min compared to the crystalline drug giving 5% drug release in two hours. These stable solid dispersions were incorporated into orally-disintegrating tablets in which the solid dispersion retained its solubility, dissolution and stability advantage.

Orally Disintegrating Tablets Containing Melt Extruded Amorphous Solid Dispersion of Tacrolimus for Dissolution Enhancement

PubMed Central

Ponnammal, Poovizhi; Kanaujia, Parijat; Ng, Wai Kiong; Tan, Reginald B. H.

2018-01-01

In order to improve the aqueous solubility and dissolution of Tacrolimus (TAC), amorphous solid dispersions of TAC were prepared by hot melt extrusion with three hydrophilic polymers, Polyvinylpyrrolidone vinyl acetate (PVP VA64), Soluplus® and Hydroxypropyl Cellulose (HPC), at a drug loading of 10% w/w. Molecular modeling was used to determine the miscibility of the drug with the carrier polymers by calculating the Hansen Solubility Parameters. Powder X-ray diffraction and differential scanning calorimetry (DSC) studies of powdered solid dispersions revealed the conversion of crystalline TAC to amorphous form. Fourier transform Infrared (FTIR) spectroscopy results indicated formation of hydrogen bond between TAC and polymers leading to stabilization of TAC in amorphous form. The extrudates were found to be stable under accelerated storage conditions for 3 months with no re-crystallization, indicating that hot melt extrusion is suitable for producing stable amorphous solid dispersions of TAC in PVP VA64, Soluplus® and HPC. Stable solid dispersions of amorphous TAC exhibited higher dissolution rate, with the solid dispersions releasing more than 80% drug in 15 min compared to the crystalline drug giving 5% drug release in two hours. These stable solid dispersions were incorporated into orally-disintegrating tablets in which the solid dispersion retained its solubility, dissolution and stability advantage. PMID:29547585

Enhancement of solubility and dissolution of coenzyme Q10 using solid dispersion formulation.

PubMed

Nepal, Pushp R; Han, Hyo-Kyung; Choi, Hoo-Kyun

2010-01-04

This study aimed to develop a stable solid dispersion of Coenzyme Q(10) (CoQ(10)) with high aqueous solubility and dissolution rate. Among various carriers screened, poloxamer 407 was most effective to form a superior solid dispersion of CoQ(10) having significantly enhanced solubility. Particularly, solid dispersion of CoQ(10) with poloxamer 407 in the weight ratio of 1:5 prepared by melting method enhanced the solubility of CoQ(10) to the greatest extent. However, it exhibited poor stability and hence Aerosil 200 (colloidal silicon dioxide) was incorporated into the solid dispersion as an adsorbent to inhibit the recrystallization process. The solid dispersion of CoQ(10), poloxamer 407 and Aerosil 200 in the weight ratio of 1:5:6 exhibited improved stability with no significant change in solubility during the 1-month stability test. Moreover, the solid dispersion formulation containing Aerosil 200 significantly enhanced the extent of drug release (approx. 75% release) as well as the dissolution rate of CoQ(10). In conclusion, the present study has developed the stable solid dispersion formulation of CoQ(10) with poloxamer 407 and Aerosil 200 for the enhanced solubility and dissolution of CoQ(10), which could also offer some additional advantages including ease of preparation, good flowability and cost-effectiveness.

Enhanced Physical Stability of Amorphous Drug Formulations via Dry Polymer Coating.

PubMed

Capece, Maxx; Davé, Rajesh

2015-06-01

Although amorphous solid drug formulations may be advantageous for enhancing the bioavailability of poorly soluble active pharmaceutical ingredients, they exhibit poor physical stability and undergo recrystallization. To address this limitation, this study investigates stability issues associated with amorphous solids through analysis of the crystallization behavior for acetaminophen (APAP), known as a fast crystallizer, using a modified form of the Avrami equation that kinetically models both surface and bulk crystallization. It is found that surface-enhanced crystallization, occurring faster at the free surface than in the bulk, is the major impediment to the stability of amorphous APAP. It is hypothesized that a novel use of a dry-polymer-coating process referred to as mechanical-dry-polymer-coating may be used to inhibit surface crystallization and enhance stability. The proposed process, which is examined, simultaneously mills and coats amorphous solids with polymer, while avoiding solvents or solutions, which may otherwise cause stability or crystallization issues during coating. It is shown that solid dispersions of APAP (64% loading) with a small particle size (28 μm) could be prepared and coated with the polymer, carnauba wax, in a vibratory ball mill. The resulting amorphous solid was found to have excellent stability as a result of inhibition of surface crystallization. © 2015 Wiley Periodicals, Inc. and the American Pharmacists Association.

Acoustic activation of water-in-oil microemulsions for controlled salt dissolution.

PubMed

Baxamusa, Salmaan; Ehrmann, Paul; Ong, Jemi

2018-06-18

The dynamic nature of the oil-water interface allows for sequestration of material within the dispersed domains of a microemulsion. Microstructural changes should therefore change the dissolution rate of a solid surface in a microemulsion. We hypothesize that microstructural changes due to formulation and cavitation in an acoustic field will enable control over solid dissolution rates. Water-in-oil microemulsions were formulated using cyclohexane, water, Triton X-100, and hexanol. The microstructure and solvation properties of Winsor Type IV formulations were characterized. Dissolution rates of KH 2 PO 4 (KDP), were measured. A kinetic analysis isolated the effect of the microstructure, and rate enhancements due to cavitation effects on the microstructure were characterized by measuring dissolution rates in an ultrasonic field. Dispersed aqueous domains of 2-6 nm radius dissolve a solid block of KDP at 0-10 nm/min. Dissolution rate is governed not by the domain-surface collision frequency but rather by a dissolution probability per domain-surface encounter. Higher probabilities are correlated with larger domains. Rapid and reversible dissolution rate increases of up to 270× were observed under ultrasonic conditions, with <20% of the increase due to bulk heating effects. The rest is attributed to cavitation-induced changes to the domain microstructure, providing a simple method for remotely activating and de-activating dissolution. Copyright © 2018 Elsevier Inc. All rights reserved.

Enhancing the bioavailability of magnolol in rabbits using melting solid dispersion with polyvinylpyrrolidone.

PubMed

Lin, Shiuan-Pey; Hou, Yu-Chi; Liao, Tzu-Yun; Tsai, Shang-Yuan

2014-03-01

Preparation of magnolol-loaded amorphous solid dispersion was investigated for improving the bioavailability. A solid dispersion of magnolol was prepared with polyvinylpyrrolidone K-30 (PVP) by melting method, and the physical properties were characterized by using differential scanning calorimetry, powder X-ray diffractometry, Fourier transformation-infrared spectroscopy and scanning electron microscope. In addition, dissolution test was also performed. Subsequently, the bioavailability of magnolol pure compound, its physical mixture and solid dispersion were compared in rabbits. The blood samples withdrawn via marginal ear vein at specific time points were assayed by HPLC method. Oral administration of the solid dispersion of magnolol with PVP significantly increased the systemic exposures of magnolol and magnolol sulfates/glucuronides by 80.1% and 142.8%, respectively, compared to those given with magnolol pure compound. Magnolol-loaded amorphous solid dispersion with PVP has demonstrated enhanced bioavailability of magnolol in rabbits.

Molecular-level understanding of protein adsorption at the interface between water and a strongly interacting uncharged solid surface.

PubMed

Penna, Matthew J; Mijajlovic, Milan; Biggs, Mark J

2014-04-09

Although protein adsorption on solids is of immense relevance, experimental limitations mean there is still a remarkable lack of understanding of the adsorption mechanism, particularly at a molecular level. By subjecting 240+ molecular dynamics simulations of two peptide/water/solid surface systems to statistical analysis, a generalized molecular level mechanism for peptide adsorption has been identified for uncharged surfaces that interact strongly with the solution phase. This mechanism is composed of three phases: (1) biased diffusion of the peptide from the bulk phase toward the surface; (2) anchoring of the peptide to the water/solid interface via interaction of a hydrophilic group with the water adjacent to the surface or a strongly interacting hydrophobic group with the surface; and (3) lockdown of the peptide on the surface via a slow, stepwise and largely sequential adsorption of its residues, which we term 'statistical zippering'. The adsorption mechanism is dictated by the existence of water layers adjacent to the solid and orientational ordering therein. By extending the solid into the solution by ~8 Å and endowing it with a charged character, the water layers ensure the peptide feels the effect of the solid at a range well beyond the dispersion force that arises from it, thus inducing biased diffusion from afar. The charging of the interface also facilitates anchoring of the peptide near the surface via one of its hydrophilic groups, allowing it time it would otherwise not have to rearrange and lockdown. Finally, the slowness of the lockdown process is dictated by the need for the peptide groups to replace adjacent tightly bound interfacial water.

Improved physicochemical characteristics of felodipine solid dispersion particles by supercritical anti-solvent precipitation process.

PubMed

Won, Dong-Han; Kim, Min-Soo; Lee, Sibeum; Park, Jeong-Sook; Hwang, Sung-Joo

2005-09-14

Solid dispersions of felodipine were formulated with HPMC and surfactants by the conventional solvent evaporation (CSE) and supercritical anti-solvent precipitation (SAS) methods. The solid dispersion particles were characterized by particle size, zeta potential, scanning electron microscopy (SEM), differential scanning calorimetry (DSC), powder X-ray diffraction (XRD), solubility and dissolution studies. The effects of the drug/polymer ratio and surfactants on the solubility of felodipine were also studied. The mean particle size of the solid dispersions was 200-250 nm; these had a relatively regular spherical shape with a narrow size distribution. The particle size of the solid dispersions from the CSE method increased at 1 h after dispersed in distilled water. However, the particle sizes of solid dispersions from the SAS process were maintained for 6 h due to the increased solubility of felodipine. The physical state of felodipine changed from crystalline to amorphous during the CSE and SAS processes, confirmed by DSC/XRD data. The equilibrium solubility of the felodipine solid dispersion prepared by the SAS process was 1.5-20 microg/ml, while the maximum solubility was 35-110 microg/ml. Moreover, the solubility of felodipine increased with decreasing drug/polymer ratio or increasing HCO-60 content. The solid dispersions from the SAS process showed a high dissolution rate of over 90% within 2 h. The SAS process system may be used to enhance solubility or to produce oral dosage forms with high dissolution rate.

Soliton solutions to the fifth-order Korteweg-de Vries equation and their applications to surface and internal water waves

NASA Astrophysics Data System (ADS)

Khusnutdinova, K. R.; Stepanyants, Y. A.; Tranter, M. R.

2018-02-01

We study solitary wave solutions of the fifth-order Korteweg-de Vries equation which contains, besides the traditional quadratic nonlinearity and third-order dispersion, additional terms including cubic nonlinearity and fifth order linear dispersion, as well as two nonlinear dispersive terms. An exact solitary wave solution to this equation is derived, and the dependence of its amplitude, width, and speed on the parameters of the governing equation is studied. It is shown that the derived solution can represent either an embedded or regular soliton depending on the equation parameters. The nonlinear dispersive terms can drastically influence the existence of solitary waves, their nature (regular or embedded), profile, polarity, and stability with respect to small perturbations. We show, in particular, that in some cases embedded solitons can be stable even with respect to interactions with regular solitons. The results obtained are applicable to surface and internal waves in fluids, as well as to waves in other media (plasma, solid waveguides, elastic media with microstructure, etc.).

Effect of Compression on the Molecular Arrangement of Itraconazole-Soluplus Solid Dispersions: Induction of Liquid Crystals or Exacerbation of Phase Separation?

PubMed

Singh, Abhishek; Bharati, Avanish; Frederiks, Pauline; Verkinderen, Olivier; Goderis, Bart; Cardinaels, Ruth; Moldenaers, Paula; Van Humbeeck, Jan; Van den Mooter, Guy

2016-06-06

Predensification and compression are unit operations imperative to the manufacture of tablets and capsules. Such stress-inducing steps can cause destabilization of solid dispersions which can alter their molecular arrangement and ultimately affect dissolution rate and bioavailability. In this study, itraconazole-Soluplus solid dispersions with 50% (w/w) drug loading prepared by hot-melt extrusion (HME) were investigated. Compression was performed at both pharmaceutically relevant and extreme compression pressures and dwell times. The starting materials, powder, and compressed solid dispersions were analyzed using modulated differential scanning calorimetry (MDSC), X-ray diffraction (XRD), small- and wide-angle X-ray scattering (SWAXS), attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR), and broadband dielectric spectroscopy (BDS). MDSC analysis revealed that compression promotes phase separation of solid dispersions as indicated by an increase in glass transition width, occurrence of a peak in the nonreversing heat flow signal, and an increase in the net heat of fusion indicating crystallinity in the systems. SWAXS analysis ruled out the presence of mesophases. BDS measurements elucidated an increase in the Soluplus-rich regions of the solid dispersion upon compression. FTIR indicated changes in the spatiotemporal architecture of the solid dispersions mediated via disruption in hydrogen bonding and ultimately altered dynamics. These changes can have significant consequences on the final stability and performance of the solid dispersions.

Dissolution-modulating mechanism of pH modifiers in solid dispersion containing weakly acidic or basic drugs with poor water solubility.

PubMed

Tran, Phuong Ha-Lien; Tran, Thao Truong-Dinh; Lee, Kyoung-Ho; Kim, Dong-Jin; Lee, Beom-Jin

2010-05-01

Although the solid dispersion method has been known to increase the dissolution rate of poorly water-soluble drugs by dispersing them in hydrophilic carriers, one obstacle of the solid dispersion method is its limited solubilization capacity, especially for pH-dependent soluble drugs. pH-modified solid dispersion, in which pH modifiers are incorporated, may be a useful method for increasing the dissolution rate of weakly acidic or basic drugs. Sufficient research, including the most recent reports, was undertaken in this review. How could the inclusion of the pH the pH modifiers in the solid dispersion system change drug structural behaviors, molecular interactions, microenvironmental pH, and/or release rate of pH modifiers, relating with the enhanced dissolution of weakly acidic or weakly basic drugs with poor water solubility? These questions have been investigated to determine the dissolution-modulating mechanism of pH modifiers in solid dispersion containing weakly acidic or basic drugs. It is believed that step-by-step mechanistic approaches could provide the ultimate solution for solubilizing several poorly water-soluble drugs with pH-dependent solubility from a solid dispersion system, as well as provide ideas for developing future dosage systems.

Solution behavior of PVP-VA and HPMC-AS-based amorphous solid dispersions and their bioavailability implications.

PubMed

Qian, Feng; Wang, Jennifer; Hartley, Ruiling; Tao, Jing; Haddadin, Raja; Mathias, Neil; Hussain, Munir

2012-10-01

To identify the mechanism behind the unexpected bio-performance of two amorphous solid dispersions: BMS-A/PVP-VA and BMS-A/HPMC-AS. Solubility of crystalline BMS-A in PVP-VA and HPMC-AS was measured by DSC. Drug-polymer interaction parameters were obtained by Flory-Huggins model fitting. Drug dissolution kinetics of spray-dried dispersions were studied under sink and non-sink conditions. BMS-A supersaturation was studied in the presence of pre-dissolved PVP-VA and HPMC-AS. Potency and crystallinity of undissolved solid dispersions were determined by HPLC and DSC. Polymer dissolution kinetics were obtained by mass balance calculation. Bioavailability of solid dispersions was assessed in dogs. In solid state, both polymers are miscible with BMS-A, while PVP-VA solublizes the drug better. BMS-A dissolves similarly from both solid dispersions in vitro regardless of dissolution method, while the HPMC-AS dispersion performed much better in vivo. At the same concentration, HPMC-AS is more effective in prolonging BMS-A supersaturation; this effect was negated by the slow dissolution rate of HPMC-AS. Further study revealed that fast PVP-VA dissolution resulted in elevated drug loading in undissolved dispersions and facilitated drug recrystallization before complete release. In contrast, the hydrophobicity and slower HPMC-AS dissolution prevented BMS-A recrystallization within the HPMC-AS matrix for >24 h. The lower bioavailability of PVP-VA dispersion was attributed to BMS-A recrystallization within the undissolved dispersion, due to hydrophilicity and fast PVP-VA dissolution rate. Polymer selection for solid dispersion development has significant impact on in vivo performance besides physical stability.

High wettability of liquid caesium iodine with solid uranium dioxide.

PubMed

Kurosaki, Ken; Suzuki, Masanori; Uno, Masayoshi; Ishii, Hiroto; Kumagai, Masaya; Anada, Keito; Murakami, Yukihiro; Ohishi, Yuji; Muta, Hiroaki; Tanaka, Toshihiro; Yamanaka, Shinsuke

2017-09-13

In March 2011, the Fukushima Daiichi Nuclear Power Plant accident caused nuclear fuel to melt and the release of high-volatility fission products into the environment. Caesium and iodine caused environmental contamination and public exposure. Certain fission-product behaviours remain unclear. We found experimentally that liquid CsI disperses extremely favourably toward solid UO 2 , exhibiting a contact angle approaching zero. We further observed the presence of CsI several tens of micrometres below the surface of the solid UO 2 sample, which would be caused by the infiltration of pores network by liquid CsI. Thus, volatile fission products released from molten nuclear fuels with complex internal composition and external structure migrate or evaporate to varying extents, depending on the nature of the solid-liquid interface and the fuel material surface, which becomes the pathway for the released fission products. Introducing the concept of the wettability of liquid chemical species of fission products in contact with solid fuels enabled developing accurate behavioural assessments of volatile fission products released by nuclear fuel.

Further insight into the mechanism of heavy metals partitioning in stormwater runoff.

PubMed

Djukić, Aleksandar; Lekić, Branislava; Rajaković-Ognjanović, Vladana; Veljović, Djordje; Vulić, Tatjana; Djolić, Maja; Naunovic, Zorana; Despotović, Jovan; Prodanović, Dušan

2016-03-01

Various particles and materials, including pollutants, deposited on urban surfaces are washed off by stormwater runoff during rain events. The interactions between the solid and dissolved compounds in stormwater runoff are phenomena of importance for the selection and improvement of optimal stormwater management practices aimed at minimizing pollutant input to receiving waters. The objective of this research was to further investigate the mechanisms responsible for the partitioning of heavy metals (HM) between the solid and liquid phases in urban stormwater runoff. The research involved the collection of samples from urban asphalt surfaces, chemical characterization of the bulk liquid samples, solids separation, particle size distribution fractionation and chemical and physico-chemical characterization of the solid phase particles. The results revealed that a negligible fraction of HM was present in the liquid phase (less than 3% by weight), while there was a strong correlation between the total content of heavy metals and total suspended solids. Examinations of surface morphology and mineralogy revealed that the solid phase particles consist predominantly of natural macroporous materials: alpha quartz (80%), magnetite (11.4%) and silicon diphosphate (8.9%). These materials have a low surface area and do not have significant adsorptive capacity. These materials have a low surface area and do not have significant adsorptive capacity. The presence of HM on the surface of solid particles was not confirmed by scanning electron microscopy and energy dispersive X-ray microanalyses. These findings, along with the results of the liquid phase sample characterization, indicate that the partitioning of HM between the liquid and solid phases in the analyzed samples may be attributed to precipitation processes. Copyright © 2015 Elsevier Ltd. All rights reserved.

Development of solid dispersion systems of dapivirine to enhance its solubility.

PubMed

Gorajana, Adinarayana; Ying, Chan Chiew; Shuang, Yeen; Fong, Pooi; Tan, Zhi; Gupta, Jyoti; Talekar, Meghna; Sharma, Manisha; Garg, Sanjay

2013-06-01

Dapivirine, formerly known as TMC 120, is a poorly-water soluble anti-HIV drug, currently being developed as a vaginal microbicide. The clinical use of this drug has been limited due to its poor solubility. The aim of this study was to design solid dispersion systems of Dapivirine to improve its solubility. Solid dispersions were prepared by solvent and fusion methods. Dapivirine release from the solid dispersion system was determined by conducting in-vitro dissolution studies. The physicochemical characteristics of the drug and its formulation were studied using Differential Scanning Calorimetry (DSC), powder X-ray Diffraction (XRD), Fourier-transform Infrared Spectroscopy (FTIR) and Scanning Electron Microscopy (SEM). A significant improvement in drug dissolution rate was observed with the solid dispersion systems. XRD, SEM and DSC results indicated the transformation of pure Dapivirine which exists in crystalline form into an amorphous form in selected solid dispersion formulations. FTIR and HPLC analysis confirmed the absence of drug-excipient interactions. Solid dispersion systems can be used to improve the dissolution rate of Dapivirine. This improvement could be attributed to the reduction or absence of drug crystallinity, existence of drug particles in an amorphous form and improved wettability of the drug.

Method of Manufacturing Micro-Disperse Particles of Sodium Borohydride

DOEpatents

Kravitz, Stanley H.; Hecht, Andrew M.; Sylwester. Alan P.; Bell, Nelson S.

2008-09-23

A compact solid source of hydrogen gas, where the gas is generated by contacting water with micro-disperse particles of sodium borohydride in the presence of a catalyst, such as cobalt or ruthenium. The micro-disperse particles can have a substantially uniform diameter of 1-10 microns, and preferably about 3-5 microns. Ruthenium or cobalt catalytic nanoparticles can be incorporated in the micro-disperse particles of sodium borohydride, which allows a rapid and complete reaction to occur without the problems associated with caking and scaling of the surface by the reactant product sodium metaborate. A closed loop water management system can be used to recycle wastewater from a PEM fuel cell to supply water for reacting with the micro-disperse particles of sodium borohydride in a compact hydrogen gas generator. Capillary forces can wick water from a water reservoir into a packed bed of micro-disperse fuel particles, eliminating the need for using an active pump.

Solid rocket exhaust in the stratosphere: Plume diffusion and chemical reactions

DOE Office of Scientific and Technical Information (OSTI.GOV)

Denison, M.R.; Lamb, J.J.; Bjorndahl, W.D.

1994-05-01

A model has been developed to examine, on a local scale, the reactions of rocket exhaust from solid rocket motors with stratospheric ozone. The effects were examined at two different altitudes. Results of the modeling study indicate that afterburning chemistry of reactive exhaust products can cause local but transient (on the order of several minutes) loss of ozone. The modeling study included potential heterogeneous reactions at aluminum oxide surfaces. Results indicate that these potential heterogeneous reactions do not have a major impact on the local plume chemistry. Homogeneous reactions appear to be of more consequence during the early dispersion ofmore » the plume. It has also been found that the rate of plume dispersion has a very significant effect on local ozone loss.« less

A solid state actuator based on polypyrrole (PPy) and a solid electrolyte NBR working in air

NASA Astrophysics Data System (ADS)

Cho, Misuk; Nam, Jaedo; Choi, Hyouk Ryeol; Koo, Jachoon; Lee, Youngkwan

2005-05-01

The solid polymer electrolyte based conducting polymer actuator was presented. In the preparation of acutuator module, an ionic liquid impregnated a synthetic rubber (NBR) and PPy were used as a solid polymer electrolyte and conducting polymer, respectively. An ionic liquid, 1-butyl-3-methylimidazolium bis (trifluoromethyl sulfonyl)imide (BMITFSI) is gradually dispersed into the NBR film and the conducting polymer, PPy was synthesized on the surface of NBR. The ionic conductivity of new type solid polymer electrolyte as a function of the immersion time was investigated. The cyclic voltammetry responsed and the redox switching dynamics of PEDOT in NBR matrix were studied. The displacement of the actuator was measured by laser beam.

Perspectives on Strategies Using Swellable Polymers in Solid Dispersions for Controlled Drug Release.

PubMed

Tran, Thao T D; Tran, Phuong H L

2017-01-01

Poorly water-soluble drugs, which commonly face the issue of poor absorption and low bioavailability, have been under ongoing research of many formulation scientists for the past few decades. Solid dispersion is one of the most effective strategies in concerns for improving bioavailability of poorly water-soluble drugs. Either application of solid dispersions in dissolution enhancement of poorly water-soluble drugs or the use of swellable polymers in controlled drug release has been reported in pharmaceutical designs widely. However, a review of strategies of using swellable polymers in solid dispersion to take a full advantage of these polymers as a current perspective in facilitating drug bioavailability enhancement is still missing. In this review, we aim to provide a summary of techniques used to formulate a swellable polymer in solid dispersion especially a description of a suitable fabrication method in design of a controlled release solid dispersion. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

Magnetic dispersive solid-phase extraction based on graphene oxide/Fe3 O4 @polythionine nanocomposite followed by atomic absorption spectrometry for zinc monitoring in water, flour, celery and egg.

PubMed

Babaei, Azar; Zeeb, Mohsen; Es-Haghi, Ali

2018-07-01

Magnetic graphene oxide nanocomposite has been proposed as a promising and sustainable sorbent for the extraction and separation of target analytes from food matrices. Sample preparation based on nanocomposite presents several advantages, such as desired efficiency, reasonable selectivity and high surface-area-to-volume ratio. A new graphene oxide/Fe 3 O 4 @polythionine (GO/Fe 3 O 4 @PTh) nanocomposite sorbent was introduced for magnetic dispersive solid-phase extraction and flame atomic absorption spectrometric detection of zinc(II) in water, flour, celery and egg. To fabricate the sorbent, an oxidative polymerization of thionine on the surface of magnetic GO was applied, while polythionine was simply employed as a surface modifier to improve extraction yield. The properties of the sorbent were characterized by transmission electron microscopy, scanning electron microscopy, X-ray diffraction, energy-dispersive X-ray analysis, vibrating sample magnetometry and Fourier transform-infrared spectroscopy. The calibration curve showed linearity in the range of 0.5-30 ng mL -1 . Limits of detection (S/N = 3) and quantification (S/N = 10) were 0.08 and 0.5 ng mL -1 , respectively. The method was applied for trace-level determination of Zn(II) in water and food samples, and its validation was investigated by recovery experiments and analyzing certified reference material. © 2018 Society of Chemical Industry. © 2018 Society of Chemical Industry.

Advanced surface chemical analysis of continuously manufactured drug loaded composite pellets.

PubMed

Hossain, Akter; Nandi, Uttom; Fule, Ritesh; Nokhodchi, Ali; Maniruzzaman, Mohammed

2017-04-15

The aim of the present study was to develop and characterise polymeric composite pellets by means of continuous melt extrusion techniques. Powder blends of a steroid hormone (SH) as a model drug and either ethyl cellulose (EC N10 and EC P7 grades) or hydroxypropyl methylcellulose (HPMC AS grade) as polymeric carrier were extruded using a Pharma 11mm twin screw extruder in a continuous mode of operation to manufacture extruded composite pellets of 1mm length. Molecular modelling study using commercial Gaussian 09 software outlined a possible drug-polymer interaction in the molecular level to develop solid dispersions of the drug in the pellets. Solid-state analysis conducted via a differential scanning calorimetry (DSC), hot stage microscopy (HSM) and X-ray powder diffraction (XRPD) analyses revealed the amorphous state of the drug in the polymer matrices. Surface analysis using SEM/energy dispersive X-ray (EDX) of the produced pellets arguably showed a homogenous distribution of the C and O atoms in the pellet matrices. Moreover, advanced chemical surface analysis conducted via atomic force microscopy (AFM) showed a homogenous phase system having the drug molecule dispersed onto the amorphous matrices while Raman mapping confirmed the homogenous single-phase drug distribution in the manufactured composite pellets. Such composite pellets are expected to deliver multidisciplinary applications in drug delivery and medical sciences by e.g. modifying drug solubility/dissolutions or stabilizing the unstable drug (e.g. hormone, protein) in the composite network. Copyright © 2016. Published by Elsevier Inc.

Preparation and evaluation of solid dispersion of atorvastatin calcium with Soluplus® by spray drying technique.

PubMed

Ha, Eun-Sol; Baek, In-hwan; Cho, Wonkyung; Hwang, Sung-Joo; Kim, Min-Soo

2014-01-01

The aim of the present study was to investigate the effect of Soluplus® on the solubility of atorvastatin calcium and to develop a solid dispersion formulation that can improve the oral bioavailability of atorvastatin calcium. We demonstrated that Soluplus® increases the aqueous solubility of atorvastatin calcium. Several solid dispersion formulations of atorvastatin calcium with Soluplus® were prepared at various drug : carrier ratios by spray drying. Physicochemical analysis demonstrated that atorvastatin calcium is amorphous in each solid dispersion, and the 2 : 8 drug : carrier ratio provided the highest degree of sustained atorvastatin supersaturation. Pharmacokinetic analysis in rats revealed that the 2 : 8 dispersion significantly improved the oral bioavailability of atorvastatin. This study demonstrates that spray-dried Soluplus® solid dispersions can be an effective method for achieving higher atorvastatin plasma levels.

Effects of polymer type and storage relative humidity on the kinetics of felodipine crystallization from amorphous solid dispersions.

PubMed

Rumondor, Alfred C F; Stanford, Lindsay A; Taylor, Lynne S

2009-12-01

The objective of this study was to investigate the effects of polymer type and storage relative humidity (RH) on the crystallization kinetics of felodipine from amorphous solid dispersions. Crystallization of the model drug felodipine from amorphous solid dispersion samples containing poly(vinyl pyrrolidone) (PVP) and hypromellose acetate succinate (HPMCAS) were evaluated. Samples at three different drug-polymer weight ratios (10, 25, and 50 wt. % polymer) were prepared and stored at six different RHs (0%, 32%, 52% or 66%, 75%, 86%, and 93%). Periodically, the fraction of the drug that had crystallized from the samples was quantified using powder X-ray diffractometry (PXRD). Felodipine crystallization rates from PVP-containing dispersions were found to be very sensitive to changes in storage RH, while crystallization rates from HPMCAS-containing dispersions were not. PVP and HPMCAS were similar in terms of their ability to inhibit crystallization at low RH, but when the storage RH was increased to 75% or above, felodipine crystallization from PVP-containing solid dispersions proceeded much faster. It is hypothesized that this trend was caused by moisture-induced drug-polymer immiscibility in PVP-felodipine system. For PVP-containing solid dispersion samples stored at 75% RH and above, crystallization of the model drug felodipine seemed to approach a kinetic plateau, whereby a fraction of the drug still remained amorphous even after storage for 500 days or more. The physical stability of solid dispersions as a function of RH is highly dependent on the polymer used to form the solid dispersion, with PVP-containing dispersions being much less physically stable at high RH than HPMCAS-containing dispersions.

Technology of stable, prolonged-release eye-drops containing Cyclosporine A, distributed between lipid matrix and surface of the solid lipid microspheres (SLM).

PubMed

Wolska, Eliza; Sznitowska, Małgorzata

2013-01-30

The aim of this study was to prepare solid lipid microspheres (SLM) with incorporated Cyclosporine A (Cs), suitable for ocular application. For this purpose, SLM were formulated by using different lipids and three different nonionic surfactants. The SLM were produced using a hot emulsification method. The SLM dispersions contained 10, 20 or 30% of lipid (w/w) and up to 2% (w/w) of Cs. The size of the microspheres with Cs ranged from 1 to 15 μm. Physically stable SLM with Cs were prepared using Compritol, as a lipid matrix, and Tween 80, as a surfactant. In contrast, dispersion with Precirol alone, formed semi-solid gels during storage, while in formulations with Precirol and Miglyol, crystals of Cs were observed. In vitro release profile of Compritol formulations showed that 40% of Cs is released within 1h, while the release of the following 40% takes more time, depending on lipid content in the formulations. The large part of Cs, added to SLM formulations (from 45 to 80%), was found on the surface of microparticles, but no drug crystallization occurred during a long-term storage. Copyright © 2012 Elsevier B.V. All rights reserved.

Polymeric Amorphous Solid Dispersions: A Review of Amorphization, Crystallization, Stabilization, Solid-State Characterization, and Aqueous Solubilization of Biopharmaceutical Classification System Class II Drugs.

PubMed

Baghel, Shrawan; Cathcart, Helen; O'Reilly, Niall J

2016-09-01

Poor water solubility of many drugs has emerged as one of the major challenges in the pharmaceutical world. Polymer-based amorphous solid dispersions have been considered as the major advancement in overcoming limited aqueous solubility and oral absorption issues. The principle drawback of this approach is that they can lack necessary stability and revert to the crystalline form on storage. Significant upfront development is, therefore, required to generate stable amorphous formulations. A thorough understanding of the processes occurring at a molecular level is imperative for the rational design of amorphous solid dispersion products. This review attempts to address the critical molecular and thermodynamic aspects governing the physicochemical properties of such systems. A brief introduction to Biopharmaceutical Classification System, solid dispersions, glass transition, and solubility advantage of amorphous drugs is provided. The objective of this review is to weigh the current understanding of solid dispersion chemistry and to critically review the theoretical, technical, and molecular aspects of solid dispersions (amorphization and crystallization) and potential advantage of polymers (stabilization and solubilization) as inert, hydrophilic, pharmaceutical carrier matrices. In addition, different preformulation tools for the rational selection of polymers, state-of-the-art techniques for preparation and characterization of polymeric amorphous solid dispersions, and drug supersaturation in gastric media are also discussed. Copyright © 2016 American Pharmacists Association®. Published by Elsevier Inc. All rights reserved.

Classification of solid dispersions: correlation to (i) stability and solubility (ii) preparation and characterization techniques.

PubMed

Meng, Fan; Gala, Urvi; Chauhan, Harsh

2015-01-01

Solid dispersion has been a topic of interest in recent years for its potential in improving oral bioavailability, especially for poorly water soluble drugs where dissolution could be the rate-limiting step of oral absorption. Understanding the physical state of the drug and polymers in solid dispersions is essential as it influences both the stability and solubility of these systems. This review emphasizes on the classification of solid dispersions based on the physical states of drug and polymer. Based on this classification, stability aspects such as crystallization tendency, glass transition temperature (Tg), drug polymer miscibility, molecular mobility, etc. and solubility aspects have been discussed. In addition, preparation and characterization methods for binary solid dispersions based on the classification have also been discussed.

Corroboration of naringin effects on the intestinal absorption and pharmacokinetic behavior of candesartan cilexetil solid dispersions using in-situ rat models.

PubMed

Surampalli, Gurunath; K Nanjwade, Basavaraj; Patil, P A

2015-01-01

The aim of this study was to corroborate the effects of naringin, a P-glycoprotein inhibitor, on the intestinal absorption and pharmacokinetics of candesartan (CDS) from candesartan cilexetil (CAN) solid dispersions using in-situ rat models. Intestinal transport and absorption studies were examined by in-situ single pass perfusion and closed-loop models. We evaluated the intestinal membrane damage in the presence of naringin by measuring the release of protein and alkaline phosphatase (ALP). We noticed 1.47-fold increase in Peff of CDS from freeze-dried CAN-loaded solid dispersions with naringin (15 mg/kg, w/w) when compared with freeze-dried solid dispersion without naringin using in-situ single pass intestinal perfusion model. However, no intestinal membrane damage was observed in the presence of naringin. Our findings from in-situ closed-loop pharmacokinetic studies showed 1.34-fold increase in AUC with elevated Cmax and shortened tmax for freeze-dried solid dispersion with naringin as compared to freeze-dried solid dispersion without naringin. This study demonstrated that increased solubilization (favored by freeze-dried solid dispersion) and efflux pump inhibition (using naringin), the relative bioavailability of CDS can be increased, suggesting an alternative potential for improving oral bioavailability of CAN.

Criteria for the selection of a solid phase to be used in immunoassays.

PubMed

Delagneau, J F; Masseyeff, R

1990-01-01

Heterogeneous immunoassays are very sensitive and only limited in terms of performance by non specific binding. They require separation of free from bound fractions and concomitant use of a solid phase coated with an immunoreactive component (i.e. immunosorbent). The improvement of these key immunosorbents is crucial and involves a great deal of expertise and capabilities. Specifications differ according to procedure (e.g. capture or competitive assay). Each routinely used solid phase, such as polystyrene wells, porous membrane or dispersible microbeads, presents specific performance characteristics, advantages, and drawbacks. Among the tasks to be implemented are optimization of the spatial orientation of immunological reagents, selection of the surface neutral hydrophilic support, acceleration of reactions by increasing the reactive surface area of the supports, streamlining and simplification of procedural steps. These various aspects are abundantly described and emphasized here.

Amorphous stabilization and dissolution enhancement of amorphous ternary solid dispersions: combination of polymers showing drug-polymer interaction for synergistic effects.

PubMed

Prasad, Dev; Chauhan, Harsh; Atef, Eman

2014-11-01

The purpose of this study was to understand the combined effect of two polymers showing drug-polymer interactions on amorphous stabilization and dissolution enhancement of indomethacin (IND) in amorphous ternary solid dispersions. The mechanism responsible for the enhanced stability and dissolution of IND in amorphous ternary systems was studied by exploring the miscibility and intermolecular interactions between IND and polymers through thermal and spectroscopic analysis. Eudragit E100 and PVP K90 at low concentrations (2.5%-40%, w/w) were used to prepare amorphous binary and ternary solid dispersions by solvent evaporation. Stability results showed that amorphous ternary solid dispersions have better stability compared with amorphous binary solid dispersions. The dissolution of IND from the ternary dispersion was substantially higher than the binary dispersions as well as amorphous drug. Melting point depression of physical mixtures reveals that the drug was miscible in both the polymers; however, greater miscibility was observed in ternary physical mixtures. The IR analysis confirmed intermolecular interactions between IND and individual polymers. These interactions were found to be intact in ternary systems. These results suggest that the combination of two polymers showing drug-polymer interaction offers synergistic enhancement in amorphous stability and dissolution in ternary solid dispersions. © 2014 Wiley Periodicals, Inc. and the American Pharmacists Association.

Preparation and Evaluation of Solid Dispersion Tablets by a Simple and Manufacturable Wet Granulation Method Using Porous Calcium Silicate.

PubMed

Fujimoto, Yumi; Hirai, Nobuaki; Takatani-Nakase, Tomoka; Takahashi, Koichi

2016-01-01

The aim of this study was to prepare and evaluate solid dispersion tablets containing a poorly water-soluble drug using porous calcium silicate (PCS) by a wet granulation method. Nifedipine (NIF) was used as the model poorly water-soluble drug. Solid dispersion tablets were prepared with the wet granulation method using ethanol and water by a high-speed mixer granulator. The binder and disintegrant were selected from 7 and 4 candidates, respectively. The dissolution test was conducted using the JP 16 paddle method. The oral absorption of NIF was studied in fasted rats. Xylitol and crospovidone were selected as the binder and disintegrant, respectively. The dissolution rates of NIF from solid dispersion formulations were markedly enhanced compared with NIF powder and physical mixtures. Powder X-ray diffraction (PXRD) confirmed the reduced crystallinity of NIF in the solid dispersion formulations. Fourier transform infrared (FT-IR) showed the physical interaction between NIF and PCS in the solid dispersion formulations. NIF is present in an amorphous state in granules prepared by the wet granulation method using water. The area under the plasma concentration-time curve (AUC) and peak concentration (C(max)) values of NIF after dosing rats with the solid dispersion granules were significantly greater than those after dosing with NIF powder. The solid dispersion formulations of NIF prepared with PCS using the wet granulation method exhibited accelerated dissolution rates and superior oral bioavailability. This method is very simple, and may be applicable to the development of other poorly water-soluble drugs.

Stabilization of a supersaturated solution of mefenamic acid from a solid dispersion with EUDRAGIT(®) EPO.

PubMed

Kojima, Taro; Higashi, Kenjirou; Suzuki, Toyofumi; Tomono, Kazuo; Moribe, Kunikazu; Yamamoto, Keiji

2012-10-01

The stabilization mechanism of a supersaturated solution of mefenamic acid (MFA) from a solid dispersion with EUDRAGIT(®) EPO (EPO) was investigated. The solid dispersions were prepared by cryogenic grinding method. Powder X-ray diffractometry, in vitro dissolution test, in vivo oral absorption study, infrared spectroscopy, and solid- and solution-state NMR spectroscopies were used to characterize the solid dispersions. Dissolution tests in acetate buffer (pH 5.5) revealed that solid dispersion showed > 200-fold higher concentration of MFA. Supersaturated solution was stable over 1 month and exhibited improved oral bioavailability of MFA in rats, with a 7.8-fold higher area under the plasma concentration-versus-time curve. Solid-state (1)H spin-lattice relaxation time (T(1)) measurement showed that MFA was almost monomolecularly dispersed in the EPO polymer matrix. Intermolecular interaction between MFA and EPO was indicated by solid-state infrared and (13)C-T(1) measurements. Solution-state (1)H-NMR measurement demonstrated that MFA existed in monomolecular state in supersaturated solution. (1)H-T(1) and difference nuclear Overhauser effect measurements indicated that cross relaxation occurred between MFA and EPO due to the small distance between them. The formation and high stability of the supersaturated solution were attributable to the specifically formed intermolecular interactions between MFA and EPO.

Dispersoid reinforced alloy powder and method of making

DOEpatents

Anderson, Iver E [Ames, IA; Terpstra, Robert L [Ames, IA

2012-06-12

A method of making dispersion-strengthened alloy particles involves melting an alloy having a corrosion and/or oxidation resistance-imparting alloying element, a dispersoid-forming element, and a matrix metal wherein the dispersoid-forming element exhibits a greater tendency to react with a reactive species acquired from an atomizing gas than does the alloying element. The melted alloy is atomized with the atomizing gas including the reactive species to form atomized particles so that the reactive species is (a) dissolved in solid solution to a depth below the surface of atomized particles and/or (b) reacted with the dispersoid-forming element to form dispersoids in the atomized particles to a depth below the surface of said atomized particles. The atomized alloy particles are solidified as solidified alloy particles or as a solidified deposit of alloy particles. Bodies made from the dispersion strengthened alloy particles, deposit thereof, exhibit enhanced fatigue and creep resistance and reduced wear as well as enhanced corrosion and/or oxidation resistance at high temperatures by virtue of the presence of the corrosion and/or oxidation resistance imparting alloying element in solid solution in the particle alloy matrix.

Dispersoid reinforced alloy powder and method of making

DOEpatents

Anderson, Iver E.; Terpstra, Robert L.

2010-04-20

A method of making dispersion-strengthened alloy particles involves melting an alloy having a corrosion and/or oxidation resistance-imparting alloying element, a dispersoid-forming element, and a matrix metal wherein the dispersoid-forming element exhibits a greater tendency to react with a reactive species acquired from an atomizing gas than does the alloying element. The melted alloy is atomized with the atomizing gas including the reactive species to form atomized particles so that the reactive species is (a) dissolved in solid solution to a depth below the surface of atomized particles and/or (b) reacted with the dispersoid-forming element to form dispersoids in the atomized particles to a depth below the surface of said atomized particles. The atomized alloy particles are solidified as solidified alloy particles or as a solidified deposit of alloy particles. Bodies made from the dispersion strengthened alloy particles, deposit thereof, exhibit enhanced fatigue and creep resistance and reduced wear as well as enhanced corrosion and/or oxidation resistance at high temperatures by virtue of the presence of the corrosion and/or oxidation resistance imparting alloying element in solid solution in the particle alloy matrix.

Microparticles Containing Curcumin Solid Dispersion: Stability, Bioavailability and Anti-Inflammatory Activity.

PubMed

Teixeira, C C C; Mendonça, L M; Bergamaschi, M M; Queiroz, R H C; Souza, G E P; Antunes, L M G; Freitas, L A P

2016-04-01

This work aimed at improving the solubility of curcumin by the preparation of spray-dried ternary solid dispersions containing Gelucire®50/13-Aerosil® and quantifying the resulting in vivo oral bioavailability and anti-inflammatory activity. The solid dispersion containing 40% of curcumin was characterised by calorimetry, infrared spectroscopy and X-ray powder diffraction. The solubility and dissolution rate of curcumin in aqueous HCl or phosphate buffer improved up to 3600- and 7.3-fold, respectively. Accelerated stability test demonstrated that the solid dispersion was stable for 9 months. The pharmacokinetic study showed a 5.5-fold increase in curcumin in rat blood plasma when compared to unprocessed curcumin. The solid dispersion also provided enhanced anti-inflammatory activity in rat paw oedema. Finally, the solid dispersion proposed here is a promising way to enhance curcumin bioavailability at an industrial pharmaceutical perspective, since its preparation applies the spray drying, which is an easy to scale up technique. The findings herein stimulate further in vivo evaluations and clinical tests as a cancer and Alzheimer chemoprevention agent.

Solid dispersion tablets of breviscapine with polyvinylpyrrolidone K30 for improved dissolution and bioavailability to commercial breviscapine tablets in beagle dogs.

PubMed

Cong, Wenjuan; Shen, Lan; Xu, Desheng; Zhao, Lijie; Ruan, Kefeng; Feng, Yi

2014-09-01

Breviscapine, one of cardiovascular drugs extracted from a Chinese herb Erigeron breviscapinus, has been frequently used to treat cardiovascular diseases such as hypertension, angina pectoris, coronary heart disease and stroke. However, its poor water solubility and low bioavailability in vivo severely restrict the clinical application. To overcome these drawbacks, breviscapine solid dispersion tablets consisting of breviscapine, polyvinylpyrrolidone K30 (PVP K30), microcrystalline cellulose and crospovidone were appropriately prepared. In vitro dissolution profiles showed that breviscapine released percentage of solid dispersion tablets reached 90 %, whereas it was only 40 % for commercial breviscapine tablets. Comparative pharmacokinetic study between solid dispersion tablets and commercial products was investigated on the normal beagle dogs after oral administration. Results showed that the bioavailability of breviscapine was greatly increased by 3.45-fold for solid dispersion tablets. The greatly improved dissolution rate and bioavailability might be attributed to intermolecular hydrogen bonding reactions between PVP K30 and scutellarin. These findings suggest that our solid dispersion tablets can greatly improve the bioavailability as well as the dissolution rate of breviscapine.

Preparation, characterization and in vitro evaluation of solid dispersions containing docetaxel.

PubMed

Chen, Jie; Qiu, Liyan; Hu, Minxin; Jin, Yi; Han, Jieru

2008-06-01

Solid dispersions using water-soluble carriers were studied for improving the dissolution of docetaxel, a poorly soluble compound. In order to obtain the most optimized formulation, we prepared many solid dispersions with different carriers, different solvents, or at a series of drug-to-carrier ratios, and compared their dissolution. The accumulative dissolution of docetaxel from poloxamer 188 was more excellent than that from PVP(k30) and glyceryl monostearate, and the dissolution of docetaxel from solid dispersion was markedly higher than that of pure docetaxel; meanwhile the increased dissolution was partly dependent on the ratios of docetaxel and poloxamer 188. The ethanol used to prepare solid dispersion is of more significant effect on the dissolution of docetaxel than that of acetone. The docetaxel/poloxamer 188 system was characterized by differential scanning calorimetry (DSC), X-ray diffractometry (XRD), and environmental scanning electron microscope (ESEM). The results of DSC, XRD, and ESEM analyses of docetaxel/poloxamer 188 system showed that there are intermolecular interactions between docetaxel and poloxamer, and the crystallinity of docetaxel disappeared. These results show that solid dispersion is a promising approach of developing docetaxel drug formulates.

Fusion production of solid dispersions containing a heat-sensitive active ingredient by hot melt extrusion and Kinetisol dispersing.

PubMed

Dinunzio, James C; Brough, Chris; Hughey, Justin R; Miller, Dave A; Williams, Robert O; McGinity, James W

2010-02-01

Many techniques for the production of solid dispersions rely on elevated temperatures and prolonged material residence times, which can result in decomposition of temperature-sensitive components. In this study, hydrocortisone was used as a model temperature-sensitive active ingredient to study the effect of formulation and processing techniques as well as to characterize the benefits of KinetiSol Dispersing for the production of solid dispersions. Preformulation studies were conducted using differential scanning calorimetry and hot stage microscopy to identify optimum carriers for the production of amorphous solid dispersions. After identification, solid dispersions were prepared by hot melt extrusion and KinetiSol Dispersing, with material characterized by X-ray diffraction, dissolution and potency testing to evaluate physicochemical properties. Results from the preformulation studies showed that vinylacetate:vinylpyrrolidone (PVPVA) copolymer allowed for hydrocortisone dissolution within the carrier at temperatures as low as 160 degrees C, while hydroxypropyl methylcellulose required temperatures upward of 180 degrees C to facilitate solubilization. Low substituted hydroxypropyl cellulose, a high glass transition temperature control, showed that the material was unable to solubilize hydrocortisone. Manufacturing process control studies using hot melt extruded compositions of hydrocortisone and PVPVA showed that increased temperatures and residence times negatively impacted product potency due to decomposition. Using KinetiSol Dispersing to reduce residence time and to facilitate lower temperature processing, it was possible to produce solid dispersions with improved product potency. This study clearly demonstrated the importance of carrier selection to facilitate lower temperature processing, as well as the effect of residence time on product potency. Furthermore, KinetiSol Dispersing provided significant advantages over hot melt extrusion due to the reduced residence times and lower required processing temperatures. This allowed for the production of solid dispersions with enhanced product potency. Copyright (c) 2009 Elsevier B.V. All rights reserved.

Application of acoustic surface wave technology to shuttle radar

NASA Technical Reports Server (NTRS)

1975-01-01

The application of surface acoustic wave (SAW) signal processing devices in the space shuttle was explored. In order to demonstrate the functions which a SAW device might perform, a breadboard pulse compression filter (PCF) module was assembled. The PCF permits a pulse radar to operate with a large duty cycle and low peak power, a regime favorable to the use of solid state RF sources. The transducer design, strong coupling compensation, circuit model analysis, fabrication limitations, and performance evaluation of a PCF are described. The nominal value of the compression ratio is 100:1 with 10-MHz bandwidth centered at 60 MHz and 10-microsecond dispersive delay. The PCF incorporates dispersive interdigital transducers and a piezoelectric lithium niobate substrate.

Molecular mechanism of polymer-assisting supersaturation of poorly water-soluble loratadine based on experimental observations and molecular dynamic simulations.

PubMed

Zhang, Shenwu; Sun, Mengchi; Zhao, Yongshan; Song, Xuyang; He, Zhonggui; Wang, Jian; Sun, Jin

2017-10-01

Polymers have been usually used to retard nucleation and crystal growth in order to maintain supersaturation, yet their roles in inhibition of nucleation and crystal growth are poorly understood. In our work, the polymer-based supersaturation performances and molecular mechanisms of poorly aqueous soluble loratadine were investigated. Two common hydrophilic polymers (hydroxylpropylmethyl cellulose acetate succinate (HPMC-AS) and poly(vinylpyrrolidone-co-vinyl-acetate) (PVP-VA)) were used. It was found that HPMC-AS was a better polymer to prevent drug molecules from aggregation and to maintain the supersaturated state in solution than PVP-VA. The in vitro dissolution experiments showed that HPMC-AS solid dispersions had more rapid release at pH 4.5 and 6.8 media than PVP-VA solid dispersions under the un-sink condition. Moreover, molecular dynamic simulation results showed that HPMC-AS was more firmly absorbed onto a surface of the drug nanoparticles than PVP-VA due to bigger hydrophobic areas of HPMC-AS. Thereby, crystallization process of loratadine was inhibited in the presence of water to provide prolonged stability of the supersaturated state. In conclusion, polymers played a key role in maintaining supersaturation state of loratadine solid dispersions by strong drug-polymer interactions and the hydrophobic characteristic of polymers.

Core-shell Fe3O4 polydopamine nanoparticles as sorbent for magnetic dispersive solid-phase extraction of copper from food samples.

PubMed

Yavuz, Emre; Tokalıoğlu, Şerife; Patat, Şaban

2018-10-15

In the present study, core-shell Fe 3 O 4 polydopamine nanoparticles were synthesized and used for the first time as an adsorbent for the vortex assisted magnetic dispersive solid phase extraction of copper from food samples. After elution, copper in the solutions was determined by FAAS. The adsorbent was characterized using X-ray diffraction, scanning electron microscopy, energy dispersive X-ray spectroscopy, Fourier transform infrared spectroscopy, Brunauer-Emmett-Teller surface area, and zeta potential measurements. Various parameters affecting the magnetic dispersive solid-phase extraction were evaluated. The optimum pH and magnetic adsorbent amount were found to be 5 and 40 mg, respectively. Elution was made by 3 mL of 2 mol L -1 HNO 3 .The major advantage of the method is the fast equilibration during adsorption without the need for vortexing or shaking. The preconcentration factor and detection limit of the method were found to be 150 and 0.22 mg L -1 , respectively. The precision (as RSD%) and adsorption capacity of the method were 3.7% and 28 mg g -1 , respectively. The method was successfully verified by analyzing four certified reference materials (SPS-WW1 Batch 114 Wastewater, TMDA-53.3 Lake water, BCR-482 Lichen and 1573a Tomato Leaves) and by addition/recovery tests of copper standard solution in organic baby food, muesli, macaroni, honey, and milk samples. Copyright © 2018 Elsevier Ltd. All rights reserved.

The effect of lipophilicity of spin-labeled compounds on their distribution in solid lipid nanoparticle dispersions studied by electron paramagnetic resonance.

PubMed

Pegi, Ahlin; Julijana, Kristl; Slavko, Pecar; Janez, Strancar; Marjeta, Sentjurc

2003-01-01

Solid lipid nanoparticles (SLN) constitute an attractive drug carrier system. The aim of this study was to investigate the influence of lipophilicity and structure of different model molecules on their distribution in SLN dispersions. SLN composed of glyceryl tripalmitate as lipid and soybean lecithin and poloxamer 188 as stabilizers were prepared by a melt-emulsification process. PC(10,3), MeFASL(10,3), C(14)-Tempo, and Tempol were incorporated into SLN as spin-labeled compounds. The partition of SP between triglyceride and water was determined experimentally by electron paramagnetic resonance (EPR) and compared with calculated partition coefficients. The distribution of molecules in SLN dispersions was determined from the parameters of EPR spectra, from the reduction kinetics of the spin-labeled compounds with sodium ascorbate, and by computer simulation of EPR spectral line shapes. The experimentally obtained partition coefficients increase in the order Tempol < MeFASL(10,3) < C(14)-Tempo, showing the same trend as the partition coefficients calculated according to Rekker. In SLN dispersions, it was estimated that the ratio of SP between solid lipid core, phospholipid layers (deeper in SLN layer or in liposomes and closer to the surface of SLN), and water is for Tempol 0:0:100, for C(14)-Tempo 46:54(20:34):0, for MeFASL(10,3) 34:65(38:27):1, and for PC(10,3) 10:89(26:3:60):1. Copyright 2002 Wiley-Liss, Inc. and the American Pharmaceutical Association

Method of generating hydrogen gas from sodium borohydride

DOEpatents

Kravitz, Stanley H.; Hecht, Andrew M.; Sylwester, Alan P.; Bell, Nelson S.

2007-12-11

A compact solid source of hydrogen gas, where the gas is generated by contacting water with micro-disperse particles of sodium borohydride in the presence of a catalyst, such as cobalt or ruthenium. The micro-disperse particles can have a substantially uniform diameter of 1-10 microns, and preferably about 3-5 microns. Ruthenium or cobalt catalytic nanoparticles can be incorporated in the micro-disperse particles of sodium borohydride, which allows a rapid and complete reaction to occur without the problems associated with caking and scaling of the surface by the reactant product sodium metaborate. A closed loop water management system can be used to recycle wastewater from a PEM fuel cell to supply water for reacting with the micro-disperse particles of sodium borohydride in a compact hydrogen gas generator. Capillary forces can wick water from a water reservoir into a packed bed of micro-disperse fuel particles, eliminating the need for using an active pump.

PEG-stabilized core-shell surface-imprinted nanoparticles.

PubMed

Moczko, Ewa; Guerreiro, Antonio; Piletska, Elena; Piletsky, Sergey

2013-08-06

Here we present a simple technique to produce target-specific molecularly imprinted polymeric nanoparticles (MIP NPs) and their surface modification in order to prevent the aggregation process that is ever-present in most nanomaterial suspensions/dispersions. Specifically, we studied the influence of surface modification of MIP NPs with polymerizable poly(ethylene glycol) on their degree of stability in water, in phosphate buffer, and in the presence of serum proteins. Grafting a polymer shell on the surface of nanoparticles decreases the surface energy, enhances the polarity, and as a result improves the dispersibility, storage, and colloidal stability as compared to those of core (unmodified) particles. Because of the unique solid-phase approach used for synthesis, the binding sites of MIP NPs are protected during grafting, and the recognition properties of nanoparticles are not affected. These results are significant for developing nanomaterials with selective molecular recognition, increased biocompatibility, and stability in solution. Materials synthesized this way have the potential to be used in a variety of technological fields, including in vivo applications such as drug delivery and imaging.

Electrode assembly for use in a solid polymer electrolyte fuel cell

DOEpatents

Raistrick, Ian D.

1989-01-01

A gas reaction fuel cell may be provided with a solid polymer electrolyte membrane. Porous gas diffusion electrodes are formed of carbon particles supporting a catalyst which is effective to enhance the gas reactions. The carbon particles define interstitial spaces exposing the catalyst on a large surface area of the carbon particles. A proton conducting material, such as a perfluorocarbon copolymer or ruthenium dioxide contacts the surface areas of the carbon particles adjacent the interstitial spaces. The proton conducting material enables protons produced by the gas reactions adjacent the supported catalyst to have a conductive path with the electrolyte membrane. The carbon particles provide a conductive path for electrons. A suitable electrode may be formed by dispersing a solution containing a proton conducting material over the surface of the electrode in a manner effective to coat carbon surfaces adjacent the interstitial spaces without impeding gas flow into the interstitial spaces.

The utilization of drug-polymer interactions for improving the chemical stability of hot-melt extruded solid dispersions.

PubMed

Guo, Zhefei; Lu, Ming; Li, Yongcheng; Pang, Huishi; Lin, Ling; Liu, Xu; Wu, Chuanbin

2014-02-01

Interactions between drugs and polymers were utilized to lower the processing temperature of hot-melt extrusion (HME), and thus minimize the thermal degradation of heat-sensitive drugs during preparation of amorphous solid dispersions. Diflunisal (DIF), which would degrade upon melting, was selected as a model drug. Hydrogen bonds between DIF and polymeric carriers (PVP K30, PVP VA64, hydroxypropyl methylcellulose and Soluplus) were revealed by differential scanning calorimetry and Fourier transform infrared spectroscopy. The hot-melt extruded solid dispersion was characterized by powder X-ray diffraction (XRD), scanning electron microscopy (SEM) and high-performance liquid chromatography (HPLC). The results of hot-stage polar microscopy indicated that DIF was dissolved in molten polymers at 160°C, much lower than the melting point of DIF (215°C). At this temperature, amorphous solid dispersions were successfully produced by HME, as confirmed by XRD and SEM. The related impurities in amorphous solid dispersions detected by HPLC were lower than 0.3%, indicating that thermal degradation was effectively minimized. The dissolution of DIF from amorphous solid dispersions was significantly enhanced as compared with the pure crystalline drug. This technique based on drug-polymer interactions to prepare chemically stable amorphous solid dispersions by HME provides an attractive opportunity for development of heat-sensitive drugs. © 2013 Royal Pharmaceutical Society.

Communication: A combined periodic density functional and incremental wave-function-based approach for the dispersion-accounting time-resolved dynamics of ⁴He nanodroplets on surfaces: ⁴He/graphene.

PubMed

de Lara-Castells, María Pilar; Stoll, Hermann; Civalleri, Bartolomeo; Causà, Mauro; Voloshina, Elena; Mitrushchenkov, Alexander O; Pi, Martí

2014-10-21

In this work we propose a general strategy to calculate accurate He-surface interaction potentials. It extends the dispersionless density functional approach recently developed by Pernal et al. [Phys. Rev. Lett. 103, 263201 (2009)] to adsorbate-surface interactions by including periodic boundary conditions. We also introduce a scheme to parametrize the dispersion interaction by calculating two- and three-body dispersion terms at coupled cluster singles and doubles and perturbative triples (CCSD(T)) level via the method of increments [H. Stoll, J. Chem. Phys. 97, 8449 (1992)]. The performance of the composite approach is tested on (4)He/graphene by determining the energies of the low-lying selective adsorption states, finding an excellent agreement with the best available theoretical data. Second, the capability of the approach to describe dispersionless correlation effects realistically is used to extract dispersion effects in time-dependent density functional simulations on the collision of (4)He droplets with a single graphene sheet. It is found that dispersion effects play a key role in the fast spreading of the (4)He nanodroplet, the evaporation-like process of helium atoms, and the formation of solid-like helium structures. These characteristics are expected to be quite general and highly relevant to explain experimental measurements with the newly developed helium droplet mediated deposition technique.

Synergistic role of solid lipid and porous silica in improving the oral delivery of weakly basic poorly water soluble drugs.

PubMed

Yasmin, Rokhsana; Rao, Shasha; Bremmell, Kristen; Prestidge, Clive

2017-01-01

Oral absorption of weakly basic drugs (e.g. cinnarizine (CIN)) is limited by their pH dependent precipitation in intestinal conditions. To overcome this challenge, a novel drug delivery system composed of solid lipid and porous silica, namely silica encapsulated solid lipid (SESL) particles, was developed via hot homogenization of melted lipid dispersion, followed by ultra-sonication of the silica stabilized homogenized melted lipid dispersion. Scanning electron microscope (SEM) images of the SESL formulation revealed non-spherical and aggregated hybrid particles, with rough exterior and structured nanoparticles visible on the surface. A 1.5, 2.2 and 7-fold improvement in the dissolution of CIN was observed for the SESL particles, under simulated intestinal non-digesting conditions, in comparison to the drug loaded in solid lipid (CIN-SL) matrix, drug loaded in porous silica (CIN-PS) and pure drug powder. Under simulated intestinal digestive condition, significant improvement in the drug solubilization was reported for the SESL formulation in compared to the individual drug loaded systems i.e. CIN-PS and CIN-SL. Thereby, silica encapsulated solid lipid system provides a promising oral delivery approach for poorly water soluble weakly basic drugs. Copyright © 2016 Elsevier B.V. All rights reserved.

Use of surfactants as plasticizers in preparing solid dispersions of poorly soluble API: stability testing of selected solid dispersions.

PubMed

Ghebremeskel, Alazar N; Vemavarapu, Chandra; Lodaya, Mayur

2006-08-01

The purpose of the study is to evaluate the effect of surfactant-plasticizers on the physical stability of amorphous drug in polymer matrices formed by hot melt extrusion. Solid dispersions of a poorly soluble drug were prepared using PVP-K30, Plasdone-S630, and HPMC-E5 as the polymeric carriers and surfactants as plasticizers. The solid dispersions were produced by hot melt extrusion at temperatures 10 degrees C above and below the glass transition temperature (Tg) of the carrier polymers using a 16 mm-Haake Extruder. The surfactants tested in this study included Tween-80 and Docusate Sodium. The particle size of the extrudate was reduced to have mean of 100-200 micron. The physical stability of the solid dispersions produced was monitored at 30 degrees C/60% for six-months and at 60 degrees C/85% for two-months in open HDPE bottles. Modulated differential scanning calorimetry, polarized light microscopy, powder X-ray diffraction and dissolution testing was performed to assess the physical stability of solid dispersions upon stress testing. The dispersions containing HPMC-E5 were observed especially to be susceptible to physical instability under an accelerated stress conditions (60 degrees C/85%RH) of the solid dispersion. About 6% conversion of amorphous drug to crystalline form was observed. Consequently, the system exhibits similar degree of re-crystallization upon addition of the surfactant. However, under 30 degrees C/60%RH condition, the otherwise amorphous Drug-HPMC-E5 system has been destabilized by the addition of the surfactant. This effect is much more reduced in the extruded solid dispersions where polymeric carriers such as Plasdone S-603 and PVP-K30 (in addition to surfactants) are present. Furthermore, the drug release from the solid dispersions was unaffected at the stress conditions reported above. Possible reasons for the enhanced stability of the dispersions are due to the surfactants ability to lower the viscosity of the melt, increase the API solubility and homogeneity in the carrier polymer. In contrast, while it is possible for the surfactants to destabilize the system by lowering the Tg and increasing the water uptake, the study confirms that this effect is minimal. By and large, the surfactants appear to be promising plasticizers to produce solid dispersions by hot melt extrusion, in so doing improving dissolution rate without compromising the physical stability of the systems.

Characterization, in Vivo and in Vitro Evaluation of Solid Dispersion of Curcumin Containing d-α-Tocopheryl Polyethylene Glycol 1000 Succinate and Mannitol.

PubMed

Song, Im-Sook; Cha, Jin-Sun; Choi, Min-Koo

2016-10-17

The aim of this study was to prepare a solid dispersion formulation of curcumin to enhance its solubility, dissolution rate, and oral bioavailability. The formulation was prepared with d-α-tocopheryl polyethylene glycol 1000 succinate (TPGS) and mannitol using solvent evaporation and freeze-drying methods, which yielded a solid dispersion composed of curcumin, TPGS, and mannitol at a ratio of 1:10:15 ( w / w / w ). The solubility and dissolution rate of the curcumin solid dispersion markedly improved compared with those of curcumin powder and a physical mixture of curcumin, TPGS, and mannitol. About 90% of the curcumin was released from the solid dispersion formulation within 10 min. After administering the formulation orally to rats, higher plasma concentrations of curcumin were observed, with increases in the maximum plasma concentration (C max ) and area under the plasma concentration-time curve (AUC) of 86- and 65-fold, respectively, compared with those of curcumin powder. The solid dispersion formulation effectively increased intestinal permeability and inhibited P-gp function. These effects increased the anti-proliferative effect of curcumin in MDA-MB-231 breast cancer cells. Moreover, 2 h incubation with curcumin powder, solid dispersion formulation, and its physical mixture resulted in differential cytotoxic effect of paclitaxel in P-gp overexpressed LLC-PK1-P-gp and MDA-MB-231 cells through the inhibition of P-gp-mediated paclitaxel efflux. In conclusion, compared with curcumin, a solid dispersion formulation of curcumin with TPGS and mannitol could be a promising option for enhancing the oral bioavailability and efficacy of curcumin through increased solubility, dissolution rate, cell permeability, and P-gp modulation.

Current trends and future perspectives of solid dispersions containing poorly water-soluble drugs.

PubMed

Vo, Chau Le-Ngoc; Park, Chulhun; Lee, Beom-Jin

2013-11-01

Over 40% of active pharmaceutical ingredients (API) in development pipelines are poorly water-soluble drugs which limit formulation approaches, clinical application and marketability because of their low dissolution and bioavailability. Solid dispersion has been considered one of the major advancements in overcoming these issues with several successfully marketed products. A number of key references that describe state-of-the-art technologies have been collected in this review, which addresses various pharmaceutical strategies and future visions for the solubilization of poorly water-soluble drugs according to the four generations of solid dispersions. This article reviews critical aspects and recent advances in formulation, preparation and characterization of solid dispersions as well as in-depth pharmaceutical solutions to overcome some problems and issues that limit the development and marketability of solid dispersion products. Copyright © 2013 Elsevier B.V. All rights reserved.

Investigation of process temperature and screw speed on properties of a pharmaceutical solid dispersion using corotating and counter-rotating twin-screw extruders.

PubMed

Keen, Justin M; Martin, Charlie; Machado, Augie; Sandhu, Harpreet; McGinity, James W; DiNunzio, James C

2014-02-01

The use of corotating twin screw hot-melt extruders to prepare amorphous drug/polymer systems has become commonplace. As small molecule drug candidates exiting discovery pipelines trend towards higher MW and become more structurally complicated, the acceptable operating space shifts below the drug melting point. The objective of this research is to investigate the extrusion process space, which should be selected to ensure that the drug is solubilized in the polymer with minimal thermal exposure, is critical in ensuring the performance, stability and purity of the solid dispersion. The properties of a model solid dispersion were investigated using both corotating and counter-rotating hot-melt twin-screw extruders operated at various temperatures and screw speeds. The solid state and dissolution performance of the resulting solid dispersions was investigated and evaluated in context of thermodynamic predictions from Flory-Huggins Theory. In addition, the residence time distributions were measured using a tracer, modelled and characterized. The amorphous content in the resulting solid dispersions was dependent on the combination of screw speed, temperature and operating mode. The counter-rotating extruder was observed to form amorphous solid dispersions at a slightly lower temperature and with a narrower residence time distribution, which also exhibited a more desirable shape. © 2013 Royal Pharmaceutical Society.

Itraconazole solid dispersion prepared by a supercritical fluid technique: preparation, in vitro characterization, and bioavailability in beagle dogs.

PubMed

Yin, Xuezhi; Daintree, Linda Sharon; Ding, Sheng; Ledger, Daniel Mark; Wang, Bing; Zhao, Wenwen; Qi, Jianping; Wu, Wei; Han, Jiansheng

2015-01-01

This research aimed to develop a supercritical fluid (SCF) technique for preparing a particulate form of itraconazole (ITZ) with good dissolution and bioavailability characteristics. The ITZ particulate solid dispersion was formulated with hydroxypropyl methylcellulose, Pluronic F-127, and L-ascorbic acid. Aggregated particles showed porous structure when examined by scanning electron microscopy. Powder X-ray diffraction and Fourier transform infrared spectra indicated an interaction between ITZ and excipients and showed that ITZ existed in an amorphous state in the composite solid dispersion particles. The solid dispersion obtained by the SCF process improved the dissolution of ITZ in media of pH 1.0, pH 4.5, and pH 6.8, compared with a commercial product (Sporanox(®)), which could be ascribed to the porous aggregated particle shape and amorphous solid state of ITZ. While the solid dispersion did not show a statistical improvement (P=0.50) in terms of oral bioavailability of ITZ compared with Sporanox(®), the C max (the maximum plasma concentration of ITZ in a pharmacokinetic curve) of ITZ was raised significantly (P=0.03) after oral administration. Thus, the SCF process has been shown to be an efficient, single step process to form ITZ-containing solid dispersion particles with good dissolution and oral bioavailability characteristics.

Characterization of the molecular distribution of drugs in glassy solid dispersions at the nano-meter scale, using differential scanning calorimetry and gravimetric water vapour sorption techniques.

PubMed

van Drooge, D J; Hinrichs, W L J; Visser, M R; Frijlink, H W

2006-03-09

The molecular distribution in fully amorphous solid dispersions consisting of poly(vinylpyrrolidone) (PVP)-diazepam and inulin-diazepam was studied. One glass transition temperature (T(g)), as determined by temperature modulated differential scanning calorimetry (TMDSC), was observed in PVP-diazepam solid dispersions prepared by fusion for all drug loads tested (10-80 wt.%). The T(g) of these solid dispersions gradually changed with composition and decreased from 177 degrees C for pure PVP to 46 degrees C for diazepam. These observations indicate that diazepam was dispersed in PVP on a molecular level. However, in PVP-diazepam solid dispersions prepared by freeze drying, two T(g)'s were observed for drug loads above 35 wt.% indicating phase separation. One T(g) indicated the presence of amorphous diazepam clusters, the other T(g) was attributed to a PVP-rich phase in which diazepam was dispersed on a molecular level. With both the value of the latter T(g) and the DeltaC(p) of the diazepam glass transition the concentrations of molecular dispersed diazepam could be calculated (27-35 wt.%). Both methods gave similar results. Water vapour sorption (DVS) experiments revealed that the PVP-matrix was hydrophobised by the incorporated diazepam. TMDSC and DVS results were used to estimate the size of diazepam clusters in freeze dried PVP-diazepam solid dispersions, which appeared to be in the nano-meter range. The inulin-diazepam solid dispersions prepared by spray freeze drying showed one T(g) for drug loads up to 35 wt.% indicating homogeneous distribution on a molecular level. However, this T(g) was independent of the drug load, which is unexpected because diazepam has a lower T(g) than inulin (46 and 155 degrees C, respectively). For higher drug loads, a T(g) of diazepam as well as a T(g) of the inulin-rich phase was observed, indicating the formation of amorphous diazepam clusters. From the DeltaC(p) of the diazepam glass transition the amount of molecularly dispersed diazepam was calculated (12-27 wt.%). In contrast to the PVP-diazepam solid dispersions, DVS-experiments revealed that inulin was not hydrophobised by diazepam. Consequently, the size of diazepam clusters could not be estimated. It was concluded that TMDSC enables characterization and quantification of the molecular distribution in amorphous solid dispersions. When the hygroscopicity of the carrier is reduced by the drug, DVS in combination with TMDSC can be used to estimate the size of amorphous drug clusters.

Characterization and enhanced nonlinear optical limiting response in carbon nanodots dispersed in solid-state hybrid organically modified silica gel glasses

NASA Astrophysics Data System (ADS)

Huang, Li; Zheng, Chan; Guo, Qiaohang; Huang, Dongdong; Wu, Xiukai; Chen, Ling

2018-02-01

Freely dispersed carbon nanodots (CNDs) were introduced into a 3-glycidoxy-propyltrimethoxysilane modified silicate gel glass (i.e. an organically modified silica or ORMOSIL) by a highly efficient and simple sol-gel process, which could be easily extended to prepare functional molecules/nanoparticles solid state optoelectronic devices. Scanning electron microscope imaging, Fourier transform infrared spectroscopy, pore structure measurements, ultraviolet-visible spectroscopy, and fluorescence spectroscopy were used to investigate the surface characteristics, structure, texture, and linear optical properties of the CND/SiO2 ORMOSIL gel glasses. Images and UV/Vis spectra confirmed the successful dispersion of CNDs in the ORMOSIL gel glass. The surface characteristics and pore structure of the host SiO2 matrix were markedly changed through the introduction of the CNDs. The linear optical properties of the guest CNDs were also affected by the sol-gel procedure. The nonlinear optical (NLO) properties of the CNDs were investigated by a nanosecond open-aperture Z-scan technique at 532 nm both in liquid and solid matrices. We found that the NLO response of the CNDs was considerably improved after their incorporation into the ORMOSIL gel glasses. Possible enhancement mechanisms were also explored. The nonlinear extinction coefficient gradually increased while the optical limiting (OL) threshold decreased as the CND doping level was increased. This result suggests that the NLO and OL properties of the composite gel glasses can be optimized by tuning the concentration of CNDs in the gel glass matrix. Our findings show that CND/SiO2 ORMOSIL gel glasses are promising candidates for optical limiters to protect sensitive instruments and human eyes from damage caused by high power lasers.

In vitro characterization of a novel polymeric system for preparation of amorphous solid drug dispersions.

PubMed

Mahmoudi, Zahra N; Upadhye, Sampada B; Ferrizzi, David; Rajabi-Siahboomi, Ali R

2014-07-01

Preparation of amorphous solid dispersions using polymers is a commonly used formulation strategy for enhancing the solubility of poorly water-soluble drugs. However, often a single polymer may not bring about a significant enhancement in solubility or amorphous stability of a poorly water-soluble drug. This study describes application of a unique and novel binary polymeric blend in preparation of solid dispersions. The objective of this study was to investigate amorphous solid dispersions of glipizide, a BCS class II model drug, in a binary polymeric system of polyvinyl acetate phthalate (PVAP) and hypromellose (hydroxypropyl methylcellulose, HPMC). The solid dispersions were prepared using two different solvent methods: rotary evaporation (rotavap) and fluid bed drug layering on sugar spheres. The performance and physical stability of the dispersions were evaluated with non-sink dissolution testing, powder X-ray diffraction (PXRD), and modulated differential scanning calorimetry (mDSC). PXRD analysis demonstrated an amorphous state for glipizide, and mDSC showed no evidence of phase separation. Non-sink dissolution testing in pH 7.5 phosphate buffer indicated more than twofold increase in apparent solubility of the drug with PVAP-HPMC system. The glipizide solid dispersions demonstrated a high glass transition temperature (Tg) and acceptable chemical and physical stability during the stability period irrespective of the manufacturing process. In conclusion, the polymeric blend of PVAP-HPMC offers a unique formulation approach for developing amorphous solid dispersions with the flexibility towards the use of these polymers in different ratios and combined quantities depending on drug properties.

Determination of sulfonamides in milk by capillary electrophoresis with PEG@MoS2 as a dispersive solid-phase extraction sorbent.

PubMed

An, Jianxin; Wang, Xuan; Ming, Meiting; Li, Jian; Ye, Nengsheng

2018-05-01

A synthetic polyethylene glycol-molybdenum disulfide (PEG@MoS 2 ) composite was prepared using a simple method, and the application of this material in dispersive solid-phase extraction (DSPE) was investigated for the enrichment of eight sulfonamides (SAs) in milk samples. The composite was characterized by energy dispersive spectroscopy, scanning electron microscopy, transmission electron microscopy, Fourier transform infrared spectroscopy and Brunauer-Emmett-Teller measurements. The results showed that the MoS 2 synthesized in the presence of PEG has the advantage of a larger surface area and that the adsorption effect of this MoS 2 was enhanced. After extraction, the eight SAs were separated by capillary zone electrophoresis with a good linear relationship ( R 2  > 0.9902) in the range of 0.3-30 µg ml -1 and good precision (between 0.32% and 9.83%). Additionally, good recoveries (between 60.52% and 110.91%) were obtained for the SAs in the milk samples. The developed PEG@MoS 2 -based DSPE method could be applied for the enrichment of SAs in real milk samples.

An improved kinetics approach to describe the physical stability of amorphous solid dispersions.

PubMed

Yang, Jiao; Grey, Kristin; Doney, John

2010-01-15

The recrystallization of amorphous solid dispersions may lead to a loss in the dissolution rate, and consequently reduce bioavailability. The purpose of this work is to understand factors governing the recrystallization of amorphous drug-polymer solid dispersions, and develop a kinetics model capable of accurately predicting their physical stability. Recrystallization kinetics was measured using differential scanning calorimetry for initially amorphous efavirenz-polyvinylpyrrolidone solid dispersions stored at controlled temperature and relative humidity. The experimental measurements were fitted by a new kinetic model to estimate the recrystallization rate constant and microscopic geometry of crystal growth. The new kinetics model was used to illustrate the governing factors of amorphous solid dispersions stability. Temperature was found to affect efavirenz recrystallization in an Arrhenius manner, while recrystallization rate constant was shown to increase linearly with relative humidity. Polymer content tremendously inhibited the recrystallization process by increasing the crystallization activation energy and decreasing the equilibrium crystallinity. The new kinetic model was validated by the good agreement between model fits and experiment measurements. A small increase in polyvinylpyrrolidone resulted in substantial stability enhancements of efavirenz amorphous solid dispersion. The new established kinetics model provided more accurate predictions than the Avrami equation.

Mechanism for enhanced absorption of a solid dispersion formulation of LY2300559 using the artificial stomach duodenum model.

PubMed

Polster, Christopher S; Wu, Sy-Juen; Gueorguieva, Ivelina; Sperry, David C

2015-04-06

An artificial stomach duodenum (ASD) model has been used to demonstrate the performance difference between two formulations of LY2300559, a low-solubility acidic developmental drug. The two formulations investigated were a conventional high-shear wet granulation (HSWG) formulation and a solid dispersion formulation. A pharmacokinetic study in humans demonstrated the enhanced performance of the solid dispersion formulation relative to the HSWG formulation. The Cmax and AUC of the solid dispersion was 2.6 and 1.9 times greater, respectively, compared to the HSWG formulation. In the ASD, the solid dispersion formulation performance was characterized by three main phases: (1) rapid release in the stomach, creating a supersaturated concentration of drug, (2) precipitation in the stomach, and (3) rapid redissolution of the precipitate in the duodenum to concentration levels that are supersaturated relative to crystalline drug. A series of complementary experiments were employed to describe this performance behavior mechanistically. Imaging experiments with a pH indicating dye showed that local pH gradients from meglumine in the solid dispersion formulation were responsible for creating a high initial supersaturation concentration in the stomach. Upon dissipation of meglumine, the drug precipitated in the stomach as an amorphous solid. Because the precipitated drug is in an amorphous form, it can then rapidly redissolve as it transits to the more neutral environment of the duodenum. This unexpected sequence of physical state changes gives a mechanistic explanation for the enhanced in vivo performance of the solid dispersion formulation relative to the HSWG formulation.

Investigation for the amorphous state of ER-34122, a dual 5-lipoxygenase/cyclooxygenase inhibitor with poor aqueous solubility, in HPMC solid dispersion prepared by the solvent evaporation method.

PubMed

Kushida, Ikuo; Gotoda, Masaharu

2013-10-01

ER-34122, a poorly water-soluble dual 5-lipoxygenase/cyclooxygenase inhibitor, exists as a crystalline form. According to an Oak Ridge thermal ellipsoid plot drawing, carbonyl oxygen O (5) makes an intermolecular hydrogen bond with the hydrogen bonded to N (3) in the crystal structure. The FTIR and the solid-state ¹³C NMR spectra suggest that the network is spread out in the amorphous state and the hydrogen bonding gets weaker than that in the crystalline phase, because the carbonyl signals significantly shift in both spectra. When amorphous ER-34122 was heated, crystallization occurred at around 140°C. Similar crystallization happened in the solid dispersion; however, the degree of crystallization was much lower than that observed in the pure amorphous material. Also, the DSC thermogram of the solid dispersion did not show any exothermic peaks implying crystallization. The heat of fusion (ΔHf) determined in the pure amorphous material was nearly equal to that for the crystalline form, whereas the ΔHf value obtained in the solid dispersion was less than a third of them. These data prove that crystallization of the amorphous form is dramatically restrained in the solid dispersion system. The carbonyl wavenumber shifts in the FTIR spectra indicate that the average hydrogen bond in the solid dispersion is lower than that in the pure amorphous material. Therefore, HPMC will suppress formation of the intermolecular network observed in ER-34122 crystal and preserve the amorphous state, which is thermodynamically less stable, in the solid dispersed system.

Laser-based linear and nonlinear guided elastic waves at surfaces (2D) and wedges (1D).

PubMed

Hess, Peter; Lomonosov, Alexey M; Mayer, Andreas P

2014-01-01

The characteristic features and applications of linear and nonlinear guided elastic waves propagating along surfaces (2D) and wedges (1D) are discussed. Laser-based excitation, detection, or contact-free analysis of these guided waves with pump-probe methods are reviewed. Determination of material parameters by broadband surface acoustic waves (SAWs) and other applications in nondestructive evaluation (NDE) are considered. The realization of nonlinear SAWs in the form of solitary waves and as shock waves, used for the determination of the fracture strength, is described. The unique properties of dispersion-free wedge waves (WWs) propagating along homogeneous wedges and of dispersive wedge waves observed in the presence of wedge modifications such as tip truncation or coatings are outlined. Theoretical and experimental results on nonlinear wedge waves in isotropic and anisotropic solids are presented. Copyright © 2013 Elsevier B.V. All rights reserved.

Measurement of cylindrical Rayleigh surface waves using line-focused PVDF transducers and defocusing measurement method.

PubMed

Lin, Chun-I; Lee, Yung-Chun

2014-08-01

Line-focused PVDF transducers and defocusing measurement method are applied in this work to determine the dispersion curve of the Rayleigh-like surface waves propagating along the circumferential direction of a solid cylinder. Conventional waveform processing method has been modified to cope with the non-linear relationship between phase angle of wave interference and defocusing distance induced by a cylindrically curved surface. A cross correlation method is proposed to accurately extract the cylindrical Rayleigh wave velocity from measured data. Experiments have been carried out on one stainless steel and one glass cylinders. The experimentally obtained dispersion curves are in very good agreement with their theoretical counterparts. Variation of cylindrical Rayleigh wave velocity due to the cylindrical curvature is quantitatively verified using this new method. Other potential applications of this measurement method for cylindrical samples will be addressed. Copyright © 2014 Elsevier B.V. All rights reserved.

Evaluate the ability of PVP to inhibit crystallization of amorphous solid dispersions by density functional theory and experimental verify.

PubMed

Wang, Bing; Wang, Dandan; Zhao, Shan; Huang, Xiaobin; Zhang, Jianbin; Lv, Yan; Liu, Xiaocen; Lv, Guojun; Ma, Xiaojun

2017-01-01

In this study, we used density functional theory (DFT) to predict polymer-drug interactions, and then evaluated the ability of poly (vinyl pyrrolidone) (PVP) to inhibit crystallization of amorphous solid dispersions by experimental-verification. Solid dispersions of PVP/resveratrol (Res) and PVP/griseofulvin (Gri) were adopted for evaluating the ability of PVP to inhibit crystallization. The density functional theory (DFT) with the B3LYP was used to calculate polymer-drug and drug-drug interactions. Fourier transform infrared spectroscopy (FTIR) was used to confirm hydrogen bonding interactions. Polymer-drug miscibility and drug crystallinity were characterized by the modulated differential scanning calorimetry (MDSC) and X-ray powder diffraction (XRD). The release profiles were studied to investigate the dissolution advantage. DFT results indicated that E PVP-Res >E Res-Res (E: represents hydrogen bonding energy). A strong interaction was formed between PVP and Res. In addition, Fourier transform infrared spectroscopy (FTIR) analysis showed hydrogen bonding formed between PVP and Res, but not between PVP and Gri. MDSC and XRD results suggested that 70-90wt% PVP/Res and PVP/Gri solid dispersions formed amorphous solid dispersions (ASDs). Under the accelerated testing condition, PVP/Res dispersions with higher miscibility quantified as 90/10wt% were more stable than PVP/Gri dispersions. The cumulative dissolution rate of 90wt% PVP/Res dispersions still kept high after 90days storage due to the strong interaction. However, the cumulative dissolution rate of PVP/Gri solid dispersions significantly dropped because of the recrystallization of Gri. Copyright © 2016 Elsevier B.V. All rights reserved.

Comparative study on solid self-nanoemulsifying drug delivery and solid dispersion system for enhanced solubility and bioavailability of ezetimibe

PubMed Central

Rashid, Rehmana; Kim, Dong Wuk; Yousaf, Abid Mehmood; Mustapha, Omer; Din, Fakhar ud; Park, Jong Hyuck; Yong, Chul Soon; Oh, Yu-Kyoung; Youn, Yu Seok; Kim, Jong Oh; Choi, Han-Gon

2015-01-01

Background The objective of this study was to compare the physicochemical characteristics, solubility, dissolution, and oral bioavailability of an ezetimibe-loaded solid self-nanoemulsifying drug delivery system (SNEDDS), surface modified solid dispersion (SMSD), and solvent evaporated solid dispersion (SESD) to identify the best drug delivery system with the highest oral bioavailability. Methods For the liquid SNEDDS formulation, Capryol 90, Cremophor EL, and Tween 80 were selected as the oil, surfactant, and cosurfactant, respectively. The nanoemulsion-forming region was sketched using a pseudoternary phase diagram on the basis of reduced emulsion size. The optimized liquid SNEDDS was converted to solid SNEDDS by spray drying with silicon dioxide. Furthermore, SMSDs were prepared using the spray drying technique with various amounts of hydroxypropylcellulose and Tween 80, optimized on the basis of their drug solubility. The SESD formulation was prepared with the same composition of optimized SMSD. The aqueous solubility, dissolution, physicochemical properties, and pharmacokinetics of all of the formulations were investigated and compared with the drug powder. Results The drug existed in the crystalline form in SMSD, but was changed into an amorphous form in SNEDDS and SESD, giving particle sizes of approximately 24, 6, and 11 µm, respectively. All of these formulations significantly improved the aqueous solubility and dissolution in the order of solid SNEDDS ≥ SESD > SMSD, and showed a total higher plasma concentration than did the drug powder. Moreover, SESD gave a higher area under the drug concentration time curve from zero to infinity than did SNEDDS and SMSD, even if they were not significantly different, suggesting more improved oral bioavailability. Conclusion Among the various formulations tested in this study, the SESD system would be strongly recommended as a drug delivery system for the oral administration of ezetimibe with poor water solubility. PMID:26491288

Modelling and calculation of flotation process in one-dimensional formulation

NASA Astrophysics Data System (ADS)

Amanbaev, Tulegen; Tilleuov, Gamidulla; Tulegenova, Bibigul

2016-08-01

In the framework of the assumptions of the mechanics of the multiphase media is constructed a mathematical model of the flotation process in the dispersed mixture of liquid, solid and gas phases, taking into account the degree of mineralization of the surface of the bubbles. Application of the constructed model is demonstrated on the example of one-dimensional stationary flotation and it is shown that the equations describing the process of ascent of the bubbles are singularly perturbed ("rigid"). The effect of size and concentration of bubbles and the volumetric content of dispersed particles on the flotation process are analyzed.

Surfactant-Free Solid Dispersions of Hydrophobic Drugs in an Amorphous Sugar Matrix Dried from an Organic Solvent.

PubMed

Takeda, Koji; Gotoda, Yuto; Hirota, Daichi; Hidaka, Fumihiro; Sato, Tomo; Matsuura, Tsutashi; Imanaka, Hiroyuki; Ishida, Naoyuki; Imamura, Koreyoshi

2017-03-06

The technique for homogeneously dispersing hydrophobic drugs in a water-soluble solid matrix (solid dispersion) is a subject that has been extensively investigated in the pharmaceutical industry. Herein, a novel technique for dispersing a solid, without the need to use a surfactant, is reported. A freeze-dried amorphous sugar sample was dissolved in an organic solvent, which contained a soluble model hydrophobic component. The suspension of the sugar and the model hydrophobic component was vacuum foam dried to give a solid powder. Four types of sugars and methanol were used as representative sugars and the organic medium. Four model drugs (indomethacin, ibuprofen, gliclazide, and nifedipine) were employed. Differential scanning calorimetry analyses indicated that the sugar and model drug (100:1) did not undergo segregation during the drying process. The dissolution of the hydrophobic drugs in water from the solid dispersion was then evaluated, and the results indicated that the C max and AUC 0-60 min of the hydrophobic drug in water were increased when the surfactant-free solid dispersion was used. Palatinose and/or α-maltose were superior to the other tested carbohydrates in increasing C max and AUC 0-60 min for all tested model drugs, and the model drug with a lower water solubility tended to exhibit a greater extent of over-dissolution.

Preparation and physicochemical characterization of spray-dried and jet-milled microparticles containing bosentan hydrate for dry powder inhalation aerosols.

PubMed

Lee, Hyo-Jung; Kang, Ji-Hyun; Lee, Hong-Goo; Kim, Dong-Wook; Rhee, Yun-Seok; Kim, Ju-Young; Park, Eun-Seok; Park, Chun-Woong

2016-01-01

The objectives of this study were to prepare bosentan hydrate (BST) microparticles as dry powder inhalations (DPIs) via spray drying and jet milling under various parameters, to comprehensively characterize the physicochemical properties of the BST hydrate microparticles, and to evaluate the aerosol dispersion performance and dissolution behavior as DPIs. The BST microparticles were successfully prepared for DPIs by spray drying from feeding solution concentrations of 1%, 3%, and 5% (w/v) and by jet milling at grinding pressures of 2, 3, and 4 MPa. The physicochemical properties of the spray-dried (SD) and jet-milled (JM) microparticles were determined via scanning electron microscopy, atomic force microscopy, dynamic light scattering particle size analysis, Karl Fischer titration, surface analysis, pycnometry, differential scanning calorimetry, powder X-ray diffraction, and Fourier transform infrared spectroscopy. The in vitro aerosol dispersion performance and drug dissolution behavior were evaluated using an Anderson cascade impactor and a Franz diffusion cell, respectively. The JM microparticles exhibited an irregular corrugated surface and a crystalline solid state, while the SD microparticles were spherical with a smooth surface and an amorphous solid state. Thus, the in vitro aerosol dispersion performance and dissolution behavior as DPIs were considerably different due to the differences in the physicochemical properties of the SD and JM microparticles. In particular, the highest grinding pressures under jet milling exhibited excellent aerosol dispersion performance with statistically higher values of 56.8%±2.0% of respirable fraction and 33.8%±2.3% of fine particle fraction and lower mass median aerodynamic diameter of 5.0±0.3 μm than the others ( P <0.05, analysis of variance/Tukey). The drug dissolution mechanism was also affected by the physicochemical properties that determine the dissolution kinetics of the SD and JM microparticles, which were well fitted into the Higuchi and zero-order models, respectively.

Investigation of phase diagrams and physical stability of drug-polymer solid dispersions.

PubMed

Lu, Jiannan; Shah, Sejal; Jo, Seongbong; Majumdar, Soumyajit; Gryczke, Andreas; Kolter, Karl; Langley, Nigel; Repka, Michael A

2015-01-01

Solid dispersion technology has been widely explored to improve the solubility and bioavailability of poorly water-soluble compounds. One of the critical drawbacks associated with this technology is the lack of physical stability, i.e. the solid dispersion would undergo recrystallization or phase separation thus limiting a product's shelf life. In the current study, the melting point depression method was utilized to construct a complete phase diagram for felodipine (FEL)-Soluplus® (SOL) and ketoconazole (KTZ)-Soluplus® (SOL) binary systems, respectively, based on the Flory-Huggins theory. The miscibility or solubility of the two compounds in SOL was also determined. The Flory-Huggins interaction parameter χ values of both systems were calculated as positive at room temperature (25 °C), indicating either compound was miscible with SOL. In addition, the glass transition temperatures of both solid dispersion systems were theoretically predicted using three empirical equations and compared with the practical values. Furthermore, the FEL-SOL solid dispersions were subjected to accelerated stability studies for up to 3 months.

Impact of surfactants on the crystallization of aqueous suspensions of celecoxib amorphous solid dispersion spray dried particles.

PubMed

Chen, Jie; Ormes, James D; Higgins, John D; Taylor, Lynne S

2015-02-02

Amorphous solid dispersions are frequently prepared by spray drying. It is important that the resultant spray dried particles do not crystallize during formulation, storage, and upon administration. The goal of the current study was to evaluate the impact of surfactants on the crystallization of celecoxib amorphous solid dispersions (ASD), suspended in aqueous media. Solid dispersions of celecoxib with hydroxypropylmethylcellulose acetate succinate were manufactured by spray drying, and aqueous suspensions were prepared by adding the particles to acidified media containing various surfactants. Nucleation induction times were evaluated for celecoxib in the presence and absence of surfactants. The impact of the surfactants on drug and polymer leaching from the solid dispersion particles was also evaluated. Sodium dodecyl sulfate and Polysorbate 80 were found to promote crystallization from the ASD suspensions, while other surfactants including sodium taurocholate and Triton X100 were found to inhibit crystallization. The promotion or inhibition of crystallization was found to be related to the impact of the surfactant on the nucleation behavior of celecoxib, as well as the tendency to promote leaching of the drug from the ASD particle into the suspending medium. It was concluded that surfactant choice is critical to avoid failure of amorphous solid dispersions through crystallization of the drug.

Cefuroxime axetil solid dispersion with polyglycolized glycerides for improved stability and bioavailability.

PubMed

Dhumal, Ravindra S; Biradar, Shailesh V; Aher, Suyog; Paradkar, Anant R

2009-06-01

Cefuroxime axetil (CA), a poorly soluble, broad spectrum cephalosporin ester prodrug, is hydrolysed by intestinal esterase prior to absorption, leading to poor and variable bioavailability. The objective was therefore to formulate a stable amorphous solid dispersion of the drug with enhanced solubility and stability against enzymatic degradation. Spray drying was used to obtain a solid dispersion of CA with Gelucire 50/13 and Aerosil 200 (SDCAGA), and a solid dispersion of CA with polyvinyl pyrrolidone (SDCAP); amorphous CA (ACA) was obtained by spray drying CA alone. The formulations were characterized by differential scanning calorimetry, X-ray powder diffraction, scanning electron microscopy and Fourier transform infrared spectroscopy studies, and compared for solubility, dissolution and bioavailability in rats. SDCAP and SDCAGA showed improved solubility and dissolution profiles owing to amorphization and formation of solid dispersions with hydrophilic carriers. The improved stability of amorphous CA in solid dispersions compared to ACA alone was attributed to hydrogen bonding interactions involving the amide of CA with the carbonyl of polyvinyl pyrrolidone in SDCAP, whereas in SDCAGA the interactions were at multiple sites involving the amide and carbonyl of CA with the carbonyl and hydroxyl of Gelucire 50/13. However, SDCAGA showed superior bioavailability compared to SDCAP, ACA and CA. Improvement in physical stability of solid dispersions was attributed to hydrogen bonding, while improvement in bioavailability of SDCAGA compared to SDCAP, in spite of comparable solubility and dissolution profile, may be attributed to Gelucire, which utilizes intestinal esterase for lipolysis, protecting the prodrug from enzymatic degradation to its non-absorbable base form.

Increased dissolution rate and oral bioavailability of hydrophobic drug glyburide tablets produced using supercritical CO₂ silica dispersion technology.

PubMed

Guan, Jibin; Han, Jihong; Zhang, Dong; Chu, Chunxia; Liu, Hongzhuo; Sun, Jin; He, Zhonggui; Zhang, Tianhong

2014-04-01

The aim of this study was to design a silica-supported solid dispersion of a water-insoluble drug, glyburide, to increase its dissolution rate and oral absorption using supercritical fluid (SCF) technology. DSC and PXRD results indicated that the encapsulated drug in the optimal solid dispersion was in an amorphous state and the product was stable for 6 months. Glyburide was adsorbed onto the porous silica, as confirmed by the SEM images and BET analysis. Furthermore, FT-IR spectroscopy confirmed that there was no change in the chemical structure of glyburide after the application of SCF. The glyburide silica-based dispersion could also be compressed into tablet form. In vitro drug release analysis of the silica solid dispersion tablets demonstrated faster release of glyburide compared with the commercial micronized tablet. In an in vivo test, the AUC of the tablets composed of the new glyburide silica-based solid dispersion was 2.01 times greater than that of the commercial micronized glyburide tablets. In conclusion, SCF technology presents a promising approach to prepare silica-based solid dispersions of hydrophobic drugs because of its ability to increase their release and oral bioavailability. Copyright © 2013 Elsevier B.V. All rights reserved.

Nanoparticles That "Remember" Temperature

DOE Office of Scientific and Technical Information (OSTI.GOV)

Klajn, Rafal; Browne, Kevin P.; Siowling, Soh

2010-06-02

Photoresponsive gold nanoparticles dispersed in a solid/frozen matrix provide a basis for sensors that “remember” whether the sample has ever exceeded the melting temperature of the matrix. The operation of these sensors rests on the ability to photoinduce metastable electric dipoles on NP surfaces – upon melting, these dipoles drive NP aggregation, precipitation, and crosslinking. These events are manifested by a pronounced color change.

Dispersoid reinforced alloy powder and method of making

DOE Office of Scientific and Technical Information (OSTI.GOV)

Anderson, Iver E.; Terpstra, Robert L.

A method of making dispersion-strengthened alloy particles involves melting an alloy having a corrosion and/or oxidation resistance-imparting alloying element, a dispersoid-forming element, and a matrix metal wherein the dispersoid-forming element exhibits a greater tendency to react with a reactive species acquired from an atomizing gas than does the alloying element. The melted alloy is atomized with the atomizing gas including the reactive species to form atomized particles so that the reactive species is (a) dissolved in solid solution to a depth below the surface of atomized particles and/or (b) reacted with the dispersoid-forming element to form dispersoids in the atomizedmore » particles to a depth below the surface of said atomized particles. The atomized alloy particles are solidified as solidified alloy particles or as a solidified deposit of alloy particles. Bodies made from the dispersion strengthened alloy particles, deposit thereof, exhibit enhanced fatigue and creep resistance and reduced wear as well as enhanced corrosion and/or oxidation resistance at high temperatures by virtue of the presence of the corrosion and/or oxidation resistance imparting alloying element in solid solution in the particle alloy matrix.« less

Dispersoid reinforced alloy powder and method of making

DOE Office of Scientific and Technical Information (OSTI.GOV)

Anderson, Iver E.; Terpstra, Robert L.

2017-10-10

A method of making dispersion-strengthened alloy particles involves melting an alloy having a corrosion and/or oxidation resistance-imparting alloying element, a dispersoid-forming element, and a matrix metal wherein the dispersoid-forming element exhibits a greater tendency to react with a reactive species acquired from an atomizing gas than does the alloying element. The melted alloy is atomized with the atomizing gas including the reactive species to form atomized particles so that the reactive species is (a) dissolved in solid solution to a depth below the surface of atomized particles and/or (b) reacted with the dispersoid-forming element to form dispersoids in the atomizedmore » particles to a depth below the surface of said atomized particles. The atomized alloy particles are solidified as solidified alloy particles or as a solidified deposit of alloy particles. Bodies made from the dispersion strengthened alloy particles, deposit thereof, exhibit enhanced fatigue and creep resistance and reduced wear as well as enhanced corrosion and/or oxidation resistance at high temperatures by virtue of the presence of the corrosion and/or oxidation resistance imparting alloying element in solid solution in the particle alloy matrix.« less

Tape method of forming a thin layer of doped lanthanum chromite particles and of bonding such on an electrode

DOEpatents

Richards, Von L.; Singhal, Subhash C.; Pal, Uday B.

1992-01-01

A combustible polymer film, useful for application of an interconnection on an electrode is made by: (1) providing doped LaCro.sub.3 particles; (2) dispersing doped LaCrO.sub.3 particles in a solvent, to provide a dispersion; (3) screening the dispersion to provide particles in the range of from 30 micrometers to 80 micrometers; (4) admixing a fugitive polymer with the particles; (5) casting the dispersion to provide a film; (6) drying the film; and (7) stripping the film. The film can then be applied to a porous, preheated electrode top surface, and then electrochemical vapor depositing a dense skeletal LaCrO.sub.3 structure, between and around the doped LaCrO.sub.3 particles. Additional solid oxide electrolyte and fuel electrode layers can then be added to provide a fuel cell.

Tape method of forming a thin layer of doped lanthanum chromite particles and of bonding such on an electrode

DOEpatents

Richards, V.L.; Singhal, S.C.; Pal, U.B.

1992-07-21

A combustible polymer film, useful for application of an interconnection on an electrode is made by: (1) providing doped LaCro[sub 3] particles; (2) dispersing doped LaCrO[sub 3] particles in a solvent, to provide a dispersion; (3) screening the dispersion to provide particles in the range of from 30 micrometers to 80 micrometers; (4) admixing a fugitive polymer with the particles; (5) casting the dispersion to provide a film; (6) drying the film; and (7) stripping the film. The film can then be applied to a porous, preheated electrode top surface, and then a dense skeletal LaCrO[sub 3] structure is electrochemically vapor deposited between and around the doped LaCrO[sub 3] particles. Additional solid oxide electrolyte and fuel electrode layers can then be added to provide a fuel cell. 4 figs.

Effect of surfactant on temperature stability of solid lipid nanoparticles studied by dynamic light scattering

NASA Astrophysics Data System (ADS)

Kumar, Sacheen; Kaur, Jaspreet

2013-06-01

Solid lipid nanoparticles are new paradigm of drug delivery system of water insoluble active pharmaceutical ingredient. Paliperidone, an antipsychotic used in treatment of schizophrenia is a water insoluble molecule with low bioavailability was studied. Macrogol glyceride surfactant, bile salt based surfactant and sodium dodecyl sulphate were used to stabilize the solid lipid as dispersed nanoparticles form by adsorbing on the surface of the nanoparticles. Anionic surfactants bile salt and sodium dodecyl sulphate were found to stabilize forming a monomolecular layer of surfactants on the surface of nanoparticles; whereas macrogol glyceride based surfactant have intrusion in the matrix of lipid nanoparticles. So intrusion of macrogol glyceride in matrix was observed by studying the change in size of nanoparticles with respect to temperature with the help of dynamic light scattering. In case of macrogol glyceride size decrease start form 50°C, for bile salt and sodium dodecyl sulphate size deacrease start at 60°C. So that structural disturbance of nanoparticles by the macrogol glyceride on the surface was found maximum as compared to anionic surfactant.

Preconcentration of Trace Neonicotinoid Insecticide Residues Using Vortex-Assisted Dispersive Micro Solid-Phase Extraction with Montmorillonite as an Efficient Sorbent.

PubMed

Moyakao, Khwankaew; Santaladchaiyakit, Yanawath; Srijaranai, Supalax; Vichapong, Jitlada

2018-04-11

In this work, we investigated montmorillonite for adsorption of neonicotinoid insecticides in vortex-assisted dispersive micro-solid phase extraction (VA-d-μ-SPE). High-performance liquid chromatography with photodiode array detection was used for quantification and determination of neonicotinoid insecticide residues, including thiamethoxam, clothianidin, imidacloprid, acetamiprid, and thiacloprid. In this method, the solid sorbent was dispersed into the aqueous sample solution and vortex agitation was performed to accelerate the extraction process. Finally, the solution was filtered from the solid sorbent with a membrane filter. The parameters affecting the extraction efficiency of the proposed method were optimized, such as amount of sorbent, sample volume, salt addition, type and volume of extraction solvent, and vortex time. The adsorbing results show that montmorillonite could be reused at least 4 times and be used as an effective adsorbent for rapid extraction/preconcentration of neonicotinoid insecticide residues. Under optimum conditions, linear dynamic ranges were achieved between 0.5 and 1000 ng mL -1 with a correlation of determination ( R² ) greater than 0.99. Limit of detection (LOD) ranged from 0.005 to 0.065 ng mL -1 , while limit of quantification (LOQ) ranged from 0.008 to 0.263 ng mL -1 . The enrichment factor (EF) ranged from 8 to 176-fold. The results demonstrated that the proposed method not only provided a more simple and sensitive method, but also can be used as a powerful alternative method for the simultaneous determination of insecticide residues in natural surface water and fruit juice samples.

Investigation of Post-Flight Solid Rocket Booster Thermal Protection System

NASA Technical Reports Server (NTRS)

Nelson, Linda A.

2006-01-01

After every Shuttle mission, the Solid Rocket Boosters (SRBs) are recovered and observed for missing material. Most of the SRB is covered with a cork-based thermal protection material (MCC-l). After the most recent shuttle mission, STS-114, the forward section of the booster appeared to have been impacted during flight. The darkened fracture surfaces indicated that this might have occurred early in flight. The scope of the analysis included microscopic observations to assess the degree of heat effects and locate evidence of the impact source as well as chemical analysis of the fracture surfaces and recovered foreign material using Fourier Transform Infrared Spectroscopy and Scanning Electron Microscopy/Energy Dispersive Spectroscopy. The amount of heat effects and presence of soot products on the fracture surface indicated that the material was impacted prior to SRB re-entry into the atmosphere. Fragments of graphite fibers found on these fracture surfaces were traced to slag inside the Solid Rocket Motor (SRM) that forms during flight as the propellant is spent and is ejected throughout the descent of the SRB after separation. The direction of the impact mark matches with the likely trajectory of SRBs tumbling prior to re-entry.

Nanocrystal-polymer nanocomposite electrochromic device

DOEpatents

Milliron, Delia; Runnerstrom, Evan; Helms, Brett; Llordes, Anna; Buonsanti, Raffaella; Garcia, Guillermo

2015-12-08

Described is an electrochromic nanocomposite film comprising a solid matrix of an oxide based material, the solid matrix comprising a plurality of transparent conducting oxide (TCO) nanostructures dispersed in the solid matrix and a lithium salt dispersed in the solid matrix. Also described is a near infrared nanostructured electrochromic device having a functional layer comprising the electrochromic nanocomposite film.

Nanolubricant: magnetic nanoparticle based

NASA Astrophysics Data System (ADS)

Trivedi, Kinjal; Parekh, Kinnari; Upadhyay, Ramesh V.

2017-11-01

In the present study magnetic nanoparticles of Fe3O4 having average particle diameter, 11.7 nm were synthesized using chemical coprecipitation technique and dispersed in alpha olefin hydrocarbon synthetic lubricating oil. The solid weight fraction of magnetic nanoparticles in the lubricating oil was varied from 0 wt% to 10 wt%. The tribological properties were studied using four-ball tester. The results demonstrate that the coefficient of friction and wear scar diameter reduces by 45% and 30%, respectively at an optimal value, i.e. 4 wt% of magnetic nanoparticles concentration. The surface characterization of worn surface was carried out using a scanning electron microscope, and energy dispersive spectroscopy. These results implied that rolling mechanism is responsible to reduce coefficient of friction while magnetic nanoparticles act as the spacer between the asperities and reduces the wear scar diameter. The surface roughness of the worn surface studied using an atomic force microscope shows a reduction in surface roughness by a factor of four when magnetic nanoparticles are used as an additive. The positive response of magnetic nanoparticles in a lubricating oil, shows the potential replacement of conventional lubricating oil.

PEG-Stabilized Core–Shell Surface-Imprinted Nanoparticles

PubMed Central

Moczko, Ewa; Guerreiro, Antonio; Piletska, Elena; Piletsky, Sergey

2016-01-01

Here we present a simple technique to produce target-specific molecularly imprinted polymeric nanoparticles (MIP NPs) and their surface modification in order to prevent the aggregation process that is ever-present in most nanomaterial suspensions/dispersions. Specifically, we studied the influence of surface modification of MIP NPs with polymerizable poly(ethylene glycol) on their degree of stability in water, in phosphate buffer, and in the presence of serum proteins. Grafting a polymer shell on the surface of nanoparticles decreases the surface energy, enhances the polarity, and as a result improves the dispersibility, storage, and colloidal stability as compared to those of core (unmodified) particles. Because of the unique solid-phase approach used for synthesis, the binding sites of MIP NPs are protected during grafting, and the recognition properties of nanoparticles are not affected. These results are significant for developing nanomaterials with selective molecular recognition, increased biocompatibility, and stability in solution. Materials synthesized this way have the potential to be used in a variety of technological fields, including in vivo applications such as drug delivery and imaging. PMID:23855734

Dielectric spectroscopy for the determination of the glass transition temperature of pharmaceutical solid dispersions.

PubMed

O'Donnell, Kevin P; Woodward, W H Hunter

2015-06-01

The purpose of this study was to evaluate analytical techniques for the measurement of the glass transition temperature of HPMC and formulated solid dispersions thereof. Unmodified samples of various grades of HPMC and solid dispersions of HPMC and itraconazole produced by hot melt extrusion were analyzed by thermomechanical analysis, differential scanning calorimetry, thermally stimulated depolarization current and dielectric spectroscopy. It was found that dielectric spectroscopy offers the best accuracy and reproducibility for analysis of the base HPMC powders regardless of the substitution type or viscosity grade and that the obtained results were not frequency dependent. The results of dielectric measurements of solid dispersions prepared by hot melt extrusion were compared with predicted values of the Gordon-Taylor equation. It was found that time-temperature superposition effects and small molecule frequency dependence makes broadly applying determination of the glass transition temperature in drug dispersions by dielectric spectroscopy prohibitively difficult.

Prediction of recrystallization behavior of troglitazone/polyvinylpyrrolidone solid dispersion by solid-state NMR.

PubMed

Ito, Atsutoshi; Watanabe, Tomoyuki; Yada, Shuichi; Hamaura, Takeshi; Nakagami, Hiroaki; Higashi, Kenjirou; Moribe, Kunikazu; Yamamoto, Keiji

2010-01-04

The purpose of this study was to elaborate the relationship between the (13)C CP/MAS NMR spectra and the recrystallization behavior during the storage of troglitazone solid dispersions. The solid dispersions were prepared by either the solvent method or by co-grinding. The recrystallization behavior under storage conditions at 40 degrees C/94% RH was evaluated by the Kolmogorov-Johnson-Mehl-Avrami (KJMA) equation. Solid dispersions prepared by the solvent method or by prolonged grinding brought about inhibition of the nucleation and the nuclei growth at the same time. No differences in the PXRD profiles were found in the samples prepared by the co-grinding and solvent methods, however, (13)C CP/MAS NMR showed significant differences in the spectra. The correlation coefficients using partial least square regression analysis between the PXRD profiles and the apparent nuclei-growth constant or induction period to nucleation were 0.1305 or 0.6350, respectively. In contrast, those between the (13)C CP/MAS NMR spectra and the constant or the period were 0.9916 or 0.9838, respectively. The (13)C CP/MAS NMR spectra had good correlation with the recrystallization kinetic parameters evaluated by the KJMA equation. Consequently, solid-state NMR was judged to be a useful tool for the prediction of the recrystallization behavior of solid dispersions.

Surface active stabilizer Tyloxapol in colloidal dispersions exerts cytostatic effects and apoptotic dismissal of cells

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kristl, Julijana; Teskac, Karmen; Milek, Miha

Solid lipid nanoparticles (SLN) have been praised for their advantageous drug delivery properties such as biocompatibility, controlled release and passive drug targeting. However, the cytotoxicity of SLN and their ingredients, especially over a longer time period, has not been investigated in detail. We examined the critical issues regarding the use of a surface active stabilizer Tyloxapol (Tyl) for the preparation of solid lipid particles (SLP) and their effects on cellular functions and viability. SLP composed of behenate, phospholipids and a stabilizer, Tyloxapol or Lutrol (Lut), were prepared by the lipid melt method, labeled with a fluorescent dye and tested onmore » Jurkat or HEK293 cells. The nano-sized particles were rapidly internalized and exhibited cytoplasmic localization. Incubation of cells with SLP-Tyl resulted in a dose- and time-dependent cytostatic effect, and also caused moderate and delayed cytotoxicity. Tyloxapol solution or SLP-Tyl dispersion caused the detachment of HEK293 cells, a decrease in cell proliferation and alterations in cellular morphology. Cell cycle analysis revealed that, while the unfavourable effects of SLP-Tyl and Tyloxapol solution are similar initially, longer incubation results in partial recovery of cells incubated with the dispersion of SLP-Tyl, whereas the presence of Tyloxapol solution induces apoptotic cell death. These findings indicate that Tyloxapol is an unfavourable stabilizer of SLP used for intracellular delivery and reinforce the role of stabilizers in a design of SLP with minimal cytotoxic properties.« less

Computation of turbulence and dispersion of cork in the NETL riser

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jiradilok, Veeraya; Gidaspow, Dimitri; Breault, R.W.

The knowledge of dispersion coefficients is essential for reliable design of gasifiers. However, a literature review had shown that dispersion coefficients in fluidized beds differ by more than five orders of magnitude. This study presents a comparison of the computed axial solids dispersion coefficients for cork particles to the NETL riser cork data. The turbulence properties, the Reynolds stresses, the granular temperature spectra and the radial and axial gas and solids dispersion coefficients are computed. The standard kinetic theory model described in Gidaspow’s 1994 book, Multiphase Flow and Fluidization, Academic Press and the IIT and Fluent codes were used tomore » compute the measured axial solids volume fraction profiles for flow of cork particles in the NETL riser. The Johnson–Jackson boundary conditions were used. Standard drag correlations were used. This study shows that the computed solids volume fractions for the low flux flow are within the experimental error of those measured, using a two-dimensional model. At higher solids fluxes the simulated solids volume fractions are close to the experimental measurements, but deviate significantly at the top of the riser. This disagreement is due to use of simplified geometry in the two-dimensional simulation. There is a good agreement between the experiment and the three-dimensional simulation for a high flux condition. This study concludes that the axial and radial gas and solids dispersion coefficients in risers operating in the turbulent flow regime can be computed using a multiphase computational fluid dynamics model.« less

Enhanced bioavailability of sirolimus via preparation of solid dispersion nanoparticles using a supercritical antisolvent process

PubMed Central

Kim, Min-Soo; Kim, Jeong-Soo; Park, Hee Jun; Cho, Won Kyung; Cha, Kwang-Ho; Hwang, Sung-Joo

2011-01-01

Background The aim of this study was to improve the physicochemical properties and bioavailability of poorly water-soluble sirolimus via preparation of a solid dispersion of nanoparticles using a supercritical antisolvent (SAS) process. Methods First, excipients for enhancing the stability and solubility of sirolimus were screened. Second, using the SAS process, solid dispersions of sirolimus-polyvinylpyrrolidone (PVP) K30 nanoparticles were prepared with or without surfactants such as sodium lauryl sulfate (SLS), tocopheryl propylene glycol succinate, Sucroester 15, Gelucire 50/13, and Myrj 52. A mean particle size of approximately 250 nm was obtained for PVP K30-sirolimus nanoparticles. Solid state characterization, kinetic solubility, powder dissolution, stability, and pharmacokinetics were analyzed in rats. Results X-ray diffraction, differential scanning calorimetry, and high-pressure liquid chromatography indicated that sirolimus existed in an anhydrous amorphous form within a solid dispersion of nanoparticles and that no degradation occurred after SAS processing. The improved supersaturation and dissolution of sirolimus as a solid dispersion of nanoparticles appeared to be well correlated with enhanced bioavailability of oral sirolimus in rats. With oral administration of a solid dispersion of PVP K30-SLS-sirolimus nanoparticles, the peak concentration and AUC0→12h of sirolimus were increased by approximately 18.3-fold and 15.2-fold, respectively. Conclusion The results of this study suggest that preparation of PVP K30-sirolimus-surfactant nanoparticles using the SAS process may be a promising approach for improving the bioavailability of sirolimus. PMID:22162657

Self-Catalyzed CdTe Wires.

PubMed

Baines, Tom; Papageorgiou, Giorgos; Hutter, Oliver S; Bowen, Leon; Durose, Ken; Major, Jonathan D

2018-04-25

CdTe wires have been fabricated via a catalyst free method using the industrially scalable physical vapor deposition technique close space sublimation. Wire growth was shown to be highly dependent on surface roughness and deposition pressure, with only low roughness surfaces being capable of producing wires. Growth of wires is highly (111) oriented and is inferred to occur via a vapor-solid-solid growth mechanism, wherein a CdTe seed particle acts to template the growth. Such seed particles are visible as wire caps and have been characterized via energy dispersive X-ray analysis to establish they are single phase CdTe, hence validating the self-catalysation route. Cathodoluminescence analysis demonstrates that CdTe wires exhibited a much lower level of recombination when compared to a planar CdTe film, which is highly beneficial for semiconductor applications.

Spatial distribution of organic functional groups supported on mesoporous silica nanoparticles: A study by conventional and DNP-enhanced 29Si solid-state NMR

DOE PAGES

Kobayashi, Takeshi; Singappuli-Arachchige, Dilini; Wang, Zhuoran; ...

2016-12-23

Solid-state NMR spectroscopy, both conventional and dynamic nuclear polarization (DNP)-enhanced, was employed to study the spatial distribution of organic functional groups attached to the surface of mesoporous silica nanoparticles via co-condensation and grafting. The most revealing information was provided by DNP-enhanced two-dimensional 29Si– 29Si correlation measurements, which unambiguously showed that post-synthesis grafting leads to a more homogeneous dispersion of propyl and mercaptopropyl functionalities than co-condensation. Furthermore, during the anhydrous grafting process, the organosilane precursors do not self-condense and are unlikely to bond to the silica surface in close proximity (less than 4 Å) due to the limited availability of suitablymore » arranged hydroxyl groups.« less

Measurement of suspended solids in lakes and oceans using satellite remote sensing data

NASA Technical Reports Server (NTRS)

Sydor, M. (Principal Investigator)

1980-01-01

Using satellite remote sensing data to measure low concentrations of suspended solids in lakes and oceans requires careful evaluation of background signals from the atmosphere and the water surface. Typical background corrections for Lake Superior are presented and the spectral distribution of the residual radiance from three major categories of turbidity in the lake are determined. The results indicate that for large bodies of water, some general information on atmospheric scattering, water clarity, and the optical properties of suspended solids allows estimates of concentrations of suspended solids to within + or - 0.5 mg/L without using real time ground truth data. Under calibrated conditions the threshold detection level is 0.3 mg/L for the fine particulates dispersed throughout the lake and 1 mg/L for the highly light absorbing effluent from rivers. Comparisons of the minimum reflectance over the open lake areas with reflection from the highly absorbing tannin water from rivers provides a check on the clarity of the atmosphere and the excessive background scatter from the water surface.

Porosity and water activity effects on stability of crystalline β-carotene in freeze-dried solids.

PubMed

Harnkarnsujarit, Nathdanai; Charoenrein, Sanguansri; Roos, Yrjö H

2012-11-01

Stability of entrapped crystalline β-carotene as affected by water activity, solids microstructure, and composition of freeze-dried systems was investigated. Aliquots (1000 mm(3) , 20% w/w solids) of solutions of maltodextrins of various dextrose equivalents (M040:DE6, M100:DE11, and M250:DE25.5), M100-sugars (1:1 glucose, fructose and sucrose), and agar for gelation with dispersed β-carotene were frozen at -20, -40, or -80 °C and freeze-dried. Glass transition and α-relaxation temperatures were determined with differential scanning calorimetry and dynamic mechanical analysis, respectively. β-Carotene contents were monitored spectrophotometrically. In the glassy solids, pore microstructure had a major effect on β-carotene stability. Small pores with thin walls and large surface area allowed β-carotene exposure to oxygen which led to a higher loss, whereas structural collapse enhanced stability of β-carotene by decreasing exposure to oxygen. As water plasticized matrices, an increase in molecular mobility in the matrix enhanced β-carotene degradation. Stability of dispersed β-carotene was highest at around 0.2 a(w) , but decreasing structural relaxation times above the glass transition correlated well with the rate of β-carotene degradation at higher a(w) . Microstructure, a(w) , and component mobility are important factors in the control of stability of β-carotene in freeze-dried solids. β-Carotene expresses various nutritional benefits; however, it is sensitive to oxygen and the degradation contributes to loss of nutritional values as well as product color. To increase stability of β-carotene in freeze-dried foods, the amount of oxygen penetration need to be limited. The modification of freeze-dried food structures, for example, porosity and structural collapse, components, and humidity effectively enhance the stability of dispersed β-carotene in freeze-dried solids. © 2012 Institute of Food Technologists®

Comparison of spray drying, electroblowing and electrospinning for preparation of Eudragit E and itraconazole solid dispersions.

PubMed

Sóti, Péter Lajos; Bocz, Katalin; Pataki, Hajnalka; Eke, Zsuzsanna; Farkas, Attila; Verreck, Geert; Kiss, Éva; Fekete, Pál; Vigh, Tamás; Wagner, István; Nagy, Zsombor K; Marosi, György

2015-10-15

Three solvent based methods: spray drying (SD), electrospinning (ES) and air-assisted electrospinning (electroblowing; EB) were used to prepare solid dispersions of itraconazole and Eudragit E. Samples with the same API/polymer ratios were prepared in order to make the three technologies comparable. The structure and morphology of solid dispersions were identified by scanning electron microscopy and solid phase analytical methods such as, X-ray powder diffraction (XRPD), differential scanning calorimetry (DSC) and Raman chemical mapping. Moreover, the residual organic solvents of the solid products were determined by static headspace-gas chromatography/mass spectroscopy measurements and the wettability of samples was characterized by contact angle measurement. The pharmaceutical performance of the three dispersion type, evaluated by dissolution tests, proved to be very similar. According to XRPD and DSC analyses, made after the production, all the solid dispersions were free of any API crystal clusters but about 10 wt% drug crystallinity was observed after three months of storage in the case of the SD samples in contrast to the samples produced by ES and EB in which the polymer matrix preserved the API in amorphous state. Copyright © 2015 Elsevier B.V. All rights reserved.

Roughness topographical effects on mean momentum and stress budgets in developed turbulent channel flows

NASA Astrophysics Data System (ADS)

Aghaei Jouybari, Mostafa; Yuan, Junlin

2017-11-01

Direct numerical simulations of turbulent channel flows are carried out over two surfaces: a synthesized sand-grain surface and a realistic turbine roughness that is characterized by more prominent large-scale surface features. To separate the effects of wall-normal variation of the roughness area fraction from the (true) variation of flow statistics, the governing equations are area-averaged using intrinsic averaging, contrary to the usually practice based on the total area (i.e., superficial averaging). Additional terms appear in the mean-momentum equation resulted from the wall-normal variation of the solid fraction and play a role in the near-wall balance. Results from surfaces with a step solidity function (e.g., cubes) will also be discussed. Compared to the sand grains, the turbine surface generates stronger form-induced fluctuations, despite weaker dispersive shear stress. This is associated with more significant form-induced productions (comparable to shear production) in Reynolds stress budgets, weaker pressure work, and, consequently, more anisotropic redistribution of turbulent kinetic energy in the roughness sublayer, which potentially leads to different turbulent responses between the two surfaces in non-equilibrium flows.

Pharmaceutical Dispersion Techniques for Dissolution and Bioavailability Enhancement of Poorly Water-Soluble Drugs.

PubMed

Zhang, Xingwang; Xing, Huijie; Zhao, Yue; Ma, Zhiguo

2018-06-23

Over the past decades, a large number of drugs as well as drug candidates with poor dissolution characteristics have been witnessed, which invokes great interest in enabling formulation of these active ingredients. Poorly water-soluble drugs, especially biopharmaceutical classification system (BCS) II ones, are preferably designed as oral dosage forms if the dissolution limit can be broken through. Minimizing a drug’s size is an effective means to increase its dissolution and hence the bioavailability, which can be achieved by specialized dispersion techniques. This article reviews the most commonly used dispersion techniques for pharmaceutical processing that can practically enhance the dissolution and bioavailability of poorly water-soluble drugs. Major interests focus on solid dispersion, lipid-based dispersion (nanoencapsulation), and liquisolid dispersion (drug solubilized in a non-volatile solvent and dispersed in suitable solid excipients for tableting or capsulizing), covering the formulation development, preparative technique and potential applications for oral drug delivery. Otherwise, some other techniques that can increase the dispersibility of a drug such as co-precipitation, concomitant crystallization and inclusion complexation are also discussed. Various dispersion techniques provide a productive platform for addressing the formulation challenge of poorly water-soluble drugs. Solid dispersion and liquisolid dispersion are most likely to be successful in developing oral dosage forms. Lipid-based dispersion represents a promising approach to surmounting the bioavailability of low-permeable drugs, though the technique needs to traverse the obstacle from liquid to solid transformation. Novel dispersion techniques are highly encouraged to develop for formulation of poorly water-soluble drugs.

Spectral modification of seismic waves propagating through solids exhibiting a resonance frequency: a 1-D coupled wave propagation-oscillation model

NASA Astrophysics Data System (ADS)

Frehner, Marcel; Schmalholz, Stefan M.; Podladchikov, Yuri

2009-02-01

A 1-D model is presented that couples the microscale oscillations of non-wetting fluid blobs in a partially saturated poroelastic medium with the macroscale wave propagation through the elastic skeleton. The fluid oscillations are caused by surface tension forces that act as the restoring forces driving the oscillations. The oscillations are described mathematically with the equation for a linear oscillator and the wave propagation is described with the 1-D elastic wave equation. Coupling is done using Hamilton's variational principle for continuous systems. The resulting linear system of two partial differential equations is solved numerically with explicit finite differences. Numerical simulations are used to analyse the effect of solids exhibiting internal oscillations, and consequently a resonance frequency, on seismic waves propagating through such media. The phase velocity dispersion relation shows a higher phase velocity in the high-frequency limit and a lower phase velocity in the low-frequency limit. At the resonance frequency a singularity in the dispersion relation occurs. Seismic waves can initiate oscillations of the fluid by transferring energy from solid to fluid at the resonance frequency. Due to this transfer, the spectral amplitude of the solid particle velocity decreases at the resonance frequency. After initiation, the oscillatory movement of the fluid continuously transfers energy at the resonance frequency back to the solid. Therefore, the spectral amplitude of the solid particle velocity is increased at the resonance frequency. Once initiated, fluid oscillations decrease in amplitude with increasing time. Consequently, the spectral peak of the solid particle velocity at the resonance frequency decreases with time.

Improvement of the dissolution rate of artemisinin by means of supercritical fluid technology and solid dispersions.

PubMed

Van Nijlen, T; Brennan, K; Van den Mooter, G; Blaton, N; Kinget, R; Augustijns, P

2003-03-26

The purpose of this study was to enhance the dissolution rate of artemisinin in order to improve the intestinal absorption characteristics. The effect of: (1) micronisation and (2) formation of solid dispersions with PVPK25 was assessed in an in vitro dissolution system [dissolution medium: water (90%), ethanol (10%) and sodium lauryl sulphate (0.1%)]. Coulter counter analysis was used to measure particle size. X-ray diffraction and DSC were used to analyse the physical state of the powders. Micronisation by means of a jet mill and supercritical fluid technology resulted in a significant decrease in particle size as compared to untreated artemisinin. All powders appeared to be crystalline. The dissolution rate of the micronised forms improved in comparison to the untreated form, but showed no difference in comparison to mechanically ground artemisinin. Solid dispersions of artemisinin with PVPK25 as a carrier were prepared by the solvent method. Both X-ray diffraction and DSC showed that the amorphous state was reached when the amount of PVPK25 was increased to 67%. The dissolution rate of solid dispersions with at least 67% of PVPK25 was significantly improved in comparison to untreated and mechanically ground artemisinin. Modulation of the dissolution rate of artemisinin was obtained by both particle size reduction and formation of solid dispersions. The effect of particle size reduction on the dissolution rate was limited. Solid dispersions could be prepared by using a relatively small amount of PVPK25. The formation of solid dispersions with PVPK25 as a carrier appears to be a promising method to improve the intestinal absorption characteristics of artemisinin. Copyright 2003 Elsevier Science B.V.

Harvesting of Scenedesmus obliquus FSP-3 using dispersed ozone flotation.

PubMed

Cheng, Ya-Ling; Juang, Yu-Chuan; Liao, Guan-Yu; Tsai, Pei-Wen; Ho, Shih-Hsin; Yeh, Kuei-Ling; Chen, Chun-Yen; Chang, Jo-Shu; Liu, Jhy-Chern; Chen, Wen-Ming; Lee, Duu-Jong

2011-01-01

The Scenedesmus obliquus FSP-3, a species with excellent potential for CO(2) capture and lipid production, was harvested using dispersed ozone flotation. While air aeration does not, ozone produces effective solid-liquid separation through flotation. Ozone dose applied for sufficient algal flotation is similar to those used in practical drinking waterworks. The algae removal rate, surface charge, and hydrophobicity of algal cells, and fluorescence characteristics and proteins and polysaccharides contents of algogenic organic matter (AOM) were determined during ozonation. Proteins released from tightly bound AOM are essential to modifying the hydrophobicity of bubble surfaces for easy cell attachment and to forming a top froth layer for collecting floating cells. Humic substances in the suspension scavenge dosed ozone that adversely affects ozone flotation efficiency of algal cells. Copyright © 2010 Elsevier Ltd. All rights reserved.

A comparative study of the effect of spray drying and hot-melt extrusion on the properties of amorphous solid dispersions containing felodipine.

PubMed

Mahmah, Osama; Tabbakh, Rami; Kelly, Adrian; Paradkar, Anant

2014-02-01

To compare the properties of solid dispersions of felodipine for oral bioavailability enhancement using two different polymers, polyvinylpyrrolidone (PVP) and hydroxypropyl methylcellulose acetate succinate (HPMCAS), by hot-melt extrusion (HME) and spray drying. Felodipine solid dispersions were prepared by HME and spray drying techniques. PVP and HPMCAS were used as polymer matrices at different drug : polymer ratios (1 : 1, 1 : 2 and 1 : 3). Detailed characterization was performed using differential scanning calorimetry, powder X-ray diffractometry, scanning electron microscopy and in-vitro dissolution testing. Dissolution profiles were evaluated in the presence of sodium dodecyl sulphate. Stability of different solid dispersions was studied under accelerated conditions (40°C/75% RH) over 8 weeks. Spray-dried formulations were found to release felodipine faster than melt extruded formulations for both polymer matrices. Solid dispersions containing HMPCAS exhibited higher drug release rates and better wettability than those produced with a PVP matrix. No significant differences in stability were observed except with HPMCAS at a 1 : 1 ratio, where crystallization was detected in spray-dried formulations. Solid dispersions of felodipine produced by spray drying exhibited more rapid drug release than corresponding melt extruded formulations, although in some cases improved stability was observed for melt extruded formulations. © 2013 Royal Pharmaceutical Society.

Study on Enhanced Dissolution of Azilsartan-Loaded Solid Dispersion, Prepared by Combining Wet Milling and Spray-Drying Technologies.

PubMed

Lu, Tianshu; Sun, Yinghua; Ding, Dawei; Zhang, Qi; Fan, Rui; He, Zhonggui; Wang, Jing

2017-02-01

The purpose of this study was to develop a combination method of wet milling and spray-drying technologies to prepare the solid dispersion and improve the dissolution rate of poorly water-soluble drug candidates. Azilsartan (AZL) was selected as the model drug for its poor water solubility. In the study, AZL-loaded solid dispersion was prepared with polyethylene glycol 6000 (PEG6000) and hydroxypropyl cellulose with super low viscosity (HPC-SL) as stabilizers by using combination of wet grinding and spray-drying methods. The high AZL loading solid dispersion was then characterized by scanning electron microscopy (SEM), differential scanning calorimetry (DSC), powder X-ray diffraction (PXRD), and Fourier transform infrared spectroscopy (FTIR). Besides, dissolution test was carried out by the paddle method and stability investigation was also conducted. As a result, the dissolution rate of the solid dispersion tablets was found to be greater than conventional tablets, but in close agreement with market tablets. Furthermore, the formulation was shown to be stable at 40 ± 2°C and 75 ± 5% for at least 6 months, owing to its decreased particle size, morphology, and its crystal form. It was concluded that the combination of wet milling and spray-drying approaches to prepare solid dispersion would be a prospective method to improve the dissolution rate of poorly water-soluble drugs.

Solid dispersions of Myricetin with enhanced solubility: Formulation, characterization and crystal structure of stability-impeding Myricetin monohydrate crystals

NASA Astrophysics Data System (ADS)

Mureşan-Pop, M.; Pop, M. M.; Borodi, G.; Todea, M.; Nagy-Simon, T.; Simon, S.

2017-08-01

Three solid dispersion forms of Myricetin combined with the Polyvinylpyrrolidone were successfully prepared by spray drying method, and characterized by X-ray powder diffraction, thermal analysis, infrared spectroscopy and optical microscopy. Zeta potential measurements provided indications on solid dispersions stability in aqueous suspension related to their storage at elevated temperature and relative humidity, which depends on the Myricetin load. By increase of Myricetin load, the stability of the solid dispersion is impeded due to growth of Myricetin monohydrate crystals. The amorphous dispersions with 10% and 50% Myricetin load are stable and, compared to pure Myricetin, their aqueous solubility is enhanced by a factor of 47 and 13, respectively. The dispersion with 80% Myricetin load is unstable on storage, and this behavior acts in conjunction with the development of Myricetin monohydrate crystals. Single-crystal X-ray diffraction results obtained for Myricetin monohydrate reveal a structure of an infinite 2D network of hydrogen-bonded molecules involving all six hydroxyl groups of Myricetin. The water molecules are positioned in between the infinite chains, and contribute via H-bonds to robust crystal packing. The calculated needle-like morphology of monohydrate form is in agreement with the optical microscopy results. The study shows that the solid amorphous dispersions with up to 50% Myricetin load are a viable option for achieving substantial solubility improvement of Myricetin, and supports their potential use in pharmaceutical applications.

Investigation into mixing capability and solid dispersion preparation using the DSM Xplore Pharma Micro Extruder.

PubMed

Sakai, Toshiro; Thommes, Markus

2014-02-01

The goal of this investigation was to qualify the DSM Xplore Pharma Micro Extruder as a formulation screening tool for early-stage hot-melt extrusion. Dispersive and distributive mixing was investigated using soluplus, copovidone or basic butylated methacrylate copolymer with sodium chloride (NaCl) in a batch size of 5 g. Eleven types of solid dispersions were prepared using various drugs and carriers in batches of 5 g in accordance with the literature. The dispersive mixing was a function of screw speed and recirculation time and the particle size was remarkably reduced after 1 min of processing, regardless of the polymers. An inverse relationship between the particle size and specific mechanical energy (SME) was also found. The SME values were higher than those in large-scale extruders. After 1 min recirculation at 200 rpm, the uniformity of NaCl content met the criteria of the European Pharmacopoeia, indicating that distributive mixing was achieved in this time. For the solid dispersions preparations, the results from different scanning calorimetry, powder X-ray diffractometry and in-vitro dissolution tests confirmed that all solid-dispersion systems were successfully prepared. These findings demonstrated that the extruder is a useful tool to screen solid-dispersion formulations and their material properties on a small scale. © 2013 Royal Pharmaceutical Society.

Evaluation of the organization of the homoionic smectite layers (Na(+) or Ca(2+)) in diluted dispersions using granulometry, microscopy and rheometry.

PubMed

Paumier, S; Pantet, A; Monnet, P

2008-09-01

Smectites are swelling clay materials with pronounced colloidal properties that are widely used in industry. These properties originate in the electrokinetic properties of the smectite layers and their linkage capacities. Thin layers may be dispersed or aggregated according to many parameters, such as concentration, particle size and morphology, exchangeable cation nature and chemical environment (pH, ionic strength). The literature usually provides general rules, like the sodium dispersion contains a lot of small units whereas the calcium dispersion contains a few large units. A volume of water molecules bound to the clay surface is considered as the immobile water phase that behaves like the solid phase obstructing the flow. The water immobilized around layers and trapped inside aggregates cannot participate to the flow. In this study, we evaluated the volume occupied by calcium and sodium units inside the dispersion containing the immobile water phase. First, the smectite was cautiously extracted from a raw bentonite and its physicochemical properties were determined. A large quantity of extracted and saturated smectite (Na-smectite and Ca-smectite) was obtained. Second, the unit size and a shape factor for each sample were evaluated using granulometry and scanning transmission electron microscopy on wet samples (Wet STEM) and some flow curves. Na-smectite dispersions contain 0.13 microm(2) surface units with a shape factor of 50. Ca-smectite dispersions contain 0.32 microm(2) surface units with a shape factor of 3.3. Finally, rheometry allowed us to evaluate the unit occupancy using an adaptation of the Krieger-Dougherty law. We used shape factors and evaluated the concentration from which the entire immobile volume was connected (6.4% for Na-smectite and 11.9% for Ca-smectite). This study explains the evolution of flow properties with increasing concentrations by the evolution of layer interactions at the microscopic scale for homoionic smectite particles in diluted dispersions.

High performance discharges in the Lithium Tokamak eXperiment with liquid lithium walls

DOE PAGES

Schmitt, J. C.; Bell, R. E.; Boyle, D. P.; ...

2015-05-15

The first-ever successful operation of a tokamak with a large area (40% of the total plasma surface area) liquid lithium wall has been achieved in the Lithium Tokamak eXperiment (LTX). These results were obtained with a new, electron beam-based lithium evaporation system, which can deposit a lithium coating on the limiting wall of LTX in a five-minute period. Preliminary analyses of diamagnetic and other data for discharges operated with a liquid lithium wall indicate that confinement times increased by 10 x compared to discharges with helium-dispersed solid lithium coatings. Ohmic energy confinement times with fresh lithium walls, solid and liquid,more » exceed several relevant empirical scaling expressions. Spectroscopic analysis of the discharges indicates that oxygen levels in the discharges limited on liquid lithium walls were significantly reduced compared to discharges limited on solid lithium walls. Finally, Tokamak operations with a full liquid lithium wall (85% of the total plasma surface area) have recently started.« less

Solid-State NMR Investigation of Drug-Excipient Interactions and Phase Behavior in Indomethacin-Eudragit E Amorphous Solid Dispersions.

PubMed

Lubach, Joseph W; Hau, Jonathan

2018-02-20

To investigate the nature of drug-excipient interactions between indomethacin (IMC) and methacrylate copolymer Eudragit® E (EE) in the amorphous state, and evaluate the effects on formulation and stability of these amorphous systems. Amorphous solid dispersions containing IMC and EE were spray dried with drug loadings from 20% to 90%. PXRD was used to confirm the amorphous nature of the dispersions, and DSC was used to measure glass transition temperatures (T g ). 13 C and 15 N solid-state NMR was utilized to investigate changes in local structure and protonation state, while 1 H T 1 and T 1ρ relaxation measurements were used to probe miscibility and phase behavior of the dispersions. T g values for IMC-EE solid dispersions showed significant positive deviations from predicted values in the drug loading range of 40-90%, indicating a relatively strong drug-excipient interaction. 15 N solid-state NMR exhibited a change in protonation state of the EE basic amine, with two distinct populations for the EE amine at -360.7 ppm (unprotonated) and -344.4 ppm (protonated). Additionally, 1 H relaxation measurements showed phase separation at high drug load, indicating an amorphous ionic complex and free IMC-rich phase. PXRD data showed all ASDs up to 90% drug load remained physically stable after 2 years. 15 N solid-state NMR experiments show a change in protonation state of EE, indicating that an ionic complex indeed forms between IMC and EE in amorphous solid dispersions. Phase behavior was determined to exhibit nanoscale phase separation at high drug load between the amorphous ionic complex and excess free IMC.

Effect of the morphology of adsorbed oleate on the wettability of a collophane surface

NASA Astrophysics Data System (ADS)

Ye, Junjian; Zhang, Qin; Li, Xianbo; Wang, Xianchen; Ke, Baolin; Li, Xianhai; Shen, Zhihui

2018-06-01

The adsorption of surfactants on a solid surface could alter its wettability, which offers a wide range of relevant applications such as mineral flotation, hydrophobic material preparation and nanomaterial dispersion. The morphology of adsorbed oleate on a collophane surface was visualized using the peakforce tapping mode of atomic force microscopy (AFM), and its effect on the wettability of collophane was analysed by contact angle measurements, adsorption measurements and molecular dynamics (MD) simulations. The AFM images demonstrated that the adsorbed structure varied with different oleate concentrations. First, the small cylindrical micelles with concomitant monolayer and bilayer structures were observed above the hemimicelle concentration (hmc) of 1 × 10-5 mol/L, which enhanced the hydrophobicity of the collophane surface, and the collophane surface was not completely covered with the oleate monolayer due to surface heterogeneity. Then, large cylindrical micelles with a major bilayer were formed as the critical micelle concentration (cmc) of 1 × 10-3 mol/L was approached, which decreased its hydrophobicity, and finally the formation of large cylindrical micelles with multilayer at the cmc caused the hydrophilicity of the collophane surface. Therefore, there was a suitable equilibrium concentration between the hmc and cmc for oleate as a collector during mineral flotation, and oleate could also be used as a dispersant for colloidal stability when its equilibrium concentration reached the cmc. The effect of the adsorbed structure on the wettability of collophane was also confirmed by MD simulations. This study provides a good understanding of the surface modification of particles by surfactants for flotation and dispersion applications.

Stability of aggregates in the environment: role of solid bridging

NASA Astrophysics Data System (ADS)

Seiphoori, A.; Jerolmack, D. J.; Arratia, P. E.

2017-12-01

Colloids in suspension may form larger flocs under favorable conditions, via diffusion- or reaction-limited aggregation. In addition, the process of drying colloidal suspensions drives colloids together via hydrodynamic forces to form aggregates, that may be stable or unstable when subject to re-wetting and transport. Channel banks, shorelines and hillslopes are examples where the periodic wetting and drying results in the aggregation of muds. If aggregates disperse, the mud structure is unstable to subsequent wetting or fluid shear and can easily be detached and transported to rivers and coasts. The effective friction that governs hillslope and channel-bank soil creep rates also depends on the stability of the soil aggregates. Yet, few studies probe the particle-scale assembly or stability of aggregates subject to environmental loads, and the effects of shape or size heterogeneity have not been examined in detail. Here we investigate the formation and stability of aggregates subject to passive re-wetting (by misting) and shearing using a simple Poiseuille flow in a microfluidic device. We study the kinetics of a wide range of silicate colloids of different size and surface charge properties using in situ microscopy and particle tracking. We find that negatively charged silica microspheres are dragged by the retreating edge of an evaporating drop and are resuspended easily on re-wetting, showing that aggregates are unstable. In contrast, a bi-disperse suspension created by the addition of silica nanoparticles forms stable deposits, where nanoparticles bind larger particles by bridging the interparticle space, a mechanism similar to capillary bridging that we refer to as "solid bridging." Although aggregate structure and dynamics of the bi-disperse system changes quantitatively with surface-charge of the nanoparticles, smaller particles always conferred stability on the aggregates. Investigation of other colloids, including asbestos fibers and various clays, reveals that this solid bridging effect is robust across variations in particle shape and material composition. These experiments suggest that natural mud and soil may form more stable aggregates than would naively be expected by considering the charge effects alone, because their inherent size heterogeneity is conducive to solid bridging.

Investigating the effect of moisture protection on solid-state stability and dissolution of fenofibrate and ketoconazole solid dispersions using PXRD, HSDSC and Raman microscopy.

PubMed

Kanaujia, Parijat; Lau, Grace; Ng, Wai Kiong; Widjaja, Effendi; Schreyer, Martin; Hanefeld, Andrea; Fischbach, Matthias; Saal, Christoph; Maio, Mario; Tan, Reginald B H

2011-09-01

Enhanced dissolution of poorly soluble active pharmaceutical ingredients (APIs) in amorphous solid dispersions often diminishes during storage due to moisture-induced re-crystallization. This study aims to investigate the influence of moisture protection on solid-state stability and dissolution profiles of melt-extruded fenofibrate (FF) and ketoconazole (KC) solid dispersions. Samples were kept in open, closed and Activ-vials(®) to control the moisture uptake under accelerated conditions. During 13-week storage, changes in API crystallinity were quantified using powder X-ray diffraction (PXRD) (Rietveld analysis) and high sensitivity differential scanning calorimetry (HSDSC) and compared with any change in dissolution profiles. Trace crystallinity was observed by Raman microscopy, which otherwise was undetected by PXRD and HSDSC. Results showed that while moisture protection was ineffective in preventing the re-crystallization of amorphous FF, KC remained X-ray amorphous despite 5% moisture uptake. Regardless of the degree of crystallinity increase in FF, the enhanced dissolution properties were similarly diminished. Moisture uptake above 10% in KC samples also led to re-crystallization and significant decrease in dissolution rates. In conclusion, eliminating moisture sorption may not be sufficient in ensuring the stability of solid dispersions. Analytical quantification of API crystallinity is crucial in detecting subtle increase in crystallinity that can diminish the enhanced dissolution properties of solid dispersions.

Extending of flat normal dispersion profile in all-solid soft glass nonlinear photonic crystal fibres

NASA Astrophysics Data System (ADS)

Siwicki, Bartłomiej; Kasztelanic, Rafał; Klimczak, Mariusz; Cimek, Jarosław; Pysz, Dariusz; Stępień, Ryszard; Buczyński, Ryszard

2016-06-01

The bandwidth of coherent supercontinuum generated in optical fibres is strongly determined by the all-normal dispersion characteristic of the fibre. We investigate all-normal dispersion limitations in all-solid oxide-based soft glass photonic crystal fibres with various relative inclusion sizes and lattice constants. The influence of material dispersion on fibre dispersion characteristics for a selected pair of glasses is also examined. A relation between the material dispersion of the glasses and the fibre dispersion has been described. We determined the parameters which limit the maximum range of flattened all-normal dispersion profile achievable for the considered pair of heavy-metal-oxide soft glasses.

Inclusion of Ti and Zr species on clay surfaces and their effect on the interaction with organic molecules

NASA Astrophysics Data System (ADS)

Rangel-Rivera, Pedro; Bachiller-Baeza, María Belén; Galindo-Esquivel, Ignacio; Rangel-Porras, Gustavo

2018-07-01

The interactions between the clay surface and the organic molecules play an important role in the efficient of these materials in adsorption and catalytic processes. These materials are often modified with the inclusion of other catalytic particles for the purpose of enhancing the activity. In this study, commercial clay K10 was modified with the particles inclusion of titanium and zirconium. The solid surfaces were examined by infrared spectroscopy, scanning electron microscopy (SEM) coupled to an energy-dispersive X-ray spectroscopy device (EDS), and X-ray photoelectron spectroscopy (XPS). Temperature programmed desorption of ammonia (TPD-NH3) and propan-2-ol decomposition test reaction were performed to probe the acid properties. The adsorption of acetic acid, ethanol, and propan-2-ol on the surface of each solid and their thermal stability were studied by diffuse reflectance infrared Fourier transform spectroscopy (DRIFT). Finally, these materials were used in the esterification of acetic acid with penta-1-ol. The real effect over the incorporation of titanium species and zirconium species on clay surface for interacting with the organic molecules was discussed.

Extending the applicability of the Tkatchenko-Scheffler dispersion correction via iterative Hirshfeld partitioning

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bučko, Tomáš, E-mail: bucko@fns.uniba.sk; Department of Computational Materials Physics, Fakultät für Physik and Center for Computational Materials Science, Universität Wien, Sensengasse, Wien 1090; Lebègue, Sébastien, E-mail: sebastien.lebegue@univ-lorraine.fr

2014-07-21

Recently we have demonstrated that the applicability of the Tkatchenko-Scheffler (TS) method for calculating dispersion corrections to density-functional theory can be extended to ionic systems if the Hirshfeld method for estimating effective volumes and charges of atoms in molecules or solids (AIM’s) is replaced by its iterative variant [T. Bučko, S. Lebègue, J. Hafner, and J. Ángyán, J. Chem. Theory Comput. 9, 4293 (2013)]. The standard Hirshfeld method uses neutral atoms as a reference, whereas in the iterative Hirshfeld (HI) scheme the fractionally charged atomic reference states are determined self-consistently. We show that the HI method predicts more realistic AIMmore » charges and that the TS/HI approach leads to polarizabilities and C{sub 6} dispersion coefficients in ionic or partially ionic systems which are, as expected, larger for anions than for cations (in contrast to the conventional TS method). For crystalline materials, the new algorithm predicts polarizabilities per unit cell in better agreement with the values derived from the Clausius-Mosotti equation. The applicability of the TS/HI method has been tested for a wide variety of molecular and solid-state systems. It is demonstrated that for systems dominated by covalent interactions and/or dispersion forces the TS/HI method leads to the same results as the conventional TS approach. The difference between the TS/HI and TS approaches increases with increasing ionicity. A detailed comparison is presented for isoelectronic series of octet compounds, layered crystals, complex intermetallic compounds, and hydrides, and for crystals built of molecules or containing molecular anions. It is demonstrated that only the TS/HI method leads to accurate results for systems where both electrostatic and dispersion interactions are important, as illustrated for Li-intercalated graphite and for molecular adsorption on the surfaces in ionic solids and in the cavities of zeolites.« less

Comparative Plasma Exposure of Albendazole after Administration of Rapidly Disintegrating Tablets in Dogs

PubMed Central

Castro, Silvina G.; Dib, Alicia; Suarez, Gonzalo; Allemandi, Daniel; Lanusse, Carlos; Sanchez Bruni, Sergio; Palma, Santiago D.

2013-01-01

The main objectives of this study were (a) to evaluate the in vitro performance of the rapid disintegration tablets as a way to improve the solid dispersions and (b) to study the in vivo pharmacokinetics of the albendazole modified formulation in dogs. Rapid disintegration of tablets seems to be a key factor for efficiency of solid dispersions with regard to improvement of the albendazole bioavailability. The in vivo assays performed on dogs showed a marked increase in drug plasma exposure when albendazole was given in solid dispersions incorporated into rapid disintegration tablets compared with conventional solid dosage form. PMID:24063016

The effect of solute additions on the steady-state creep behavior of dispersion-strengthened aluminum.

NASA Technical Reports Server (NTRS)

Reynolds, G. H.; Lenel, F. V.; Ansell, G. S.

1971-01-01

The effect of solute additions on the steady-state creep behavior of coarse-grained dispersion-strengthened aluminum alloys was studied. Recrystallized dispersion-strengthened solid solutions were found to have stress and temperature sensitivities quite unlike those observed in single-phase solid solutions having the same composition and grain size. The addition of magnesium or copper to the matrix of a recrystallized dispersion-strengthened aluminum causes a decrease in the steady-state creep rate which is much smaller than that caused by similar amounts of solute in single-phase solid solutions. All alloys exhibited essentially a 4.0 power stress exponent in agreement with the model of Ansell and Weertman. The activation energy for steady-state creep in dispersion-strengthened Al-Mg alloys, as well as the stress dependence, was in agreement with the physical model of dislocation climb over the dispersed particles.

Preparation and characterization of solid dispersion freeze-dried efavirenz - polyvinylpyrrolidone K-30.

PubMed

Fitriani, Lili; Haqi, Alianshar; Zaini, Erizal

2016-01-01

The aim of this research is to prepare and characterize solid dispersion of efavirenz - polyvinylpyrrolidone (PVP) K-30 by freeze drying to increase its solubility. Solid dispersion of efavirenz - PVP K-30 was prepared by solvent evaporation method with ratio 2:1, 1:1, and 1:2 and dried using a freeze dryer. Characterizations were done by scanning electron microscopy (SEM), powder X-ray diffraction analysis, differential thermal analysis (DTA), and Fourier transform infrared (FT-IR) spectroscopy. Solubility test was carried out in CO2-free distilled water, and efavirenz assay was conducted using high-performance liquid chromatography with acetonitrile:acetic acid (80:20) as the mobile phases. Powder X-ray diffractogram showed a decrease in the peak intensity, which indicated the crystalline altered to amorphous phase. DTA thermal analysis showed a decrease in the melting point of the solid dispersion compared to intact efavirenz. SEM results indicated the changes in the morphology of the crystal into an amorphous form compared to pure components. FT-IR spectroscopy analysis showed a shift wavenumber of the spectrum efavirenz and PVP K-30. The solubility of solid dispersion at ratio 2:1, 1:1, and 1:2 was 6.777 μg/mL, 6.936 μg/mL, and 14,672 μg/mL, respectively, whereas the solubility of intact efavirenz was 0.250 μg/mL. In conclusion, the solubility of solid dispersion increased significantly (P < 0.05).

Biomimetic Dissolution: A Tool to Predict Amorphous Solid Dispersion Performance.

PubMed

Puppolo, Michael M; Hughey, Justin R; Dillon, Traciann; Storey, David; Jansen-Varnum, Susan

2017-11-01

The presented study describes the development of a membrane permeation non-sink dissolution method that can provide analysis of complete drug speciation and emulate the in vivo performance of poorly water-soluble Biopharmaceutical Classification System class II compounds. The designed membrane permeation methodology permits evaluation of free/dissolved/unbound drug from amorphous solid dispersion formulations with the use of a two-cell apparatus, biorelevant dissolution media, and a biomimetic polymer membrane. It offers insight into oral drug dissolution, permeation, and absorption. Amorphous solid dispersions of felodipine were prepared by hot melt extrusion and spray drying techniques and evaluated for in vitro performance. Prior to ranking performance of extruded and spray-dried felodipine solid dispersions, optimization of the dissolution methodology was performed for parameters such as agitation rate, membrane type, and membrane pore size. The particle size and zeta potential were analyzed during dissolution experiments to understand drug/polymer speciation and supersaturation sustainment of felodipine solid dispersions. Bland-Altman analysis was performed to measure the agreement or equivalence between dissolution profiles acquired using polymer membranes and porcine intestines and to establish the biomimetic nature of the treated polymer membranes. The utility of the membrane permeation dissolution methodology is seen during the evaluation of felodipine solid dispersions produced by spray drying and hot melt extrusion. The membrane permeation dissolution methodology can suggest formulation performance and be employed as a screening tool for selection of candidates to move forward to pharmacokinetic studies. Furthermore, the presented model is a cost-effective technique.

Development of novel fast-dissolving tacrolimus solid dispersion-loaded prolonged release tablet.

PubMed

Cho, Jung Hyun; Kim, Yong-Il; Kim, Dong-Wuk; Yousaf, Abid Mehmood; Kim, Jong Oh; Woo, Jong Soo; Yong, Chul Soon; Choi, Han-Gon

2014-04-11

The goal of this research was to develop a novel prolonged release tablet bioequivalent to the commercial sustained release capsule. A number of tacrolimus-loaded fast-dissolving solid dispersions containing various amounts of DOSS were prepared using the spray drying technique. Their solubility, dissolution and pharmacokinetics in rats were studied. DOSS increased drug solubility and dissolution in the solid dispersions. Compared with the drug powder, the solubility, dissolution and bioavailability of tacrolimus with the fast-dissolving solid dispersion containing tacrolimus/HP-β-CD/DOSS in the weight ratio of 5:40:4 were boosted by approximately 700-, 30- and 2-fold, respectively. Several tablet formulations were accomplished with this solid dispersion in combination with various ratios of HPMC/ethylcellulose. The release behaviour and pharmacokinetic studies in beagle dogs were assessed compared with the commercial prolonged release capsule. A decrease in HPMC/ethylcellulose ratios reduced the dissolution of tacrolimus from the tablets. Particularly, the tacrolimus-loaded prolonged release tablet consisting of fast-dissolving tacrolimus solid dispersion, HPMC, ethylcellulose and talc at the weight ratio of 20:66:112:2 exhibited a dissolution profile similar to that produced by the commercial prolonged release capsule. Furthermore, there were no significant differences in the AUC, Cmax, Tmax and MRT values between them in beagle dogs. Consequently, this tacrolimus-loaded prolonged release tablet might be bioequivalent to the tacrolimus-loaded commercial capsule. Copyright © 2013 Elsevier B.V. All rights reserved.

Melt extrusion vs. spray drying: The effect of processing methods on crystalline content of naproxen-povidone formulations.

PubMed

Haser, Abbe; Cao, Tu; Lubach, Joe; Listro, Tony; Acquarulo, Larry; Zhang, Feng

2017-05-01

Our hypothesis is that melt extrusion is a more suitable processing method than spray drying to prepare amorphous solid dispersions of drugs with a high crystallization tendency. Naproxen-povidone K25 was used as the model system in this study. Naproxen-povidone K25 solid dispersions at 30% and 60% drug loadings were characterized by modulated DSC, powder X-ray diffraction, FT-IR, and solid-state 13 C NMR to identify phase separation and drug recrystallization during processing and storage. At 30% drug loading, hydrogen bond (H-bond) sites of povidone K25 were not saturated and the glass transition (T g ) temperature of the formulation was higher. As a result, both melt-extruded and spray-dried materials were amorphous initially and remained so after storage at 40°C. At 60% drug loading, H-bond sites were saturated, and T g was low. We were not able to prepare amorphous materials. The initial crystallinity of the formulations was 0.4%±0.2% and 5.6%±0.6%, and increased to 2.7%±0.3% and 21.6%±1.0% for melt-extruded and spray-dried materials, respectively. Spray-dried material was more susceptible to re-crystallization during processing, due to the high diffusivity of naproxen molecules in the formulation matrix and lack of kinetic stabilization from polymer solution. A larger number of crystalline nucleation sites and high surface area made the spray-dried material more susceptible to recrystallization during storage. This study demonstrated the unique advantages of melt extrusion over spray drying for the preparation of amorphous solid dispersions of naproxen at high drug level. Copyright © 2017 Elsevier B.V. All rights reserved.

POTENTIAL FOR NITROSAMINE FORMATION RESULTING FROM THE USE OF RHODAMINE WT FOR TIME-OF-TRAVEL STUDIES: A COMBINED LABORATORY AND FIELD INVESTIGATION.

USGS Publications Warehouse

Johnson, Sharon M.; Steinheimer, Thomas R.

1984-01-01

Rhodamine WT is used by surface water hydrologists for time of travel and dispersion studies in which flow characteristics of surface streams are determined. Surface water contamination by nitrosamines formed from Rhodamine WT and nitrite ion has been studied. A method for residue analysis of N-nitrosodiethylamine (NDEA) has been developed and evaluated using river samples spiked with Rhodamine WT and nitrite ion. It permits rapid and reliable determination of NDEA at a minimum concentration of 0. 03 mu g/L. The method uses solid-phase extraction and capillary gas chromatography.

Pseudospectral modeling and dispersion analysis of Rayleigh waves in viscoelastic media

USGS Publications Warehouse

Zhang, K.; Luo, Y.; Xia, J.; Chen, C.

2011-01-01

Multichannel Analysis of Surface Waves (MASW) is one of the most widely used techniques in environmental and engineering geophysics to determine shear-wave velocities and dynamic properties, which is based on the elastic layered system theory. Wave propagation in the Earth, however, has been recognized as viscoelastic and the propagation of Rayleigh waves presents substantial differences in viscoelastic media as compared with elastic media. Therefore, it is necessary to carry out numerical simulation and dispersion analysis of Rayleigh waves in viscoelastic media to better understand Rayleigh-wave behaviors in the real world. We apply a pseudospectral method to the calculation of the spatial derivatives using a Chebyshev difference operator in the vertical direction and a Fourier difference operator in the horizontal direction based on the velocity-stress elastodynamic equations and relations of linear viscoelastic solids. This approach stretches the spatial discrete grid to have a minimum grid size near the free surface so that high accuracy and resolution are achieved at the free surface, which allows an effective incorporation of the free surface boundary conditions since the Chebyshev method is nonperiodic. We first use an elastic homogeneous half-space model to demonstrate the accuracy of the pseudospectral method comparing with the analytical solution, and verify the correctness of the numerical modeling results for a viscoelastic half-space comparing the phase velocities of Rayleigh wave between the theoretical values and the dispersive image generated by high-resolution linear Radon transform. We then simulate three types of two-layer models to analyze dispersive-energy characteristics for near-surface applications. Results demonstrate that the phase velocity of Rayleigh waves in viscoelastic media is relatively higher than in elastic media and the fundamental mode increases by 10-16% when the frequency is above 10. Hz due to the velocity dispersion of P and S waves. ?? 2011 Elsevier Ltd.

Structural characterization of the phospholipid stabilizer layer at the solid-liquid interface of dispersed triglyceride nanocrystals with small-angle x-ray and neutron scattering

NASA Astrophysics Data System (ADS)

Schmiele, Martin; Schindler, Torben; Unruh, Tobias; Busch, Sebastian; Morhenn, Humphrey; Westermann, Martin; Steiniger, Frank; Radulescu, Aurel; Lindner, Peter; Schweins, Ralf; Boesecke, Peter

2013-06-01

Dispersions of crystalline nanoparticles with at least one sufficiently large unit cell dimension can give rise to Bragg reflections in the small-angle scattering range. If the nanocrystals possess only a small number of unit cells along these particular crystallographic directions, the corresponding Bragg reflections will be broadened. In a previous study of phospholipid stabilized dispersions of β-tripalmitin platelets [Unruh, J. Appl. Crystallogr.JACGAR0021-889810.1107/S0021889807044378 40, 1008 (2007)], the x-ray powder pattern simulation analysis (XPPSA) was developed. The XPPSA method facilitates the interpretation of the rather complicated small-angle x-ray scattering (SAXS) curves of such dispersions of nanocrystals. The XPPSA method yields the distribution function of the platelet thicknesses and facilitates a structural characterization of the phospholipid stabilizer layer at the solid-liquid interface between the nanocrystals and the dispersion medium from the shape of the broadened 001 Bragg reflection. In this contribution an improved and extended version of the XPPSA method is presented. The SAXS and small-angle neutron scattering patterns of dilute phospholipid stabilized tripalmitin dispersions can be reproduced on the basis of a consistent simulation model for the particles and their phospholipid stabilizer layer on an absolute scale. The results indicate a surprisingly flat arrangement of the phospholipid molecules in the stabilizer layer with a total thickness of only 12 Å. The stabilizer layer can be modeled by an inner shell for the fatty acid chains and an outer shell including the head groups and additional water. The experiments support a dense packing of the phospholipid molecules on the nanocrystal surfaces rather than isolated phospholipid domains.

Development of solid dispersions of artemisinin for transdermal delivery.

PubMed

Shahzad, Yasser; Sohail, Sadia; Arshad, Muhammad Sohail; Hussain, Talib; Shah, Syed Nisar Hussain

2013-11-30

Solid dispersions of the poorly soluble drug artemisinin were developed using polymer blends of polyvinylpyrrolidone (PVP) and polyethylene glycol (PEG) with the aim of enhancing solubility and in vitro permeation of artemisinin through skin. Formulations were characterised using a combination of molecular dynamics (MD) simulations, differential scanning calorimetry (DSC), X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FT-IR). Solubility of artemisinin was determined in two solvents: de-ionised water and phosphate buffered saline (PBS; pH 7.4), while in vitro drug permeation studies were carried out using rabbit skin as a model membrane. MD simulations revealed miscibility between the drug and polymers. DSC confirmed the molecular dispersion of the drug in the polymer blend. Decrease in crystallinity of artemisinin with respect to polymer content and the absence of specific drug-polymer interactions were confirmed using XRD and FT-IR, respectively. The solubility of artemisinin was dramatically enhanced for the solid dispersions, as was the permeation of artemisinin from saturated solid-dispersion vehicles relative to that from saturated solutions of the pure drug. The study suggests that high energy solid forms of artemisinin could possibly enable transdermal delivery of artemisinin. Copyright © 2013 Elsevier B.V. All rights reserved.

Self-nanoemulsifying drug delivery system of nifedipine: impact of hydrophilic-lipophilic balance and molecular structure of mixed surfactants.

PubMed

Weerapol, Yotsanan; Limmatvapirat, Sontaya; Nunthanid, Jurairat; Sriamornsak, Pornsak

2014-04-01

A simple but novel mixed surfactant system was designed to fabricate a self-nanoemulsifying drug delivery system (SNEDDS) based on hydrophilic-lipophilic balance (HLB) value. The impacts of HLB and molecular structure of surfactants on the formation of SNEDDS were investigated. After screening various oils and surfactants, nifedipine (NDP)-loaded liquid SNEDDS was formulated with Imwitor(®) 742 as oil and Tween(®)/Span(®) or Cremophor(®)/Span(®) as mixed surfactant. Droplet size of the emulsions obtained after dispersing SNEDDS containing Tween(®)/Span(®) in aqueous medium was independent of the HLB of a mixed surfactant. The use of the Cremophor(®)/Span(®) blend gave nanosized emulsion at higher HLB. The structure of the surfactant was found to influence the emulsion droplet size. Solid SNEDDS was then prepared by adsorbing NDP-loaded liquid SNEDDS comprising Cremophor(®) RH40/Span(®) 80 onto Aerosil(®) 200 or Aerosil(®) R972 as inert solid carrier. Solid SNEDDS formulations using higher amounts (30-50% w/w) of Aerosil(®) 200 exhibited good flow properties with smooth surface and preserved the self-emulsifying properties of liquid SNEDDS. Differential scanning calorimetry and X-ray diffraction studies of solid SNEDDS revealed the transformation of the crystalline structure of NDP due to its molecular dispersion state. In vitro dissolution study demonstrated higher dissolution of NDP from solid SNEDDS compared with NDP powder.

Dispersoid reinforced alloy powder and method of making

DOEpatents

Anderson, Iver E; Terpstra, Robert L

2014-10-21

A method of making dispersion-strengthened alloy particles involves melting an alloy having a corrosion and/or oxidation resistance-imparting alloying element, a dispersoid-forming element, and a matrix metal wherein the dispersoid-forming element exhibits a greater tendency to react with a reactive species acquired from an atomizing gas than does the alloying element. The melted alloy is atomized with the atomizing gas including the reactive species to form atomized particles so that the reactive species is (a) dissolved in solid solution to a depth below the surface of atomized particles and/or (b) reacted with the dispersoid-forming element to form dispersoids in the atomized particles to a depth below the surface of said atomized particles. Bodies made from the dispersion strengthened solidified particles exhibit enhanced fatigue and creep resistance and reduced wear as well as enhanced corrosion and/or oxidation resistance at high temperatures.

Preparation, characterization and in vitro/vivo evaluation of tectorigenin solid dispersion with improved dissolution and bioavailability.

PubMed

Shuai, Shuping; Yue, Shanlan; Huang, Qingting; Wang, Wei; Yang, Junyi; Lan, Ke; Ye, Liming

2016-08-01

The purpose of this study was to develop and evaluate a novel amorphous solid dispersion system for tectorigenin (TG). TG is one of isoflavone aglycones extracted from Iris tectorum and flowers of Pueraria thunbergiana, but its poor water solubility and low membrane permeability have severely restricted the clinical application. To increase the aqueous solubility and oral bioavailability of TG, we prepared the solid dispersions of tectorigenin (TG-SD) using a simple solvent evaporation process with TG, polyvinylpyrrolidone (PVP) and PEG4000 at weight ratio of 7:54:9 after tested in several ratios. The prepared solid dispersions of tectorigenin are duly characterized for drug morphological conversion, in vitro dissolution and in vivo bioavailability. The X-ray diffraction (XRD), differential scanning calorimetry (DSC) and scanning electron microscopy (SEM) studies have indicated the morphological conversion of tectorigenin to amorphous form. In vitro release profiles revealed that the % release of TG-SD was achieved 4.35-fold higher than that of the pure drug after 150 min. The oral bioavailability of the solid dispersion in rats was also increased based on AUC0-t and C max of TG-SD, which were 4.8- and 13.1-fold higher than that of TG crystal, respectively. It is worth noting that physical mixture containing TG, PEG4000 and PVP produced a similar level of oral exposure as TG-SD, suggesting that PEG4000 and PVP were able to enhance bioavailability of TG in rats. However, with the reduction of particle size, TG-SD provided the fastest oral absorption compared to physical mixture and pure drug. These results demonstrated that the efficacy of solid dispersions for the enhancement of TG oral bioavailability was by increasing its aqueous solubility and the solid dispersion formulation could be a viable option for enhancing the oral bioavailability of TG.

Dynamics of solid dispersions in oil during the lubrication of point contacts. Part 1: Graphite

NASA Technical Reports Server (NTRS)

Cusano, C.; Sliney, H. E.

1981-01-01

A Hertzian contact was lubricated with dispersed graphite in mineral oils under boundary lubrication conditions. The contact was optically observed under pure rolling, combined rolling and sliding, and pure sliding conditions. The contact was formed with a steel ball on the flat surface of a glass disk. Photomicrographs are presented which show the distribution of the graphite in and around the contact. Friction and surface damage are also shown for conditions when the base oils are used alone and when graphite is added to the base oils. Under pure rolling and combined rolling and sliding conditions, it is found that, for low speeds, a graphite film can form which will separate the contacting surfaces. Under pure sliding conditions, graphite accumulates at the inlet and sweeps around the contact, but very little of the graphite passes through the contact. The accumulated graphite appears to act as a barrier which reduces the supply of oil available to the contact for boundary lubrication. Friction data show no clear short term beneficial or detrimental effect caused by addition of graphite to the base oil. However, during pure sliding, more abrasion occurs on the polished balls lubricated with the dispersion than on those lubricated with the base oil alone. All observations were for the special case of a highly-polished ball on a glass surface and may not be applicable to other geometries and materials, or to rougher surfaces.

Extensive Diminution of Particle Size and Amorphization of a Crystalline Drug Attained by Eminent Technology of Solid Dispersion: A Comparative Study.

PubMed

Singh, Gurjeet; Sharma, Shailesh; Gupta, Ghanshyam Das

2017-07-01

The present study emphasized on the use of solid dispersion technology to triumph over the drawbacks associated with the highly effective antihypertensive drug telmisartan using different polymers (poloxamer 188 and locust bean gum) and methods (modified solvent evaporation and lyophilization). It is based on the comparison between selected polymers and methods for enhancing solubility through particle size reduction. The results showed different profiles for particle size, solubility, and dissolution of formulated amorphous systems depicting the great influence of polymer/method used. The resulting amorphous solid dispersions were characterized using x-ray diffraction (XRD), differential scanning calorimetry, scanning electron microscopy (SEM), transmission electron microscopy (TEM), and particle size analysis. The optimized solid dispersion (TEL 19) prepared with modified locust bean gum using lyophilization technique showed reduced particle size of 184.5 ± 3.7 nm and utmost solubility of 702 ± 5.47 μg/mL in water, which is quite high as compared to the pure drug (≤1 μg/mL). This study showed that the appropriate selection of carrier may lead to the development of solid dispersion formulation with desired solubility and dissolution profiles. The optimized dispersion was later formulated into fast-dissolving tablets, and further optimization was done to obtain the tablets with desired properties.

Effect of composition in the development of carbamazepine hot-melt extruded solid dispersions by application of mixture experimental design.

PubMed

Djuris, Jelena; Ioannis, Nikolakakis; Ibric, Svetlana; Djuric, Zorica; Kachrimanis, Kyriakos

2014-02-01

This study investigates the application of hot-melt extrusion for the formulation of carbamazepine (CBZ) solid dispersions, using polyethyleneglycol-polyvinyl caprolactam-polyvinyl acetate grafted copolymer (Soluplus, BASF, Germany) and polyoxyethylene-polyoxypropylene block copolymer (Poloxamer 407). In agreement with the current Quality by Design principle, formulations of solid dispersions were prepared according to a D-optimal mixture experimental design, and the influence of formulation composition on the properties of the dispersions (CBZ heat of fusion and release rate) was estimated. Prepared solid dispersions were characterized using differential scanning calorimetry, attenuated total reflectance infrared spectroscopy and hot stage microscopy, as well as by determination of the dissolution rate of CBZ from the hot-melt extrudates. Solid dispersions of CBZ can be successfully prepared using the novel copolymer Soluplus. Inclusion of Poloxamer 407 as a plasticizer facilitated the processing and decreased the hardness of hot-melt extrudates. Regardless of their composition, all hot-melt extrudates displayed an improvement in the release rate compared to the pure CBZ, with formulations having the ratio of CBZ : Poloxamer 407 = 1 : 1 showing the highest increase in CBZ release rate. Interactions between the mixture components (CBZ and polymers), or quadratic effects of the components, play a significant role in overall influence on the CBZ release rate. © 2013 Royal Pharmaceutical Society.

Modified sedimentation-dispersion model for solids in a three-phase slurry column

DOE Office of Scientific and Technical Information (OSTI.GOV)

Smith, D.N.; Ruether, J.A.; Shah, Y.T.

1986-03-01

Solids distribution data for a three-phase, batch-fluidized slurry bubble column (SBC) are presented, using air as the gas phase, pure liquids and solutions as the liquid phase, and glass beads and carborundum catalyst powder as the solid phase. Solids distribution data for the three-phase SBC operated in a continuous mode of operation are also presented, using nitrogen as the gas phase, water as the liquid phase, and glass beads as the solid phase. A new model to provide a reasonable approach to predict solids concentration distributions for systems containing polydispersed solids is presented. The model is a modification of standardmore » sedimentation-dispersion model published earlier. Empirical correlations for prediction of hindered settling velocity and solids dispersion coefficient for systems containing polydispersed solids are presented. A new method of evaluating critical gas velocity (CGV) from concentrations of the sample withdrawn at the same port of the SBC is presented. Also presented is a new mapping for CGV which separates the two regimes in the SBC, namely, incomplete fluidization and complete fluidization.« less

Feasibility of an advanced thrust termination assembly for a solid propellant rocket motor

NASA Technical Reports Server (NTRS)

1975-01-01

A total of 68 quench tests were conducted in a vented bomb assembly (VBA). Designed to simulate full-scale motor operating conditions, this laboratory apparatus uses a 2-inch-diameter, end-burning propellant charge and an insulated disc of consolidated hydrated aluminum sulfate along with the explosive charge necessary to disperse the salt and inject it onto the burning surface. The VBA was constructed to permit variation of motor design parameters of interest; i.e., weight of salt per unit burning surface area, weight of explosive per unit weight of salt, distance from salt surface to burning surface, incidence angle of salt injection, chamber pressure, and burn time. Completely satisfactory salt quenching, without re-ignition, occurred in only two VBA tests. These were accomplished with a quench charge ratio (QCR) of 0.023 lb salt per square inch of burning surface at dispersing charge ratios (DCR) of 13 and 28 lb of salt per lb of explosive. Candidate materials for insulating salt charges from the rocket combustion environment were evaluated in firings of 5-inch-diameter, uncured end-burner motors. A pressed, alumina ceramic fiber material was selected for further evaluation and use in the final demonstration motor.

Self-assembly of large-scale crack-free gold nanoparticle films using a ‘drain-to-deposit’ strategy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yang, Guang; Hallinan, Daniel T.

2016-04-26

Gold nanoparticles are widely studied due to the ease of controlled synthesis, facile surface modification, and interesting physical properties. However, a technique for depositing large-area, crack-free monolayers on solid substrates is lacking. Herein is presented a method for accomplishing this. Spherical gold nanoparticles were synthesized as an aqueous dispersion. Assembly into monolayers and ligand exchange occurred simultaneously at an organic/aqueous interface. Then the monolayer film was deposited onto arbitrary solid substrates by slowly pumping out the lower, aqueous phase. This allowed the monolayer film (and liquid–liquid interface) to descend without significant disturbance, eventually reaching substrates contained in the aqueous phase.more » The resulting macroscopic quality of the films was found to be superior to films transferred by Langmuir techniques. The surface plasmon resonance and Raman enhancement of the films were evaluated and found to be uniform across the surface of each film.« less

Modeling Oblique Impact Dynamics of Particle-Laden Nanodroplets

NASA Astrophysics Data System (ADS)

Yong, Xin; Qin, Shiyi

2016-11-01

A fundamental understanding of the impact dynamics of nanoscopic droplets laden with nanoparticles has important implications for materials printing and thin film processing. Using many-body dissipative particle dynamics (MDPD), we model nanometer sized suspension droplets imping on dry solid substrate with oblique angles, and compare their behavior with pure liquid droplets. Equilibrated floating droplets containing two types of nanoparticles, namely fully-wetted hydrophilic particles and surface-active Janus particles, impact onto the solid surface with varying initial velocities and impact angles. The velocity components in the normal and tangential directions to the substrate defines normal and tangential Reynolds and Weber numbers, which are used to classify impact regimes. Droplets with nanoparticles dispersed in the bulk and covering the droplet surface (resembling liquid marbles) exhibit quite different behavior in the course of impact. We also reveal the influences of substrate wettability and its interaction with nanoparticles on the impact dynamics. In addition, the vapor film beneath an impinging droplet shows no significant effect on the impact dynamics in our MDPD simulations.

High-temperature friction and wear studies of Fe-Cu-Sn alloy with graphite as solid lubricant under dry sliding conditions

NASA Astrophysics Data System (ADS)

Mushtaq, Shuhaib; Wani, M. F.

2018-02-01

Solid lubricants are particularly used in the advanced mechanical motion systems with extreme conditions such as (high temperature, vacuum, radiation, extreme contact pressure, etc). The main focus of this paper is to study the dry sliding friction and wear behavior of Fe-Cu-Sn alloy with varying wt% of graphite at high temperature up to 423 K. The influence of temperature, sliding distance and load on friction and wear behavior of Fe-Cu-Sn alloy against EN8 steel was studied using ball (EN8) on disc (Fe-Cu-Sn alloy). Lower wear and lower friction of Fe-Cu-Sn alloy were observed at high temperature, as compared to room temperature. Surface morphological and surface analytical studies of fresh and worn surfaces were carried out using optical microscopy, 3D profilometer, scanning electron microscope, energy dispersive x-ray spectroscopy, XRD, and Raman spectroscopy to understand the friction and wear behavior.

Enhancement of in-vitro drug dissolution of ketoconazole for its optimal in-vivo absorption using Nanoparticles and Solid Dispersion forms of the drug

NASA Astrophysics Data System (ADS)

Syed, Mohammed Irfan

Ketoconazole is one of the most widely prescribed oral antifungal drugs for the systemic treatment of various fungal infections. However, due its hydrophobic nature and poor solubility profiles in the gastro-intestinal fluids, variations in its bioavailability have been documented. Therefore, to enhance its dissolution in the biological fluids, this study was initiated to develop and evaluate Nanoparticles and Solid Dispersion forms of the drug. Nanoparticles of ketoconazole were developed by Wet Bead Milling technique using PVP-10k as the stabilizing material at a weight ratio of (2:1). Solid dispersion powder was prepared by Hot Melt method using PEG-8000 at a weight ratio of (1:2). A commercial product containing 200mg of ketoconazole tablet and pure drug powder were used as the control for comparison purposes. The dissolution studies were carried out in SGF, SIF, USP; and SIF with 0.2% sodium lauryl sulfate using the USP-II method for a 2 hours period. Physical characterizations were carried out using SEM, DSC, XRD and FTIR studies. Wet Bead Milling method yielded nanoparticles in the particles size range of (100-300nm.). First all samples were evaluated for their in-vitro dissolution in SGF at pH=1.2. After 15 minutes, the amounts of drug dissolved were observed to be 27% from both the pure powder and commercial tablet (control), 29% from solid dispersion and 100% from the Nanoparticles dosage form. This supports the fact that Nanoparticles had a strong influence on the dissolution rate of the drug and exhibited much faster dissolution of ketoconazole. When the same formulations were studied in the SIF, USP medium, the control formulation gave 3%, solid dispersion 8% and Nanoparticles 8% drug dissolution after 2 hours period. This could be because the weakly basic ketoconazole drug remained un-dissociated in the alkaline medium. Since this medium was unable to clearly distinguish the dissolution profiles from different formulation of the drug, the SIF solution was modified to include 0.02%, 0.05% and 0.1% sodium lauryl sulfate. Here, after 2 hours, the amount of drug dissolved was calculated to be 10% from controls, 21% from solid dispersion and 36% from nanoparticles in SIF with 0.02% SLS. Drug release was 20% from controls, 41% from solid dispersion and 52% from nanoparticle formulation in SIF with 0.05% SLS. Whereas amount of drug released in SIF with 0.1% SLS showed 21% from the control, 62% from solid dispersion and 85% from Nanoparticles respectively. This data supports that the ketoconazole Nanoparticles and its solid-dispersion exhibit many fold increase in dissolution of the drug, which could lead to a less variable and enhanced in-vivo drug absorption profiles. In addition, the data from the Physical Characterization (DSC, XRD and FTIR) supports that there were no interaction within the ingredients occurred in Nanoparticles and solid-dispersion formulations of the drug sample. Wet Bead Milling and Hot Melt methods proved useful in developing the Nanoparticles and solid dispersion form of ketoconazole. Results from particle size analysis were in correlation with data obtained from Scanning electron Microscopy and size of the nanoparticles was below 100nm. The dissolution studies with the modified simulated intestinal fluid (SIF) exhibited several fold increase in the dissolution of the drug compared to the pure drug powder and the commercial products used as the control. Also, the results from the physical characterization studies clearly support the stability of ketoconazole in both of these formulations.

Site specific solubility improvement using solid dispersions of HPMC-AS/HPC SSL--mixtures.

PubMed

Zecevic, Damir Elmar; Meier, Robin; Daniels, Rolf; Wagner, Karl-Gerhard

2014-07-01

Many upcoming drug candidates are pH-dependent poorly soluble weak bases in the pH range of the gastrointestinal tract. This often leads to a high in vivo variability and bioavailability issues. Aiming to overcome these limitations, the design of solid dispersions for site specific dissolution improvement or maintenance of a potent supersaturation over the entire gastro-intestinal pH-range, is proposed to assure a reliable drug therapy. Solid dispersions containing different ratios of Dipyridamole (DPD) or Griseofulvin (GRI) and the enteric polymer hydroxypropylmethylcellulose-acetate succinate (HPMC-AS) and the water soluble low-viscosity hydroxypropylcellulose (HPC-SSL) were prepared by hot melt extrusion (HME). The solid dispersions were evaluated for their solid state, dissolution characteristics applying a three pH-step dissolution method following an acidic to neutral pH transition and stability. The use of HPMC-AS in binary mixtures with DPD and GRI facilitated increased solubility and supersaturation at pH-controlled release of the preserved amorphous state of the dispersed drug, which even inverted the pH-dependent solubility profile of the weakly basic model drug (Dipyridamole). I.e. a potent site specific delivery system was created. With ternary solid dispersions of API, HPMC-AS and HPC-SSL, tailored release profiles with superior supersaturation over the applied pH-range could be obtained. At the same time, binary and ternary mixtures showed favorable stability properties at a temperature difference between glass transition temperature and the applied storage temperature of down to 16°C. Copyright © 2014 Elsevier B.V. All rights reserved.

Designed Synthesis of Mesoporous Solid-Supported Lewis Acid-Base Pairs and Their CO2 Adsorption Behaviors.

PubMed

Zakharova, Maria V; Masoumifard, Nima; Hu, Yimu; Han, Jongho; Kleitz, Freddy; Fontaine, Frédéric-Georges

2018-04-18

Conventional amines and phosphines, such as diethylenetriamine, diphenylpropylphosphine, triethylamine, and tetramethylpiperidine, were grafted or impregnated on the surface of metalated SBA-15 materials, such as Ti-, Al-, and Zr-SBA-15, to generate air-stable solid-supported Lewis acid-base pairs. The Lewis acidity of the metalated materials before and after the introduction of Lewis bases was verified by means of pyridine adsorption-Fourier transform infrared spectroscopy. Detailed characterization of the materials was achieved by solid-state 13 C and 31 P MAS NMR spectroscopy, low-temperature N 2 physisorption, X-ray photoelectron spectroscopy, and energy-dispersive X-ray mapping analyses. Study of their potential interactions with CO 2 was performed using CO 2 adsorption isotherm experiments, which provided new insights into their applicability as solid CO 2 adsorbents. A correlation between solid-supported Lewis acid-base pair strength and the resulting affinity to CO 2 is discussed based on the calculation of isosteric enthalpy of adsorption.

Formation of nano/micro-dispersions with improved dissolution properties upon dispersion of ritonavir melt extrudate in aqueous media.

PubMed

Tho, Ingunn; Liepold, Bernd; Rosenberg, Joerg; Maegerlein, Markus; Brandl, Martin; Fricker, Gert

2010-04-16

The objective of the study was to characterise the aqueous dispersions of ritonavir melt extrudates. More specifically to look into the particular system formed when melt extrudate of a poorly soluble drug dissolved in a hydrophilic polymer matrix containing a surfactant is dispersed in an aqueous medium. Melt extrudates with and without ritonavir were studied. The drug containing extrudate was confirmed to be molecular dispersions of drug in a polymer/surfactant matrix. Particulate dispersions were formed in water from both drug and placebo extrudates. The dispersions were investigated with respect to mean particle size and particle size distribution (photon correlation spectroscopy and optical particle counting), surface charge (zeta potential), particle composition (ultracentrifugation), tendency to form aggregates and precipitate (turbidity), in vitro dissolution rate and drug release. It was concluded that dispersion of melt extrudates in aqueous medium give rise to nano/micro-dispersions. The stability of the nano/micro-dispersion is sensitive to anions and may be subjected to association/aggregation/flocculation as time proceeds after preparation of dispersion. Melt extrudate showed improved dissolution rate and drug release properties compared to crystalline raw material. From studies of single components and physical mixtures of the formulation composition it can be concluded that the drug delivery system itself, namely solid dispersion prepared by melt extrusion technology, plays a key role for the formation of the observed particles. 2010 Elsevier B.V. All rights reserved.

Quantitatively identifying the roles of interfacial water and solid surface in governing peptide adsorption.

PubMed

Xu, Zhijun; Yang, Xiao; Wei, Qichao; Zhao, Weilong; Cui, Beiliang; Yang, Xiaoning; Sahai, Nita

2018-06-11

Understanding the molecular mechanism of protein adsorption on solids is critical to their applications in materials synthesis and tissue engineering. Though the water phase at the surface/water interface has been recognized as three types: free water in the bulk region, intermediate water phase and surface-bound water layers adjacent to the surface, the roles of the water and surface in determining the protein adsorption are not clearly identified, particularly at the quantitative level. Herein, we provide a methodology involving the combination of microsecond strengthen sampling simulation and force integration to quantitatively characterize the water-induced contribution and the peptide-surface interactions into the adsorption free energy. Using hydroxyapatite and graphene surfaces as examples, we demonstrate how the distinct interfacial features dominate the delicate force balance between these two thermodynamics parameters, leading to surface preference/resistance to peptide adsorption. Specifically, the water layer provides sustained repelling force against peptide adsorption, as indicated by a monotonic increase in the water-induced free energy profile, whereas the contribution to the free energy from the surface effect is thermodynamically favorable, thus acting as the dominant driving force for peptide adsorptions. More importantly, the revealed adsorption mechanism is critically dictated by the distribution of water phase at the solid/water interface, which plays a crucial role in establishing the force balance between the interactions of the peptide with the water layer and the surface. For the HAP surface, the charged peptide exhibits strong binding affinity to the surface, which is ascribed to the controlling contribution of peptide-surface interaction in the intermediate water phase and the surface-bound water layers are observed as the origin of bioresistance of solid surfaces towards the adsorption of charge-neutral peptides. The preferred peptide adsorption on the graphene, however, is dominated by the surface-induced component at the water layers adjacent to the surface. Our results further elucidate that the intermediate water phase significantly shortens the effective range of the surface dispersion force to guide the diffusion of the peptide to the interface, in sharp contrast to the observation in interfacial systems involving the strong water-surface interaction.

Mechanism of drug release from polymethacrylate-based extrudates and milled strands prepared by hot-melt extrusion.

PubMed

Albers, Jessica; Alles, Rainer; Matthée, Karin; Knop, Klaus; Nahrup, Julia Schulze; Kleinebudde, Peter

2009-02-01

The aim of the study was the formulation of solid dispersions of the poorly water-soluble drug celecoxib and a polymethacrylate carrier by hot-melt extrusion. The objectives were to elucidate the mechanism of drug release from obtained extrudates and milled strands addicted to the solid-state properties of the solid dispersions and to examine and eliminate stability problems occurring under storage, exposure of mechanical stress, and in vitro dissolution. Transparent extrudates containing up to 60% drug could be prepared with a temperature setting below the melting point of celecoxib. XRPD and DSC measurements indicated the formation of a glassy solid solution, where the drug is molecularly dispersed in the carrier. The amorphous state of the glassy solid solution could be maintained during the exposure of mechanical stress in a milling process, and was stable under storage for at least 6 months. Solid-state properties and SEM images of extrudates after dissolution indicated a carrier-controlled dissolution, whereby the drug is molecularly dispersed within the concentrated carrier layer. The glassy solid solution showed a 58-fold supersaturation in 0.1 N HCl within the first 10 min, which was followed by a recrystallization process. Recrystallization could be inhibited by an external addition of HPMC.

Phosphorus Enrichment as a New Composition in the Solid Electrolyte Interphase of High-Voltage Cathodes and Its Effects on Battery Cycling

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yan, Pengfei; Zheng, Jianming; Kuppan, Saravanan

2015-11-10

Immersion of a solid into liquid often leads to the modification of both the structure and chemistry of surface of the solid, which subsequently affects the chemical and physical properties of the system. For the case of the rechargeable lithium ion battery, such a surface modification is termed as solid electrolyte interphase (SEI) layer, which has been perceived to play critical role for the stable operation of the batteries. However, the structure and chemical composition of SEI layer and its spatial distribution and dependence on the battery operating condition remain unclear. By using aberration corrected scanning transmission electron microscopy coupledmore » with ultra-high sensitive energy dispersive x-ray spectroscopy, we probed the structure and chemistry of SEI layer on several high voltage cathodes. We show that layer-structured cathodes, when cycled at a high cut off voltage, can form a P-rich SEI layer on their surface, which is a direct evidence of Li-salt (LiPF6) decomposition. Our systematical investigations indicate such cathode/Li-salt side reaction shows strong dependence on structure of the cathode materials, operating voltage and temperature, indicating the feasibility of SEI engineering. These findings provide us valuable insights into the complex interface between the high-voltage cathode and the electrolyte.« less

Cationic flocculants carrying hydrophobic functionalities: applications for solid/liquid separation.

PubMed

Schwarz, S; Jaeger, W; Paulke, B-R; Bratskaya, S; Smolka, N; Bohrisch, J

2007-07-26

The flocculation behaviors of three series of polycations with narrow molecular weight distributions carrying hydrophobic substituents on their backbones [poly(N-vinylbenzyl-N,N,N-trimethylammonium chloride), poly(N-vinylbenzyl-N,N-dimethyl-N-butylammonium chloride), and poly(N-vinylbenzylpyridinium chloride)] were investigated in dispersions of monodisperse polystyrene latexes and kaolin. Apparently, the charge density of the polycations decreases with increasing substituent hydrophobicity and increasing molecular weight of the polyelectrolytes. The necessary amount of flocculant for phase separation in dispersions with high substrate surface charge densities increases with increasing hydrophobicity of the polyelectrolyte. Nevertheless, the introduction of hydrophobic functionalities is beneficial, resulting in a substantial broadening of the range between the minimum and maximum amounts of flocculant necessary for efficient flocculation (flocculation window). An increase in ionic strength supports this effect. When the substrate has a low charge density, the hydrophobic interactions play a much more significant role in the flocculation process. Here, the minimum efficient doses remained the same for all three polyelectrolytes investigated, but the width of the flocculation window increased as the polycation hydrophobicity and the molecular weight increased. The necessary amount of flocculant increased with an increase in particle size at constant solid content of the dispersion, as well as with a decreasing number of particles at a constant particle size.

Chemical reactions in low-g

NASA Technical Reports Server (NTRS)

Grodzka, P. G.; Facemire, B. R.

1978-01-01

The Apollo-Soyuz flight experiment, 'Chemical Foams' demonstrated that foams and air/liquid dispersions are much more stable in low-gravity than on the ground. It thus should be possible to conduct unique chemical reactions in space foams. The low-g results and subsequent ground work on the formaldehyde clock reaction indicate that the reaction is strongly influenced by (1) dissociated and undissociated solution species being adsorbed at solid/liquid and gas/liquid surfaces and (2) chemical reaction rates apparently being affected by long-range forces determined by the liquid mass and the extent and nature of all surface interfaces.

Development of solid self-emulsifying drug delivery system (SEDDS) I: use of poloxamer 188 as both solidifying and emulsifying agent for lipids.

PubMed

Shah, Ankita V; Serajuddin, Abu T M

2012-10-01

To develop solid self-emulsifying drug delivery systems (SEDDS) for lipids using poloxamer 188 as both solidifying and emulsifying agents. Mixtures of various lipids with poloxamer 188 and PEG 8000 were prepared at ~75°C. The molten mixtures, with and without dissolved drugs (fenofibrate and probucol), were then cooled to room temperature. When solids formed, they were characterized by powder XRD, DSC, microscopy using cross-polarization and confocal fluorescence techniques, dispersion test in water and particle size analysis of dispersions. When mixed with poloxamer 188 or PEG 8000, lipids consisting of monoesters of fatty acids with glycerol or propylene glycol formed solid systems, but not di- and tri-esters, which showed phase separation. Added to water, the solid systems containing poloxamer 188 started to disperse in water forming oil globules of 200-600 nm. No emulsification of lipids was observed from solids containing PEG 8000, indicating that the surfactant property of poloxamer 188 was responsible for emulsification. Powder XRD, DSC and microscopic examination revealed that poloxamer 188 and PEG 8000 maintained their crystallinity in solid systems, while the lipids were interspersed in between crystalline regions. The drug remained solubilized in the lipid phase. A novel solid SEDDS is developed where the drug can be solubilized in liquid lipids and then the lipidic solution can be converted to solid mass by dispersing into the microstructure of poloxamer 188.

Inventory of oral anticancer agents: Pharmaceutical formulation aspects with focus on the solid dispersion technique.

PubMed

Sawicki, E; Schellens, J H M; Beijnen, J H; Nuijen, B

2016-11-01

Dissolution from the pharmaceutical formulation is a prerequisite for complete and consistent absorption of any orally administered drug, including anticancer agents (oncolytics). Poor dissolution of an oncolytic can result in low oral bioavailability, high variability in blood concentrations and with that suboptimal or even failing therapy. This review discusses pharmaceutical formulation aspects and absorption pharmacokinetics of currently licensed orally administered oncolytics. In nearly half of orally dosed oncolytics poor dissolution is likely to play a major role in low and unpredictable absorption. Dissolution-limited drug absorption can be improved with a solid dispersion which is a formulation method that induces super-saturated drug dissolution and with that it enhances in vivo absorption. This review discusses formulation principles with focus on the solid dispersion technology and how it works to enhance drug absorption. There are currently three licensed orally dosed oncolytics formulated as a solid dispersion (everolimus, vemurafenib and regorafenib) and these formulations result in remarkably improved dissolution and absorption compared to what can be achieved with conventional formulations of the respective oncolytics. Because of the successful implementation of these three solid dispersion formulations, we encourage the application of this formulation method for poorly soluble oral oncolytics. Copyright © 2016 Elsevier Ltd. All rights reserved.

Pollenkitt wetting mechanism enables species-specific tunable pollen adhesion.

PubMed

Lin, Haisheng; Gomez, Ismael; Meredith, J Carson

2013-03-05

Plant pollens are microscopic particles exhibiting a remarkable breadth of complex solid surface features. In addition, many pollen grains are coated with a viscous liquid, "pollenkitt", thought to play important roles in pollen dispersion and adhesion. However, there exist no quantitative studies of the effects of solid surface features or pollenkitt on adhesion of pollen grains, and it remains unclear what role these features play in pollen adhesion and transport. We report AFM adhesion measurements of five pollen species with a series of test surfaces in which each pollen has a unique solid surface morphology and pollenkitt volume. The results indicate that the combination of surface morphology (size and shape of echinate or reticulate features) with the pollenkitt volume provides pollens with a remarkably tunable adhesion to surfaces. With pollenkitt removed, pollen grains had relatively low adhesion strengths that were independent of surface chemistry and scalable with the tip radius of the pollen's ornamentation features, according to the Hamaker model. With the pollenkitt intact, adhesion was up to 3-6 times higher than the dry grains and exhibited strong substrate dependence. The adhesion enhancing effect of pollenkitt was driven by the formation of pollenkitt capillary bridges and was surprisingly species-dependent, with echinate insect-pollinated species (dandelion and sunflower) showing significantly stronger adhesion and higher substrate dependence than wind-pollinated species (ragweed, poplar, and olive). The combination of high pollenkitt volume and large convex, spiny surface features in echinate entomophilous varieties appears to enhance the spreading area of the liquid pollenkitt relative to varieties of pollen with less pollenkitt volume and less pronounced surface features. Measurements of pollenkitt surface energy indicate that the adhesive strength of capillary bridges is primarily dependent on nonpolar van der Waals interactions, with some contribution from the Lewis basic component of surface energy.

Synthesis of Thermoresponsive Amphiphilic Polyurethane Gel as a New Cell Printing Material near Body Temperature.

PubMed

Tsai, Yi-Chun; Li, Suming; Hu, Shiaw-Guang; Chang, Wen-Chi; Jeng, U-Ser; Hsu, Shan-hui

2015-12-23

Waterborne polyurethane (PU) based on poly(ε-caprolactone) (PCL) diol and a second oligodiol containing amphiphilic blocks was synthesized in this study. The microstructure was characterized by dynamic light scattering (DLS), small-angle X-ray scattering (SAXS), and rheological measurement of the PU dispersion. The surface hydrophilicity measurement, infrared spectroscopy, wide-angle X-ray diffraction, mechanical and thermal analyses were conducted in solid state. It was observed that the presence of a small amount of amphiphilic blocks in the soft segment resulted in significant changes in microstructure. When 90 mol % PCL diol and 10 mol % amphiphilic blocks of poly(l-lactide)-poly(ethylene oxide) (PLLA-PEO) diol were used as the soft segment, the synthesized PU had a water contact angle of ∼24° and degree of crystallinity of ∼14%. The dispersion had a low viscosity below room temperature. As the temperature was raised to body temperature (37 °C), the dispersion rapidly (∼170 s) underwent sol-gel transition with excellent gel modulus (G' ≈ 6.5 kPa) in 20 min. PU dispersions with a solid content of 25-30% could be easily mixed with cells in sol state, extruded by a 3D printer, and deposited layer by layer as a gel. Cells remained alive and proliferating in the printed hydrogel scaffold. We expect that the development of novel thermoresponsive PU system can be used as smart injectable hydrogel and applied as a new type of bio-3D printing ink.

Effluent monitoring of the December 10, 1974, Titan 3-E launch at Air Force Eastern Test Range, Florida

NASA Technical Reports Server (NTRS)

Wornom, D. E.; Woods, D. C.

1978-01-01

Surface and airborne field measurements of the cloud behavior and effluent dispersion from a solid rocket motor launch vehicle are presented. The measurements were obtained as part of a continuing launch vehicle effluent monitoring program to obtain experimental field measurements in order to evaluate a model used to predict launch vehicle environmental impact. Results show that the model tends to overpredict effluent levels.

Solid state welding processes for an oxide dispersion strengthened nickel-chromium-aluminum alloy

NASA Technical Reports Server (NTRS)

Moore, T. J.

1975-01-01

Solid-state welding processes were evaluated for joining TD-NiCrAl (Ni-16Cr-4Al-2ThO2) alloy sheet. Both hot-press and resistance spot welding techniques were successfully applied in terms of achieving grain growth across the bond line. Less success was achieved with a resistance seam welding process. In stress-rupture shear and tensile shear tests of lap joints at 1100 C, most failures occurred in the parent material, which indicates that the weld quality was good and that the welds were not a plane of weakness. The overall weld quality was not as good as previously attained with TD-NiCr, probably because the presence of alumina at the faying surfaces and the developmental TD-NiCrAl sheet, which was not of the quality of the TD-NiCr sheet in terms of surface flatness and dimensional control.

Modified fly ash from municipal solid waste incineration as catalyst support for Mn-Ce composite oxides

NASA Astrophysics Data System (ADS)

Chen, Xiongbo; Liu, Ying; Yang, Ying; Ren, Tingyan; Pan, Lang; Fang, Ping; Chen, Dingsheng; Cen, Chaoping

2017-08-01

Fly ash from municipal solid waste incineration was modified by hydrothermal treatment and used as catalyst support for Mn-Ce composite oxides. The prepared catalyst showed good activity for the selective catalytic reduction (SCR) of NO by NH3. A NO conversion of 93% could be achieved at 300 °C under a GHSV of 32857 h-1. With the help of characterizations including XRD, BET, SEM, TEM, XPS and TPR, it was found that hydrothermal treatment brought a large surface area and abundant mesoporous to the modified fly ash, and Mn-Ce composite oxides were highly dispersed on the surface of the support. These physical and chemical properties were the intrinsic reasons for the good SCR activity. This work transformed fly ash into high value-added products, providing a new approach to the resource utilization and pollution control of fly ash.

Fabricating Germanium Interfaces for Battery Applications

NASA Astrophysics Data System (ADS)

Serino, Andrew Clark

The experimental results presented herein detail the importance of material surfaces in device performance. We have demonstrated this importance by furthering and applying our understanding of germanium surfaces to a number of real-world applications. Pure and stable dispersions of germanane, an "all-surface" form of germanium, were created through solid-state synthesis followed by ultrasonication and centrifugation. These dispersions were used to fabricate germanane-based, high-performance, Li-ion anodes with capacities of ˜1100 mA-h/g, capacity retention over 100 cycles, and Coulombic efficiency of 99%. Additionally, carborane monolayers were self-assembled on Ge(100) and Ge(111) surfaces through carboxylic acid tethers, and found to be capable of tuning the surface work function by ˜0.4 eV without significantly affecting surface wettability. These capabilities are important for increasing device efficiency while minimizing complications associated with processing. Lastly, we introduce the concept of the molecular battery, a possible design using a layer-by-layer deposition approach, and our steps toward its realization. In this pursuit, we explored the assembly of metal-organic coordination of carborane-based linkers, as well as the capabilities of a film of benzene-based linkers (<50 nm) as a Li-ion battery separator using a Ge anode as a tool for analyzing performance.

Matrix solid-phase dispersion coupled with homogeneous ionic liquid microextraction for the determination of sulfonamides in animal tissues using high-performance liquid chromatography.

PubMed

Wang, Zhibing; He, Mengyu; Jiang, Chunzhu; Zhang, Fengqing; Du, Shanshan; Feng, Wennan; Zhang, Hanqi

2015-12-01

Matrix solid-phase dispersion coupled with homogeneous ionic liquid microextraction was developed and applied to the extraction of some sulfonamides, including sulfamerazine, sulfamethazine, sulfathiazole, sulfachloropyridazine, sulfadoxine, sulfisoxazole, and sulfaphenazole, in animal tissues. High-performance liquid chromatography was applied to the separation and determination of the target analytes. The solid sample was directly treated by matrix solid-phase dispersion and the eluate obtained was treated by homogeneous ionic liquid microextraction. The ionic liquid was used as the extraction solvent in this method, which may result in the improvement of the recoveries of the target analytes. To avoid using organic solvent and reduce environmental pollution, water was used as the elution solvent of matrix solid-phase dispersion. The effects of the experimental parameters on recoveries, including the type and volume of ionic liquid, type of dispersant, ratio of sample to dispersant, pH value of elution solvent, volume of elution solvent, amount of salt in eluate, amount of ion-pairing agent (NH4 PF6 ), and centrifuging time, were evaluated. When the present method was applied to the analysis of animal tissues, the recoveries of the analytes ranged from 85.4 to 118.0%, and the relative standard deviations were lower than 9.30%. The detection limits for the analytes were 4.3-13.4 μg/kg. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Formulation and optimization of mouth dissolve tablets containing rofecoxib solid dispersion.

PubMed

Sammour, Omaima A; Hammad, Mohammed A; Megrab, Nagia A; Zidan, Ahmed S

2006-06-16

The purpose of the present investigation was to increase the solubility and dissolution rate of rofecoxib by the preparation of its solid dispersion with polyvinyl pyrrolidone K30 (PVP K30) using solvent evaporation method. Drug-polymer interactions were investigated using differential scanning calorimetry (DSC), x-ray diffraction (XRD), and Fourier transform infrared spectroscopy (FTIR). For the preparation of rofecoxib mouth dissolve tablets, its 1:9 solid dispersion with PVP K30 was used with various disintegrants and sublimable materials. In an attempt to construct a statistical model for the prediction of disintegration time and percentage friability, a 3(2) randomized full and reduced factorial design was used to optimize the influence of the amounts of superdisintegrant and subliming agent. The obtained results showed that dispersion of the drug in the polymer considerably enhanced the dissolution rate. The drug-to-carrier ratio was the controlling factor for dissolution improvement. FTIR spectra revealed no chemical incompatibility between the drug and PVP K30. As indicated from XRD and DSC data, rofecoxib was in the amorphous form, which explains the better dissolution rate of the drug from its solid dispersions. Concerning the optimization study, the multiple regression analysis revealed that an optimum concentration of camphor and a higher percentage of crospovidone are required for obtaining rapidly disintegrating tablets. In conclusion, this investigation demonstrated the potential of experimental design in understanding the effect of the formulation variables on the quality of mouth dissolve tablets containing solid dispersion of a hydrophobic drug.

Simultaneous determination of phenolic compounds in Equisetum palustre L. by ultra high performance liquid chromatography with tandem mass spectrometry combined with matrix solid-phase dispersion extraction.

PubMed

Wei, Zuofu; Pan, Youzhi; Li, Lu; Huang, Yuyang; Qi, Xiaolin; Luo, Meng; Zu, Yuangang; Fu, Yujie

2014-11-01

A method based on matrix solid-phase dispersion extraction followed by ultra high performance liquid chromatography with tandem mass spectrometry is presented for the extraction and determination of phenolic compounds in Equisetum palustre. This method combines the high efficiency of matrix solid-phase dispersion extraction and the rapidity, sensitivity, and accuracy of ultra high performance liquid chromatography with tandem mass spectrometry. The influential parameters of the matrix solid-phase dispersion extraction were investigated and optimized. The optimized conditions were as follows: silica gel was selected as dispersing sorbent, the ratio of silica gel to sample was selected to be 2:1 (400/200 mg), and 8 mL of 80% methanol was used as elution solvent. Furthermore, a fast and sensitive ultra high performance liquid chromatography with tandem mass spectrometry method was developed for the determination of nine phenolic compounds in E. palustre. This method was carried out within <6 min, and exhibited satisfactory linearity, precision, and recovery. Compared with ultrasound-assisted extraction, the proposed matrix solid-phase dispersion procedure possessed higher extraction efficiency, and was more convenient and time saving with reduced requirements on sample and solvent amounts. All these results suggest that the developed method represents an excellent alternative for the extraction and determination of active components in plant matrices. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Electrochemical Deposition of Niobium onto the Surface of Copper Using a Novel Choline Chloride-Based Ionic Liquid

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wixtroma, Alex I.; Buhlera, Jessica E.; Reece, Charles E.

2013-06-01

Recent research has shown that choline chloride-based solutions can be used to replace acid-based electrochemical polishing solutions. In this study niobium metal was successfully deposited on the surface of copper substrate via electrochemical deposition using a novel choline chloride-based ionic liquid. The niobium metal used for deposition on the Cu had been dissolved in the solution from electrochemical polishing of a solid niobium piece prior to the deposition. The visible coating on the surface of the Cu was analyzed using scanning electron microscopy (SEM) and electron dispersive x-ray spectroscopy (EDX). This deposition method effectively recycles previously dissolved niobium from electrochemicalmore » polishing.« less

A study of the effect of solid particle impact and particle shape on the erosion morphology of ductile metals

NASA Technical Reports Server (NTRS)

Rao, P. V.; Young, S. G.; Buckley, D. H.

1984-01-01

Impulsive versus steady jet impingement of spherical glass bead particles on metal surfaces was studied using a gas gun facility and a commercial sand blasting apparatus. Crushed glass particles were also used in the sand blasting apparatus as well as glass beads. Comparisons of the different types of erosion patterns were made. Scanning electron microscopy, surface profilometry and energy dispersive X-ray spectroscopy analysis were used to characterize erosion patterns. The nature of the wear can be divided into cutting and deformation, each with its own characteristic features. Surface chemistry analysis indicates the possiblity of complex chemical and/or mechanical interactions between erodants and target materials.

A study of the nature of solid particle impact and shape on the erosion morphology of ductile metals

NASA Technical Reports Server (NTRS)

Rao, P. V.; Young, S. G.; Buckley, D. H.

1982-01-01

Impulsive versus steady jet impingement of spherical glass bead particles on metal surfaces was studied using a gas gun facility and a commercial sand blasting apparatus. Crushed glass particles were also used in the sand blasting apparatus as well as glass beads. Comparisons of the different types of erosion patterns were made. Scanning electron microscopy, surface profilometry and energy dispersive X-ray spectroscopy analysis were used to characterize erosion patterns. The nature of the wear can be divided into cutting and deformation, each with its own characteristic features. Surface chemistry analysis indicates the possibility of complex chemical and/or mechanical interactions between erodants and target materials.

Computational design and fabrication of core-shell magnetic molecularly imprinted polymer for dispersive micro-solid-phase extraction coupled with high-performance liquid chromatography for the determination of rhodamine 6G.

PubMed

Xie, Jin; Xie, Jie; Deng, Jian; Fang, Xiangfang; Zhao, Haiqing; Qian, Duo; Wang, Hongjuan

2016-06-01

A novel core-shell magnetic nano-adsorbent with surface molecularly imprinted polymer coating was fabricated and then applied to dispersive micro-solid-phase extraction followed by determination of rhodamine 6G using high-performance liquid chromatography. The molecularly imprinted polymer coating was prepared by copolymerization of dopamine and m-aminophenylboronic acid (functional monomers), in the presence of rhodamine 6G (template). The selection of the suitable functional monomers was based on the interaction between different monomers and the template using the density functional theory. The ratios of the monomers to template were further optimized by an OA9 (3(4) ) orthogonal array design. The binding performances of the adsorbent were evaluated by static, kinetic, and selective adsorption experiments. The results reveal that the adsorbent possesses remarkable affinity and binding specificity for rhodamine 6G because of the enhanced Lewis acid-base interaction between the B(Ш) embedded in the imprinted cavities and the template. The nano-adsorbent was successfully applied to dispersive micro-solid-phase extraction coupled to high-performance liquid chromatography for the trace determination of rhodamine 6G in samples with a detection limit of 2.7 nmol/L. Spiked recoveries ranged from 93.0-99.1, 89.5-92.7, and 86.9-105% in river water, matrimony vine and paprika samples, respectively, with relative standard deviations of less than 4.3%. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Surface acidity scales: Experimental measurements of Brønsted acidities on anatase TiO2 and comparison with coinage metal surfaces

NASA Astrophysics Data System (ADS)

Silbaugh, Trent L.; Boaventura, Jaime S.; Barteau, Mark A.

2016-08-01

The first quantitative surface acidity scale for Brønsted acids on a solid surface is presented through the use of titration-displacement and equilibrium experiments on anatase TiO2. Surface acidities of species on TiO2 correlated with gas phase acidities, as was previously observed in qualitative studies of Brønsted acid displacement on Ag(110), Cu(110) and Au(111). A 90% compression of the surface acidity scale relative to the gas phase was observed due to compensation from the covalent component of the conjugate base - surface bond. Adsorbed conjugate bases need not be completely anionic for correlations with gas phase acidities to hold. Positive and negative substituent effects, such as substituted fluorine and hydrocarbon sidechain dispersion interactions with the surface, may modify the surface acidity scale, in agreement with previous experimental and theoretical work on Au(111).

Screening Smokes

DTIC Science & Technology

1942-03-15

It should be capable of being readily dispersed . 6. It would be desirable to use a material which reacts with the atmosphere to edd weight. (White...experimental unit handling 15 gip.m. at 5000 lbs. (equivalent in liquid volume dispersed to well over 1000 small Tweedales) has a theoretical...of real promise. "> - 9 - Solid Smokes It has bt»an suggested that various a*mnd8ntly-avallable solid materials might be dispersed as

Evaluation of a molecularly imprinted polymer for determination of steroids in goat milk by matrix solid phase dispersion.

PubMed

Gañán, Judith; Morante-Zarcero, Sonia; Gallego-Picó, Alejandrina; Garcinuño, Rosa María; Fernández-Hernando, Pilar; Sierra, Isabel

2014-08-01

A molecularly imprinted polymer-matrix solid-phase dispersion methodology for simultaneous determination of five steroids in goat milk samples was proposed. Factors affecting the extraction recovery such as sample/dispersant ratio and washing and elution solvents were investigated. The molecularly imprinted polymer used as dispersant in the matrix solid-phase dispersion procedure showed high affinity to steroids, and the obtained extracts were sufficiently cleaned to be directly analyzed. Analytical separation was performed by micellar electrokinetic chromatography using a capillary electrophoresis system equipped with a diode array detector. A background electrolyte composed of borate buffer (25mM, pH 9.3), sodium dodecyl sulfate (10mM) and acetonitrile (20%) was used. The developed MIP-MSPD methodology was applied for direct determination of testosterone (T), estrone (E1), 17β-estradiol (17β-E2), 17α-ethinylestradiol (EE2) and progesterone (P) in different goat milk samples. Mean recoveries obtained ranged from 81% to 110%, with relative standard deviations (RSD)≤12%. The molecularly imprinted polymer-matrix solid-phase dispersion method is fast, selective, cost-effective and environment-friendly compared with other pretreatment methods used for extraction of steroids in milk. Copyright © 2014 Elsevier B.V. All rights reserved.

Rheology Guided Rational Selection of Processing Temperature To Prepare Copovidone-Nifedipine Amorphous Solid Dispersions via Hot Melt Extrusion (HME).

PubMed

Yang, Fengyuan; Su, Yongchao; Zhang, Jingtao; DiNunzio, James; Leone, Anthony; Huang, Chengbin; Brown, Chad D

2016-10-03

The production of amorphous solid dispersions via hot melt extrusion (HME) relies on elevated temperature and prolonged residence time, which can result in potential degradation and decomposition of thermally sensitive components. Herein, the rheological properties of a physical mixture of polymer and an active pharmaceutical ingredient (API) were utilized to guide the selection of appropriate HME processing temperature. In the currently studied copovidone-nifedipine system, a critical temperature, which is substantially lower (∼13 °C) than the melting point of crystalline API, was captured during a temperature ramp examination and regarded as the critical point at which the API could molecularly dissolve into the polymer. Based on the identification of this critical point, various solid dispersions were prepared by HME processing below, at, and above the critical temperature (both below and above the melting temperature (T m ) of crystalline API). In addition, the resultant extrudates along with two control solid dispersions prepared by physical mixing and cryogenic milling were assessed by X-ray diffraction, differential scanning calorimetry, hot stage microscopy, rheology, and solid-state NMR. Physicochemical properties of resultant solid dispersions indicated that the identified critical temperature is sufficient for the polymer-API system to reach a molecular-level mixing, manifested by the transparent and smooth appearance of extrudates, the absence of API crystalline diffraction and melting peaks, dramatically decreased rheological properties, and significantly improved polymer-API miscibility. Once the critical temperature has been achieved, further raising the processing temperature only results in limited improvement of API dispersion, reflected by slightly reduced storage modulus and complex viscosity and limited improvement in miscibility.

Dissolution enhancement of atorvastatin calcium by co-grinding technique.

PubMed

Prabhu, Priyanka; Patravale, Vandana

2016-08-01

Atorvastatin calcium (AC) is a BCS class II drug which shows poor bioavailability due to inadequate dissolution. Solid dispersions present a promising option to enhance the solubility of poorly soluble drugs. Co-grinding with hydrophilic excipients is an easy and economical technique to improve the solubility of poorly soluble drugs and is free from usage of organic solvents. The aim of the present study was to explore novel carrier VBP-1 (organosulphur compound) for formulating a solid dispersion by using a simple, commercially viable co-grinding technique to enhance the dissolution of AC and to develop an oral formulation of the same. Composition of the solid dispersion was optimized based on the release profile in pH 1.2 buffer. The optimized solid dispersion was further characterized for flow properties, DSC, FTIR spectroscopy, XRD, contact angle, SEM studies and release profile in phosphate buffer pH 6.8. The developed solid dispersion gave similar release profile as the innovator formulation (Lipitor® tablets) in both pH 1.2 buffer and phosphate buffer pH 6.8. The developed solid dispersion was formulated into hard gelatin capsules (size 3). The developed capsules were found to give similar release as the innovator formulation in both pH 1.2 buffer and phosphate buffer pH 6.8. The developed capsules were found to be stable for a period of 6 months. Anti-hyperlipidemic efficacy studies in rats showed higher reduction in cholesterol and triglyceride levels by the developed capsules in comparison to pure AC. In conclusion, novel carrier VBP-1 was successfully employed to enhance the dissolution of AC using co-grinding technique.

Physiochemical Characterization and Release Rate Studies of SolidDispersions of Ketoconazole with Pluronic F127 and PVP K-30

PubMed Central

Kumar, Pankaj; Mohan, Chander; KanamSrinivasan Uma Shankar, Mara; Gulati, Monica

2011-01-01

In the present study solid dispersions of the antifungal drug Ketoconazole were prepared with Pluronic F-127 and PVP K-30 with an intention to improve its dissolution properties. Investigations of the properties of the dispersions were performed using release studies, Differential scanning calorimetery (DSC), X-ray powder diffraction (XRD) and Fourier transform infrared (FTIR). The results obtained showed that the rate of dissolution of Ketoconazole was considerably improved when formulated in solid dispersions with PVP K-30 and Pluronic F-127 as compared with pure drug and physical mixtures. The results from DSC and XRD studies showed the transition of crystalline nature of drug to amorphous form, while FTIR studies demonstrated the absence of drug-carriers interaction. PMID:24250403

Method of forming components for a high-temperature secondary electrochemical cell

DOEpatents

Mrazek, Franklin C.; Battles, James E.

1983-01-01

A method of forming a component for a high-temperature secondary electrochemical cell having a positive electrode including a sulfide selected from the group consisting of iron sulfides, nickel sulfides, copper sulfides and cobalt sulfides, a negative electrode including an alloy of aluminum and an electrically insulating porous separator between said electrodes. The improvement comprises forming a slurry of solid particles dispersed in a liquid electrolyte such as the lithium chloride-potassium chloride eutetic, casting the slurry into a form having the shape of one of the components and smoothing the exposed surface of the slurry, cooling the cast slurry to form the solid component, and removing same. Electrodes and separators can be thus formed.

Interfacial interaction track of amorphous solid dispersions established by water-soluble polymer and indometacin.

PubMed

Li, Jing; Fan, Na; Wang, Xin; Li, Chang; Sun, Mengchi; Wang, Jian; Fu, Qiang; He, Zhonggui

2017-08-30

The present work studied interfacial interactions of amorphous solid dispersions matrix of indometacin (IMC) that established using PVP K30 (PVP) and PEG 6000 (PEG) by focusing on their interaction forces and wetting process. Infrared spectroscopy (IR), raman spectroscopy, X-ray photoelectron spectra and contact angle instrument were used throughout the study. Hydrogen bond energy formed between PEG and IMC were stronger than that of PVP and IMC evidenced by molecular modeling measurement. The blue shift of raman spectroscopy confirmed that hydrogen bonding forces were formed between IMC and two polymers. The contact angle study can be used as an easy method to determine the dissolution mechanism of amorphous solid dispersions through fitting the profile of contact angle of water on a series of tablets. It is believed that the track of interfacial interactions will certainly become powerful tools to for designing and evaluating amorphous solid dispersions. Copyright © 2017 Elsevier B.V. All rights reserved.

Developing dissolution testing methodologies for extended-release oral dosage forms with supersaturating properties. Case example: Solid dispersion matrix of indomethacin.

PubMed

Tajiri, Tomokazu; Morita, Shigeaki; Sakamoto, Ryosaku; Mimura, Hisahi; Ozaki, Yukihiro; Reppas, Christos; Kitamura, Satoshi

2015-07-25

The objective of this study was to develop an in vitro dissolution test method with discrimination ability for an extended-release solid dispersion matrix of a lipophilic drug using the United States Pharmacopeia (USP) Apparatus 4, flow-through cell apparatus. In the open-loop configuration, the sink condition was maintained by manipulating the flow rate of the dissolution medium. To evaluate the testing conditions, the drug release mechanism from an extended-release solid dispersion matrix containing hydrophobic and hydrophilic polymers was investigated. As the hydroxypropyl methylcellulose (HPMC) maintained concentrations of indomethacin higher than the solubility in a dissolution medium, the release of HPMC into the dissolution medium was also quantified using size-exclusion chromatography. We concluded that the USP Apparatus 4 is suitable for application to an in vitro dissolution method for orally administered extended-release solid dispersion matrix formulations containing poorly water-soluble drugs. Copyright © 2015 Elsevier B.V. All rights reserved.

Unctuous ZrO2 nanoparticles with improved functional attributes as lubricant additives

NASA Astrophysics Data System (ADS)

Espina Casado, Jorge; Fernández González, Alfonso; José del Reguero Huerga, Ángel; Rodríguez-Solla, Humberto; Díaz-García, Marta Elena; Badía-Laíño, Rosana

2017-12-01

One of the main drawbacks in the application of metal-oxide nanoparticles as lubricant additives is their poor stability in organic media, despite the good anti-wear, friction-reducing and high-load capacity properties described for these materials. In this work, we present a novel procedure to chemically cap the surface of ZrO2 nanoparticles (ZrO2NPs) with long hydrocarbon chains in order to obtain stable dispersions of ZrO2NPs in non-aqueous media without disrupting their attributes as lubricant additives. C-8, C-10 and C-16 saturated flexible chains were attached to the ZrO2NP surface and their physical and chemical characterization was performed by transmission electron microscopy, thermogravimetric analysis, attenuated total reflectance Fourier transform infrared spectroscopy, x-ray photoelectron spectroscopy and solid-state nuclear magnetic resonance. The dispersion stability of the modified ZrO2NPs in non-aqueous media was studied using static multiple light scattering. Tribological tests demonstrated that dispersions of the long-chain capped ZrO2NPs in base lubricating oils exhibited low friction coefficients and improved the anti-wear properties of the base oil when compared with the raw lubricating oil.

Entropy-driven motility of Sinorhizobium meliloti on a semi-solid surface

PubMed Central

Dilanji, Gabriel E.; Teplitski, Max; Hagen, Stephen J.

2014-01-01

Sinorhizobium meliloti growing on soft agar can exhibit an unusual surface spreading behaviour that differs from other bacterial surface motilities. Bacteria in the colony secrete an exopolysaccharide-rich mucoid fluid that expands outward on the surface, carrying within it a suspension of actively dividing cells. The moving slime disperses the cells in complex and dynamic patterns indicative of simultaneous bacterial growth, swimming and aggregation. We find that while flagellar swimming is required to maintain the cells in suspension, the spreading and the associated pattern formation are primarily driven by the secreted exopolysaccharide EPS II, which creates two entropy-increasing effects: an osmotic flow of water from the agar to the mucoid fluid and a crowding or depletion attraction between the cells. Activation of these physical/chemical phenomena may be a useful function for the high molecular weight EPS II, a galactoglucan whose biosynthesis is tightly regulated by the ExpR/SinI/SinR quorum-sensing system: unlike bacterial colonies that spread via bacterium-generated, physical propulsive forces, S. meliloti under quorum conditions may use EPS II to activate purely entropic forces within its environment, so that it can disperse by passively ‘surfing’ on those forces. PMID:24741008

Synthesis of TiO2-poly(3-hexylthiophene) hybrid particles through surface-initiated Kumada catalyst-transfer polycondensation.

PubMed

Boon, Florian; Moerman, David; Laurencin, Danielle; Richeter, Sébastien; Guari, Yannick; Mehdi, Ahmad; Dubois, Philippe; Lazzaroni, Roberto; Clément, Sébastien

2014-09-30

TiO2/conjugated polymers are promising materials in solar energy conversion where efficient photoinduced charge transfers are required. Here, a "grafting-from" approach for the synthesis of TiO2 nanoparticles supported with conjugated polymer brushes is presented. Poly(3-hexylthiophene) (P3HT), a benchmark material for organic electronics, was selectively grown from TiO2 nanoparticles by surface-initiated Kumada catalyst-transfer polycondensation. The grafting of the polymer onto the surface of the TiO2 nanoparticles by this method was demonstrated by (1)H and (13)C solid-state NMR, X-ray photoelectron spectrometry, thermogravimetric analysis, transmission electron microscopy, and UV-visible spectroscopy. Sedimentation tests in tetrahydrofuran revealed improved dispersion stability for the TiO2@P3HT hybrid material. Films were produced by solvent casting, and the quality of the dispersion of the modified TiO2 nanoparticles was evaluated by atomic force microscopy. The dispersion of the P3HT-coated TiO2 NPs in the P3HT matrix was found to be homogeneous, and the fibrillar structure of the P3HT matrix was maintained which is favorable for charge transport. Fluorescence quenching measurements on these hybrid materials in CHCl3 indicated improved photoinduced electron-transfer efficiency. All in all, better physicochemical properties for P3HT/TiO2 hybrid material were reached via the surface-initiated "grafted-from" approach compared to the "grafting-onto" approach.

Physicochemical characterization of D-mannitol polymorphs: the challenging surface energy determination by inverse gas chromatography in the infinite dilution region.

PubMed

Cares-Pacheco, M G; Vaca-Medina, G; Calvet, R; Espitalier, F; Letourneau, J-J; Rouilly, A; Rodier, E

2014-11-20

Nowadays, it is well known that surface interactions play a preponderant role in mechanical operations, which are fundamental in pharmaceutical processing and formulation. Nevertheless, it is difficult to correlate surface behaviour in processes to physical properties measurement. Indeed, most pharmaceutical solids have multiple surface energies because of varying forms, crystal faces and impurities contents or physical defects, among others. In this paper, D-mannitol polymorphs (α, β and δ) were studied through different characterization techniques highlighting bulk and surface behaviour differences. Due to the low adsorption behaviour of β and δ polymorphs, special emphasis has been paid to surface energy analysis by inverse gas chromatography, IGC. Surface energy behaviour has been studied in Henry's domain showing that, for some organic solids, the classical IGC infinite dilution zone is never reached. IGC studies highlighted, without precedent in literature, dispersive surface energy differences between α and β mannitol, with a most energetically active α form with a γ(s)(d) of 74.9 mJ·m⁻². Surface heterogeneity studies showed a highly heterogeneous α mannitol with a more homogeneous β (40.0 mJ·m⁻²) and δ mannitol (40.3 mJ·m⁻²). Moreover, these last two forms behaved similarly considering surface energy at different probe concentrations. Copyright © 2014 Elsevier B.V. All rights reserved.

Application of hot melt extrusion for improving bioavailability of artemisinin a thermolabile drug.

PubMed

Kulkarni, C; Kelly, A L; Gough, T; Jadhav, V; Singh, K K; Paradkar, A

2018-02-01

Hot melt extrusion has been used to produce a solid dispersion of the thermolabile drug artemisinin. Formulation and process conditions were optimized prior to evaluation of dissolution and biopharmaceutical performance. Soluplus ® , a low T g amphiphilic polymer especially designed for solid dispersions enabled melt extrusion at 110 °C although some drug-polymer incompatibility was observed. Addition of 5% citric acid as a pH modifier was found to suppress the degradation. The area under plasma concentration time curve (AUC 0-24h ) and peak plasma concentration (C max ) were four times higher for the modified solid dispersion compared to that of pure artemisinin.

Ultra-pure, water-dispersed Au nanoparticles produced by femtosecond laser ablation and fragmentation

PubMed Central

Kubiliūtė, Reda; Maximova, Ksenia A; Lajevardipour, Alireza; Yong, Jiawey; Hartley, Jennifer S; Mohsin, Abu SM; Blandin, Pierre; Chon, James WM; Sentis, Marc; Stoddart, Paul R; Kabashin, Andrei; Rotomskis, Ričardas; Clayton, Andrew HA; Juodkazis, Saulius

2013-01-01

Aqueous solutions of ultra-pure gold nanoparticles have been prepared by methods of femtosecond laser ablation from a solid target and fragmentation from already formed colloids. Despite the absence of protecting ligands, the solutions could be (1) fairly stable and poly size-dispersed; or (2) very stable and monodispersed, for the two fabrication modalities, respectively. Fluorescence quenching behavior and its intricacies were revealed by fluorescence lifetime imaging microscopy in rhodamine 6G water solution. We show that surface-enhanced Raman scattering of rhodamine 6G on gold nanoparticles can be detected with high fidelity down to micromolar concentrations using the nanoparticles. Application potential of pure gold nanoparticles with polydispersed and nearly monodispersed size distributions are discussed. PMID:23888114

Dissolution enhancement of efavirenz by solid dispersion and PEGylation techniques

PubMed Central

Madhavi, B. Bindu; Kusum, B.; Chatanya, CH. Krishna; Madhu, M. Naga; Harsha, V. Sri; Banji, David

2011-01-01

Background: Efavirenz is the preferred nonnucleotide reverse transcriptase inhibitor for first-line antiretroviral treatment in many countries. It is orally active and is specific for human immunodeficiency virus type 1. Its effectiveness can be attributed to its long half-life, which is 52–76 h after multiple doses. The drug is having poor water solubility. The formulation of poorly soluble drug for oral delivery will be one of the biggest challenges for formulation scientists in the research field. Among the available approaches, the solid dispersion technique has often proved to be the most commonly used method in improving dissolution and bioavailability of the drugs because of its simplicity and economy in preparation and evaluation. Materials and Methods: Solid dispersions were prepared by solvent evaporation and physical mixture methods by using polyethylene glycol as the hydrophilic carrier and PEGylated product was also prepared. The prepared products were evaluated for various parameters, such as polymer interaction, saturation solubility study, and drug release studies. The drug release data were analyzed by fitting it into various kinetic models. Results: There is an improvement in the dissolution from 16% to 70% with solid dispersion technology. Higuchi model was found to be the best fit model. Conclusion: Solid dispersion is the simple, efficient, and economic method to improve the dissolution of the poorly water-soluble drugs. PMID:23071917

Solubility Enhancement of a Poorly Water Soluble Drug by Forming Solid Dispersions using Mechanochemical Activation

PubMed Central

Rojas-Oviedo, I.; Retchkiman-Corona, B.; Quirino-Barreda, C. T.; Cárdenas, J.; Schabes-Retchkiman, P. S.

2012-01-01

Mechanochemical activation is a practical cogrinding operation used to obtain a solid dispersion of a poorly water soluble drug through changes in the solid state molecular aggregation of drug-carrier mixtures and the formation of noncovalent interactions (hydrogen bonds) between two crystalline solids such as a soluble carrier, lactose, and a poorly soluble drug, indomethacin, in order to improve its solubility and dissolution rate. Samples of indomethacin and a physical mixture with a weight ratio of 1:1 of indomethacin and lactose were ground using a high speed vibrating ball mill. Particle size was determined by electron microscopy, the reduction of crystallinity was determined by calorimetry and transmission electron microscopy, infrared spectroscopy was used to find evidence of any interactions between the drug and the carrier and the determination of apparent solubility allowed for the corroboration of changes in solubility. Before grinding, scanning electron microscopy showed the drug and lactose to have an average particle size of around 50 and 30 μm, respectively. After high speed grinding, indomethacin and the mixture had a reduced average particle size of around 5 and 2 μm, respectively, showing a morphological change. The ground mixture produced a solid dispersion that had a loss of crystallinity that reached 81% after 30 min of grinding while the drug solubility of indomethacin within the solid dispersion increased by 2.76 fold as compared to the pure drug. Drug activation due to hydrogen bonds between the carboxylic group of the drug and the hydroxyl group of lactose as well as the decrease in crystallinity of the solid dispersion and the reduction of the particle size led to a better water solubility of indomethacin. PMID:23798775

Ultrathin-shell boron nitride hollow spheres as sorbent for dispersive solid-phase extraction of polychlorinated biphenyls from environmental water samples.

PubMed

Fu, Meizhen; Xing, Hanzhu; Chen, Xiangfeng; Chen, Fan; Wu, Chi-Man Lawrence; Zhao, Rusong; Cheng, Chuange

2014-11-21

Boron nitride hollow spheres with ultrathin-shells were synthesized and used as sorbents for dispersive solid-phase extraction of aromatic pollutants at trace levels from environmental water samples. Polychlorinated biphenyls (PCBs) were selected as target compounds. Sample quantification and detection were performed by gas chromatography-tandem mass spectrometry. Extraction parameters influencing the extraction efficiency were optimized through response surface methodology using the Box-Behnken design. The proposed method achieved good linearity within the concentration range of 0.15-250 ng L(-1) PCBs, low limits of detection (0.04-0.09 ng L(-1), S/N=3:1), good repeatability of the extractions (relative standard deviation, <12%, n=6), and satisfactory recoveries between 84.9% and 101.0% under optimal conditions. Real environmental samples collected from rivers, local lakes, rain and spring waters were analyzed using the developed method. Results demonstrated that the hexagonal boron nitride-based material has significant potential as a sorbent for organic pollutant extraction from environmental water samples. Copyright © 2014 Elsevier B.V. All rights reserved.

A high performance quasi-solid-state supercapacitor based on CuMnO2 nanoparticles

NASA Astrophysics Data System (ADS)

Wang, Lu; Arif, Muhammad; Duan, Guorong; Chen, Shenming; Liu, Xiaoheng

2017-07-01

Mixed metal or transition metal oxides hold an unveiled potential as one of the most promising energy storage material because of their excellent stability, reliable conductivity, and convenient use. In this work, CuMnO2 nanoparticles are successfully prepared by a facile hydrothermal process with the help of dispersing agent cetyltrimethylammonium bromide (CTAB). CuMnO2 nanoparticles possess a uniform quadrilateral shape, small size (approximately 25 × 25 nm-35 × 35 nm), excellent dispersity, and large specific surface specific (56.9 m2 g-1) with an interparticle mesoporous structure. All these characteristics can bring benefit for their application in supercapacitor. A quasi-solid-state symmetric supercapacitor device is assembled by using CuMnO2 nanoparticles as both positive electrode and negative electrode. The device exhibits good supercapacitive performance with a high specific capacitance (272 F g-1), a maximum power density of 7.56 kW kg-1 and a superior cycling stability of 18,000 continuous cycles, indicating an excellent potential to be used in energy storage device.

Dissolution and oral bioavailability enhancement of praziquantel by solid dispersions.

PubMed

Liu, Yanyan; Wang, Tianzi; Ding, Wenya; Dong, Chunliu; Wang, Xiaoting; Chen, Jianqing; Li, Yanhua

2018-06-01

The aim of the present investigation was to enhance the solubility, dissolution, and oral bioavailability of praziquantel (PZQ), a poorly water-soluble BCS II drug (Biopharmaceutical Classification System), using a solid dispersion (SD) technique involving hydrophilic copolymers. The SD formulations were prepared by a solvent evaporation method with PZQ and PEG 4000 (polyethylene glycol 4000), PEG 6000, or P 188 polymers at various weight ratios or a combination of PEG 4000/P 188. The optimized SD formulation, which had the highest solubility in distilled water, was further characterized by its surface morphology, crystallinity, and dissolution in 0.1 M HCl with 0.2% w/v of sodium dodecyl sulfate (SDS). X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) revealed the amorphous form of PZQ in the SDs. Moreover, at an oral dosage of 5 mg/kg PZQ, the SDs had higher C max values and areas under the curve (AUCs) compared to those of commercial PZQ tablets. Preparation of PZQ-loaded SDs using PEG 4000/P 188 is a promising strategy to improve the oral bioavailability of PZQ.

Atypical effects of incorporated surfactants on stability and dissolution properties of amorphous polymeric dispersions.

PubMed

Al-Obaidi, Hisham; Lawrence, M Jayne; Buckton, Graham

2016-11-01

To understand the impact of ionic and non-ionic surfactants on the dissolution and stability properties of amorphous polymeric dispersions using griseofulvin (GF) as a model for poorly soluble drugs. Solid dispersions of the poorly water-soluble drug, griseofulvin (GF) and the polymers, poly(vinylpyrrolidone) (PVP) and poly(2-hydroxypropyl methacrylate) (PHPMA), have been prepared by spray drying and bead milling and the effect of the ionic and non-ionic surfactants, namely sodium dodecyl sulphate (SDS) and Tween-80, on the physico-chemical properties of the solid dispersions studied. The X-ray powder diffraction data and hot-stage microscopy showed a fast re-crystallisation of GF. While dynamic vapour sorption (DVS) measurements indicated an increased water uptake, slow dissolution rates were observed for the solid dispersions incorporating surfactants. The order by which surfactants free dispersions were prepared seemed critical as indicated by DVS and thermal analysis. Dispersions prepared by milling with SDS showed significantly better stability than spray-dried dispersions (drug remained amorphous for more than 6 months) as well as improved dissolution profile. We suggest that surfactants can hinder the dissolution by promoting aggregation of polymeric chains, however that effect depends mainly on how the particles were prepared. © 2016 Royal Pharmaceutical Society.

Polyurethanes from fluoroalkyl propyleneglycol polyethers

NASA Technical Reports Server (NTRS)

Trischler, F. D. (Inventor)

1969-01-01

A description is given of highly stable polyurethane polymers prepared by reacting a polyether with a diisocyanate. Compounded stocks of these polymers may be shaped and cured in conventional equipment used in the rubber industry. The solutions are dispersed gels prepared from the polymers and may be used for forming supported or unsupported films for coating fabrics or solid surfaces, and for forming adhesive bonds between a wide variety of plastics, elastomers, fabrics, metals, wood, leather, ceramics and the like.

Enabling thermal processing of ritonavir-polyvinyl alcohol amorphous solid dispersions by KinetiSol® Dispersing.

PubMed

LaFountaine, Justin S; Jermain, Scott V; Prasad, Leena Kumari; Brough, Chris; Miller, Dave A; Lubda, Dieter; McGinity, James W; Williams, Robert O

2016-04-01

Polyvinyl alcohol has received little attention as a matrix polymer in amorphous solid dispersions (ASDs) due to its thermal and rheological limitations in extrusion processing and limited organic solubility in spray drying applications. Additionally, in extrusion processing, the high temperatures required to process often exclude thermally labile APIs. The purpose of this study was to evaluate the feasibility of processing polyvinyl alcohol amorphous solid dispersions utilizing the model compound ritonavir with KinetiSol® Dispersing (KSD) technology. The effects of KSD rotor speed and ejection temperature on the physicochemical properties of the processed material were evaluated. Powder X-ray diffraction and modulated differential scanning calorimetry were used to confirm amorphous conversion. Liquid chromatography-mass spectroscopy was used to characterize and identify degradation pathways of ritonavir during KSD processing and (13)C nuclear magnetic resonance spectroscopy was used to investigate polymer stability. An optimal range of processing conditions was found that resulted in amorphous product and minimal to no drug and polymer degradation. Drug release of the ASD produced from the optimal processing conditions was evaluated using a non-sink, pH-shift dissolution test. The ability to process amorphous solid dispersions with polyvinyl alcohol as a matrix polymer will enable further investigations of the polymer's performance in amorphous systems for poorly water-soluble compounds. Copyright © 2016 Elsevier B.V. All rights reserved.

End Functionalized Nonionic Water-Dispersible Conjugated Polymers.

PubMed

Zhan, Ruoyu; Liu, Bin

2017-09-01

2,7-Dibromofluorene monomers carrying two or four oligo(ethylene glycol) (OEG) side chains are synthesized. Heck coupling between the monomers and 1,4-divinylbenzene followed by end capping with [4-(4-bromophenoxy)butyl]carbamic acid tert-butyl ester leads to two nonionic water-dispersible poly(fluorene-alt-1,4-divinylenephenylene)s end-functionalized with amine groups after hydrolysis. In water, the polymer with a lower OEG density (P1) has poor water dispersibility with a quantum yield of 0.24, while the polymer with a higher OEG density (P2) possesses excellent water-dispersibility with a high quantum yield of 0.45. Both polymers show fluorescence enhancement and blue-shifted absorption and emission maxima in the presence of surfactant sodium dodecyl sulfate and dodecyltrimethylammonium bromide. The polymers are also resistant to ionic strength with minimal nonspecific interactions to bovine serum albumin. When biotin is incorporated into the end of the polymer backbones through N-hydroxysuccinimide/amine coupling reaction, the biotinylated polymers interact specifically with streptavidin on solid surface. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kobayashi, Takeshi; Singappuli-Arachchige, Dilini; Wang, Zhuoran

Solid-state NMR spectroscopy, both conventional and dynamic nuclear polarization (DNP)-enhanced, was employed to study the spatial distribution of organic functional groups attached to the surface of mesoporous silica nanoparticles via co-condensation and grafting. The most revealing information was provided by DNP-enhanced two-dimensional 29Si– 29Si correlation measurements, which unambiguously showed that post-synthesis grafting leads to a more homogeneous dispersion of propyl and mercaptopropyl functionalities than co-condensation. Furthermore, during the anhydrous grafting process, the organosilane precursors do not self-condense and are unlikely to bond to the silica surface in close proximity (less than 4 Å) due to the limited availability of suitablymore » arranged hydroxyl groups.« less

Surface instabilities in shock loaded granular media

NASA Astrophysics Data System (ADS)

Kandan, K.; Khaderi, S. N.; Wadley, H. N. G.; Deshpande, V. S.

2017-12-01

The initiation and growth of instabilities in granular materials loaded by air shock waves are investigated via shock-tube experiments and numerical calculations. Three types of granular media, dry sand, water-saturated sand and a granular solid comprising PTFE spheres were experimentally investigated by air shock loading slugs of these materials in a transparent shock tube. Under all shock pressures considered here, the free-standing dry sand slugs remained stable while the shock loaded surface of the water-saturated sand slug became unstable resulting in mixing of the shocked air and the granular material. By contrast, the PTFE slugs were stable at low pressures but displayed instabilities similar to the water-saturated sand slugs at higher shock pressures. The distal surfaces of the slugs remained stable under all conditions considered here. Eulerian fluid/solid interaction calculations, with the granular material modelled as a Drucker-Prager solid, reproduced the onset of the instabilities as seen in the experiments to a high level of accuracy. These calculations showed that the shock pressures to initiate instabilities increased with increasing material friction and decreasing yield strain. Moreover, the high Atwood number for this problem implied that fluid/solid interaction effects were small, and the initiation of the instability is adequately captured by directly applying a pressure on the slug surface. Lagrangian calculations with the directly applied pressures demonstrated that the instability was caused by spatial pressure gradients created by initial surface perturbations. Surface instabilities are also shown to exist in shock loaded rear-supported granular slugs: these experiments and calculations are used to infer the velocity that free-standing slugs need to acquire to initiate instabilities on their front surfaces. The results presented here, while in an idealised one-dimensional setting, provide physical understanding of the conditions required to initiate instabilities in a range of situations involving the explosive dispersion of particles.

Stirring-controlled solidified floating solid-liquid drop microextraction as a new solid phase-enhanced liquid-phase microextraction method by exploiting magnetic carbon nanotube-nickel hybrid.

PubMed

Ghazaghi, Mehri; Mousavi, Hassan Zavvar; Shirkhanloo, Hamid; Rashidi, Alimorad

2017-01-25

A specific technique is introduced to overcome limitations of classical solidification of floating organic drop microextraction, such as tedious and time-consuming centrifuge step and using disperser solvent, by facile and efficient participation of solid and liquid phases. In this proposed method of stirring-controlled solidified floating solid-liquid drop microextraction (SC-SF-SLDME), magnetic carbon nanotube-nickel hybrid (MNi-CNT) as a solid part of the extractors are dispersed ultrasonically in sample solution, and the procedure followed by dispersion of liquid phase (1-undecanol) through high-rate stirring and easily recollection of MNi-CNT in organic solvent droplets through hydrophobic force. With the reduction in speed of stirring, one solid-liquid drop is formed on top of the solution. MNi-CNT acts as both extractor and the coalescence helper between organic droplets for a facile recollection. MNi-CNT was prepared by spray pyrolysis of nickel oleate/toluene mixture at 1000 °C. Four tyrosine kinase inhibitors were selected as model analytes and the effecting parameters were investigated. The results confirmed that magnetic nanoadsorbent has an important role in the procedure and complete collection of dispersed solvent is not achieved in the absence of the solid phase. Also, short extraction time exhibited success of the proposed method and effect of dispersed solid/liquid phases. The limits of quantification (LOQs) for imatinib, sunitinib, erlotinib, and nilotinib were determined to be as low as 0.7, 1.7, 0.6, and 1.0 μg L -1 , respectively. The intra-day precisions (RSDs) were lower than 4.5%. Method performance was investigated by determination of mentioned tyrosine kinase inhibitors (TKIs) in human serum and cerebrospinal fluid samples with good recoveries in the range of 93-98%. Copyright © 2016 Elsevier B.V. All rights reserved.

Morphological instability of a thermophoretically growing deposit

NASA Technical Reports Server (NTRS)

Castillo, Jose L.; Garcia-Ybarra, Pedro L.; Rosner, Daniel E.

1992-01-01

The stability of the planar interface of a structureless solid growing from a depositing component dilute in a carrier fluid is studied when the main solute transport mechanism is thermal (Soret) diffusion. A linear stability analysis, carried out in the limit of low growth Peclet number, leads to a dispersion relation which shows that the planar front is unstable either when the thermal diffusion factor of the condensing component is positive and the latent heat release is small or when the thermal diffusion factor is negative and the solid grows over a thermally-insulating substrate. Furthermore, the influence of interfacial energy effects and constitutional supersaturation in the vicinity of the moving interface is analyzed in the limit of very small Schmidt numbers (small solute Fickian diffusion). The analysis is relevant to physical vapor deposition of very massive species on cold surfaces, as in recent experiments of organic solid film growth under microgravity conditions.

Rayleigh-type waves in nonlocal micropolar solid half-space.

PubMed

Khurana, Aarti; Tomar, S K

2017-01-01

Propagation of Rayleigh type surface waves in nonlocal micropolar elastic solid half-space has been investigated. Two modes of Rayleigh-type waves are found to propagate under certain approximations. Frequency equations of these Rayleigh type modes and their conditions of existence have been derived. These frequency equations are found to be dispersive in character due to the presence of micropolarity and nonlocality parameters in the medium. One of the frequency equations is a counterpart of the classical Rayleigh waves and the other is new and has appeared due to micropolarity of the medium. Phase speeds of these waves are computed numerically for Magnesium crystal and their variation against wavenumber are presented graphically. Comparisons have been made between the phase speeds of Rayleigh type waves through nonlocal micropolar, local micropolar and elastic solid half-spaces. Copyright © 2016 Elsevier B.V. All rights reserved.

Molecularly Imprinted Nanomicrospheres as Matrix Solid-Phase Dispersant Combined with Gas Chromatography for Determination of Four Phosphorothioate Pesticides in Carrot and Yacon

PubMed Central

Zhou, Mengchun; Hu, Nana; Shu, Shaohua; Wang, Mo

2015-01-01

An efficient, rapid, and selective method for sample pretreatment, namely, molecularly imprinted matrix solid-phase dispersion (MI-MSPD) coupled with gas chromatography (GC), was developed for the rapid isolation of four phosphorothioate organophosphorus pesticides (tolclofos-methyl, phoxim, chlorpyrifos, and parathion-methyl) from carrot and yacon samples. New molecularly imprinted polymer nanomicrospheres were synthesized by using typical structural analogue tolclofos-methyl as a dummy template via surface grafting polymerization on nanosilica. Then, these four pesticides in carrot and yacon were extracted and adsorbed using the imprinted nanomicrospheres and further determined by gas chromatography. Under the optimized conditions, a good linearity of four pesticides was obtained in a range of 0.05–17.0 ng·g−1 with R varying from 0.9971 to 0.9996, and the detection limit of the method was 0.012~0.026 ng·g−1 in carrot and yacon samples. The recovery rates at two spiked levels were in the range of 85.4–105.6% with RSD ≤9.6%. The presented MI-MSPD method combined the advantages of MSPD for allowing the extraction, dispersion, and homogenization in two steps and the advantages of MIPs for high affinity and selectivity towards four phosphorothioate pesticides, which could be applied to the determination of pesticide residues in complicated vegetal samples. PMID:25954569

Molecularly imprinted nanomicrospheres as matrix solid-phase dispersant combined with gas chromatography for determination of four phosphorothioate pesticides in carrot and yacon.

PubMed

Zhou, Mengchun; Hu, Nana; Shu, Shaohua; Wang, Mo

2015-01-01

An efficient, rapid, and selective method for sample pretreatment, namely, molecularly imprinted matrix solid-phase dispersion (MI-MSPD) coupled with gas chromatography (GC), was developed for the rapid isolation of four phosphorothioate organophosphorus pesticides (tolclofos-methyl, phoxim, chlorpyrifos, and parathion-methyl) from carrot and yacon samples. New molecularly imprinted polymer nanomicrospheres were synthesized by using typical structural analogue tolclofos-methyl as a dummy template via surface grafting polymerization on nanosilica. Then, these four pesticides in carrot and yacon were extracted and adsorbed using the imprinted nanomicrospheres and further determined by gas chromatography. Under the optimized conditions, a good linearity of four pesticides was obtained in a range of 0.05-17.0 ng·g(-1) with R varying from 0.9971 to 0.9996, and the detection limit of the method was 0.012~0.026 ng·g(-1) in carrot and yacon samples. The recovery rates at two spiked levels were in the range of 85.4-105.6% with RSD ≤9.6%. The presented MI-MSPD method combined the advantages of MSPD for allowing the extraction, dispersion, and homogenization in two steps and the advantages of MIPs for high affinity and selectivity towards four phosphorothioate pesticides, which could be applied to the determination of pesticide residues in complicated vegetal samples.

Using Supercritical Fluid Technology (SFT) in Preparation of Tacrolimus Solid Dispersions.

PubMed

Obaidat, Rana M; Tashtoush, Bassam M; Awad, Alaa Abu; Al Bustami, Rana T

2017-02-01

Tacrolimus is an immunosuppressant agent that suffers from poor and variable bioavailability. This can be related to limited solubility and dissolution. The main objective of this study is to use SFT to prepare solid dispersions of tacrolimus in order to enhance its dissolution. SFT was selected since it offers several advantages over conventional techniques such as efficiency and stability. Several solid dispersions of tacrolimus were prepared using SFT to enhance its dissolution. The selected polymers included soluplus, PVP, HPMC, and porous chitosan. TPGS was used as a surfactant additive with chitosan, HPMC, and PVP. Soluplus dispersions were used to study the effect of processing parameters (time, temperature, and pressure) on loading efficiency (LE) and dissolution of the preparation. Physicochemical characterization was performed using DSC, X-ray diffraction, FTIR analysis, SEM, and in vitro drug release. Stability testing was evaluated after 3 months for selected dispersions. Significant improvement for the release profile was achieved for the prepared dispersions. Better release achieved in the soluplus dispersions which reached maximum cumulative release equal to 98.76% after 24 h. Drug precipitated in its amorphous form in all prepared dispersions except those prepared from chitosan. All dispersions were physically stable except for PVP preparations that contained TPGS which started to re-crystallize after one month. Prepared dispersions were proved to be affected by supercritical processing parameters. In conclusion, SFT was successfully used to prepare dispersions of tacrolimus that exhibited higher dissolution than raw drug. Dissolution rate and stability are affected by the type of the polymer.

The Effect of Water and Confinement on Self-Assembly of Imidazolium Based Ionic Liquids at Mica Interfaces

PubMed Central

Cheng, H.-W.; Dienemann, J.-N.; Stock, P.; Merola, C.; Chen, Y.-J.; Valtiner, M.

2016-01-01

Tuning chemical structure and molecular layering of ionic liquids (IL) at solid interfaces offers leverage to tailor performance of ILs in applications such as super-capacitors, catalysis or lubrication. Recent experimental interpretations suggest that ILs containing cations with long hydrophobic tails form well-ordered bilayers at interfaces. Here we demonstrate that interfacial bilayer formation is not an intrinsic quality of hydrophobic ILs. In contrast, bilayer formation is triggered by boundary conditions including confinement, surface charging and humidity present in the IL. Therefore, we performed force versus distance profiles using atomic force microscopy and the surface forces apparatus. Our results support models of disperse low-density bilayer formation in confined situations, at high surface charging and/or in the presence of water. Conversely, interfacial structuring of long-chain ILs in dry environments and at low surface charging is disordered and dominated by bulk structuring. Our results demonstrate that boundary conditions such as charging, confinement and doping by impurities have decisive influence on structure formation of ILs at interfaces. As such, these results have important implications for understanding the behavior of solid/IL interfaces as they significantly extend previous interpretations. PMID:27452615

The Effect of Water and Confinement on Self-Assembly of Imidazolium Based Ionic Liquids at Mica Interfaces.

PubMed

Cheng, H-W; Dienemann, J-N; Stock, P; Merola, C; Chen, Y-J; Valtiner, M

2016-07-25

Tuning chemical structure and molecular layering of ionic liquids (IL) at solid interfaces offers leverage to tailor performance of ILs in applications such as super-capacitors, catalysis or lubrication. Recent experimental interpretations suggest that ILs containing cations with long hydrophobic tails form well-ordered bilayers at interfaces. Here we demonstrate that interfacial bilayer formation is not an intrinsic quality of hydrophobic ILs. In contrast, bilayer formation is triggered by boundary conditions including confinement, surface charging and humidity present in the IL. Therefore, we performed force versus distance profiles using atomic force microscopy and the surface forces apparatus. Our results support models of disperse low-density bilayer formation in confined situations, at high surface charging and/or in the presence of water. Conversely, interfacial structuring of long-chain ILs in dry environments and at low surface charging is disordered and dominated by bulk structuring. Our results demonstrate that boundary conditions such as charging, confinement and doping by impurities have decisive influence on structure formation of ILs at interfaces. As such, these results have important implications for understanding the behavior of solid/IL interfaces as they significantly extend previous interpretations.

Comparative Analysis of Hexagonal Solid Silica and Nitro-benzene Filled Hollow Core Photonic Crystal Fiber

NASA Astrophysics Data System (ADS)

Shahiruddin; Singh, Dharmendra K.; Hassan, M. A.

2018-02-01

A comparative study of five ring solid core and nitrobenzene filled hollow core liquid filled photonic crystal fiber (PCF) are presented. Considering the same structure, one is used as solid silica and another one is filled with nitrobenzene in the core. Here the paper elaborates the confinement loss, dispersion properties and birefringence of an index-guiding PCF with asymmetric cladding designed and analyzed by the finite-element method. The proposed structure shows the low confinement loss in case of solid silica, negative dispersion in nitrobenzene filled hollow core PCF and high birefringence in both the cases. The calculated values shows flat zero confinement loss in 0.7 µm to 1.54 µm range, flat zero dispersion is achieved in solid core and -2000 ps/km-nm in nitrobenzene filled hollow core PCF and high birefringence in the range of 10-3 in nitrobenzene filled hollow core PCF. Results show the relative analysis at different air fill fraction.

Enhanced visible light-induced photocatalytic activity of surface-modified BiOBr with Pd nanoparticles

NASA Astrophysics Data System (ADS)

Meng, Xiangchao; Li, Zizhen; Chen, Jie; Xie, Hongwei; Zhang, Zisheng

2018-03-01

Palladium nanoparticles well-dispersed on BiOBr surfaces were successfully prepared via a two-step process, namely hydrothermal synthesis of BiOBr followed by photodeposition of palladium. Surface-exposed palladium nanoparticles may improve the harvesting capacity of visible light photons via the surface plasmonic resonance effect to produce extra electrons. Palladium is an excellent electron acceptor, and therefore favours the separation of photogenerated electron/hole pairs. As a result, palladium significantly improves the photocatalytic activity of BiOBr in the removal of organic pollutants (phenol) under visible light irradiation. In addition to as-prepared samples which were comprehensively characterized, the mechanism for the enhancement via the deposition of palladium nanoparticles was also proposed based on results. This work may serve as solid evidence to confirm that surface-deposited palladium nanoparticles are capable of improving photocatalytic activity, and that photodeposition may be an effective approach to load metal nanoparticles onto a surface.

Thermodynamic phase behavior of API/polymer solid dispersions.

PubMed

Prudic, Anke; Ji, Yuanhui; Sadowski, Gabriele

2014-07-07

To improve the bioavailability of poorly soluble active pharmaceutical ingredients (APIs), these materials are often integrated into a polymer matrix that acts as a carrier. The resulting mixture is called a solid dispersion. In this work, the phase behaviors of solid dispersions were investigated as a function of the API as well as of the type and molecular weight of the carrier polymer. Specifically, the solubility of artemisinin and indomethacin was measured in different poly(ethylene glycol)s (PEG 400, PEG 6000, and PEG 35000). The measured solubility data and the solubility of sulfonamides in poly(vinylpyrrolidone) (PVP) K10 and PEG 35000 were modeled using the perturbed-chain statistical associating fluid theory (PC-SAFT). The results show that PC-SAFT predictions are in a good accordance with the experimental data, and PC-SAFT can be used to predict the whole phase diagram of an API/polymer solid dispersion as a function of the kind of API and polymer and of the polymer's molecular weight. This remarkably simplifies the screening process for suitable API/polymer combinations.

Evaluation of the recrystallization kinetics of hot-melt extruded polymeric solid dispersions using an improved Avrami equation

PubMed Central

Feng, Xin; Ye, Xingyou; Park, Jun-Bom; Lu, Wenli; Morott, Joe; Beissner, Brad; Lian, Zhuoyang John; Pinto, Elanor; Bi, Vivian; Porter, Stu; Durig, Tom; Majumdar, Soumyajit; Repka, Michael A.

2017-01-01

The recrystallization of an amorphous drug in a solid dispersion system could lead to a loss in the drug solubility and bioavailability. The primary objective of the current research was to use an improved kinetic model to evaluate the recrystallization kinetics of amorphous structures and to further understand the factors influencing the physical stability of amorphous solid dispersions. Amorphous solid dispersions of fenofibrate with different molecular weights of hydroxypropylcellulose, HPC (Klucel™ LF, EF, ELF) were prepared utilizing hot-melt extrusion technology. Differential scanning calorimetry was utilized to quantitatively analyze the extent of recrystallization in the samples stored at different temperatures and relative humidity (RH) conditions. The experimental data were fitted into the improved kinetics model of a modified Avrami equation to calculate the recrystallization rate constants. Klucel LF, the largest molecular weight among the HPCs used, demonstrated the greatest inhibition of fenofibrate recrystallization. Additionally, the recrystallization rate (k) decreased with increasing polymer content, however exponentially increased with higher temperature. Also k increased linearly rather than exponentially over the range of RH studied. PMID:25224341

Evaluation of the recrystallization kinetics of hot-melt extruded polymeric solid dispersions using an improved Avrami equation.

PubMed

Feng, Xin; Ye, Xingyou; Park, Jun-Bom; Lu, Wenli; Morott, Joe; Beissner, Brad; Lian, Zhuoyang John; Pinto, Elanor; Bi, Vivian; Porter, Stu; Durig, Tom; Majumdar, Soumyajit; Repka, Michael A

2015-01-01

The recrystallization of an amorphous drug in a solid dispersion system could lead to a loss in the drug solubility and bioavailability. The primary objective of the current research was to use an improved kinetic model to evaluate the recrystallization kinetics of amorphous structures and to further understand the factors influencing the physical stability of amorphous solid dispersions. Amorphous solid dispersions of fenofibrate with different molecular weights of hydroxypropylcellulose, HPC (Klucel™ LF, EF, ELF) were prepared utilizing hot-melt extrusion technology. Differential scanning calorimetry was utilized to quantitatively analyze the extent of recrystallization in the samples stored at different temperatures and relative humidity (RH) conditions. The experimental data were fitted into the improved kinetics model of a modified Avrami equation to calculate the recrystallization rate constants. Klucel LF, the largest molecular weight among the HPCs used, demonstrated the greatest inhibition of fenofibrate recrystallization. Additionally, the recrystallization rate (k) decreased with increasing polymer content, however exponentially increased with higher temperature. Also k increased linearly rather than exponentially over the range of RH studied.

Physicochemical characterization of solid dispersions of carbamazepine formulated by supercritical carbon dioxide and conventional solvent evaporation method.

PubMed

Sethia, Sundeep; Squillante, Emilio

2002-09-01

Solid dispersions of carbamazepine (CBZ) were formulated by supercritical fluid processing (SCP) and conventional solvent evaporation in polyethylene glycol (PEG) 8000 with either Gelucire 44/14 or vitamin E TPGS NF (d-alpha-tocopheryl PEG 1000 succinate). Formulations were evaluated by dissolution, scanning electron microscopy, powder X-ray diffraction, and differential scanning calorimetry, and excipient cytotoxicity in Caco-2 cells by MTS [3-(4,5-dimethylthiazol-2-yl)-5-(3-carboxymethoxyphenyl)-2-(4-sulfophenyl)-2H-tetrazolium, inner salt] assay. CBZ release was enhanced from supercritical fluid-treated CBZ and the CBZ/PEG 8000 (1:5), CBZ/PEG 8000/TPGS or Gelucire 44/14 (1:4:1) solid dispersions. The radically altered morphologies of SCP samples seen by scanning electron microscopy suggested polymorphic change that was confirmed by the X-ray diffraction and differential scanning calorimetry. Disappearance of the characteristic CBZ melting peak indicated that CBZ was dissolved inside the carrier system. Polymorphic change of CBZ during SCP led to faster dissolution. Therefore, SCP provides advantages over solid dispersions prepared by conventional processes. Copyright 2002 Wiley-Liss Inc.

Modification of polydopamine-coated Fe3O4 nanoparticles with multi-walled carbon nanotubes for magnetic-μ-dispersive solid-phase extraction of antiepileptic drugs in biological matrices.

PubMed

Zhang, Ruiqi; Wang, Siming; Yang, Ye; Deng, Yulan; Li, Di; Su, Ping; Yang, Yi

2018-06-01

In this study, multi-walled carbon nanotubes were coated on the surface of magnetic nanoparticles modified by polydopamine. The synthesized composite was characterized and applied to magnetic-μ-dispersive solid-phase extraction of oxcarbazepine (OXC), phenytoin (PHT), and carbamazepine (CBZ) from human plasma, urine, and cerebrospinal fluid samples prior to analysis by a high-performance liquid chromatography-photodiode array detector. The extraction parameters were investigated and the optimum condition was obtained when the variables were set to the following: sorbent type, Fe 3 O 4 @polyDA-MWCNTs (length < 2 μm); sample pH, 6; amount of sorbent, 15 mg; sorption time, 1.5 min at room temperature; type and volume of the eluent, 2.5 mL methanol; and salt content, none added. Under the optimized conditions, the calibration curves are linear in the concentration range 2-2000 ng/mL, the limits of detection are in the range 0.4-3.1 ng/mL, and the relative standard deviations and relative recoveries of plasma (spiked at 200 ng/mL) and CSF (spiked at 50 ng/mL) are in the ranges 1.4-8.2% and 92.8-96.5%, respectively. The applicability of the method was successfully confirmed by extraction and determination of OXC, PHT, and CBZ in biological matrices. Graphical abstract Magnetic multi-walled carbon nanotube core-shell composites were applied as magnetic-μ-dispersive solid-phase extraction adsorbents for determination of antiepileptic drugs in biological matrices.

Probing hydrogen bonding in cocrystals and amorphous dispersions using (14)N-(1)H HMQC solid-state NMR.

PubMed

Tatton, Andrew S; Pham, Tran N; Vogt, Frederick G; Iuga, Dinu; Edwards, Andrew J; Brown, Steven P

2013-03-04

Cocrystals and amorphous solid dispersions have generated interest in the pharmaceutical industry as an alternative to more established solid delivery forms. The identification of intermolecular hydrogen bonding interactions in a nicotinamide palmitic acid cocrystal and a 50% w/w acetaminophen-polyvinylpyrrolidone solid dispersion are reported using advanced solid-state magic-angle spinning (MAS) NMR methods. The application of a novel (14)N-(1)H HMQC experiment, where coherence transfer is achieved via through-space couplings, is shown to identify specific hydrogen bonding motifs. Additionally, (1)H isotropic chemical shifts and (14)N electric field gradient (EFG) parameters, both accessible from (14)N-(1)H HMQC experiments, are shown to be sensitive to changes in hydrogen bonding geometry. Numerous indicators of molecular association are accessible from this experiment, including NH cross-peaks occurring from intermolecular hydrogen bonds and changes in proton chemical shifts or electric field gradient parameters. First-principles calculations using the GIPAW approach that yield accurate estimates of isotropic chemical shifts, and EFG parameters were used to assist in assignment. It is envisaged that (14)N-(1)H HMQC solid state NMR experiments could become a valuable screening technique of solid delivery forms in the pharmaceutical industry.

Both solubility and chemical stability of curcumin are enhanced by solid dispersion in cellulose derivative matrices.

PubMed

Li, Bin; Konecke, Stephanie; Wegiel, Lindsay A; Taylor, Lynne S; Edgar, Kevin J

2013-10-15

Amorphous solid dispersions (ASD) of curcumin (Cur) in cellulose derivative matrices, hydroxypropylmethylcellulose acetate succinate (HPMCAS), carboxymethylcellulose acetate butyrate (CMCAB), and cellulose acetate adipate propionate (CAAdP) were prepared in order to investigate the structure-property relationship and identify polymer properties necessary to effectively increase Cur aqueous solution concentration. XRD results indicated that all investigated solid dispersions were amorphous, even at a 9:1 Cur:polymer ratio. Both stability against crystallization and Cur solution concentration from these ASDs were significantly higher than those from physical mixtures and crystalline Cur. Remarkably, curcumin was also stabilized against chemical degradation in solution. Chemical stabilization was polymer-dependent, with stabilization in CAAdP>CMCAB>HPMCAS>PVP, while matrices enhanced solution concentration as PVP>HPMCAS>CMCAB≈CAAdP. HPMCAS/Cur dispersions have useful combinations of pH-triggered release profile, chemical stabilization, and strong enhancement of Cur solution concentration. Copyright © 2013 Elsevier Ltd. All rights reserved.

Self-assembled Gemini surfactant film-mediated dispersion stability.

PubMed

Rabinovich, Y I; Kanicky, J R; Pandey, S; Oskarsson, H; Holmberg, K; Moudgil, B M; Shah, D O

2005-08-15

The force-distance curves of 12-2-12 and 12-4-12 Gemini quaternary ammonium bromide surfactants on mica and silica surfaces obtained by atomic force microscopy (AFM) were correlated with the structure of the adsorption layer. The critical micelle concentration was measured in the presence or absence of electrolyte. The electrolyte effect (the decrease of CMC) is significantly more pronounced for Gemini than for single-chain surfactants. The maximum compressive force, F(max), of the adsorbed surfactant aggregates was determined. On the mica surface in the presence of 0.1 M NaCl, the Gemini micelles and strong repulsive barrier appear at surfactant concentrations 0.02-0.05 mM, which is significantly lower than that for the single C(12)TAB (5-10 mM). This difference between single and Gemini surfactants can be explained by a stronger adsorption energy of Gemini surfactants. The low concentration of Gemini at which this surfactant forms the strong micellar layer on the solid/solution interface proves that Gemini aggregates (micelles) potentially act as dispersing agent in processes such as chemical mechanical polishing or collector in flotation. The AFM force-distance results obtained for the Gemini surfactants were used along with turbidity measurements to determine how adsorption of Gemini surfactants affects dispersion stability. It has been shown that Gemini (or two-chain) surfactants are more effective dispersing agents, and that in the presence of electrolyte, the silica dispersion stability at pH 4.0 can also be achieved at very low surfactant concentrations ( approximately 0.02 mM).

Self dispersing mixed micelles forming systems for enhanced dissolution and intestinal permeability of hydrochlorothiazide.

PubMed

Sultan, Amal A; El-Gizawy, Sanaa A; Osman, Mohamed A; El Maghraby, Gamal M

2017-01-01

Mixed micelles provide promising strategy for enhancing dissolution and permeability of drugs. However, their fluid nature limited the stability of the loaded drug and hindered the development of stable oral dosage form. Accordingly, the objective was to develop solid self dispersing mixed micelle forming systems (MMFS) for enhanced dissolution and intestinal permeability of hydrochlorothiazide. Pseudoternary phase diagrams were constructed using sodium cholate, lecithin with either poloxamer 407 or PEG 4000 to determine the composition of MMFS. Both polymer free and poloxamer or PEG containing MMFS were prepared as homogenous matrices or as solid self dispersing powder. The later was developed by adsorption of MMFS on avicel-aerosil mixture. Differential scanning calorimetry provided an evidence for existence of hydrochlorothiazide as molecular dispersion in the MMFS. Dispersing polymer free, PEG 4000 or poloxamer based MMFS in aqueous medium produced micelles having size values of 119, 52.6 and 28nm, respectively. The zeta potential values were -61.8, -59.5 and -19.5mV for the same systems, respectively. Preparation of solid self dispersing MMFS enhanced the dissolution rate of hydrochlorothiazide. The intestinal absorption of hydrochlorothiazide from its aqueous solution and polymer incorporating mixed micellar systems was monitored using in situ rabbit intestinal perfusion technique. The permeability results showed a clear trend for enhanced membrane transport of the drug after being incorporated into poloxamer containing mixed micellar system. The study thus introduced a versatile easily formulated solid self dispersing system with high potential for solving the dissolution and permeability problems of class IV drugs. Copyright © 2016 Elsevier B.V. All rights reserved.

Method of forming components for a high-temperature secondary electrochemical cell

DOEpatents

Mrazek, F.C.; Battles, J.E.

1981-05-22

A method of forming a component for a high-temperature secondary electrochemical cell having a positive electrode including a sulfide selected from the group consisting of iron sulfides, nickel sulfides, copper sulfides and cobalt sulfides, a negative electrode including an alloy of aluminum and an electrically insulating porous separator between said electrodes is described. The improvement comprises forming a slurry of solid particles dispersed in a liquid electrolyte such as the lithium chloride-potassium chloride eutectic, casting the slurry into a form having the shape of one of the components and smoothing the exposed surface of the slurry, cooling the cast slurry to form the solid component, and removing same. Electrodes and separators can be thus formed.

Multiphase Modeling of Water Injection on Flame Deflector

NASA Technical Reports Server (NTRS)

Vu, Bruce T.; Bachchan, Nili; Peroomian, Oshin; Akdag, Vedat

2013-01-01

This paper describes the use of an Eulerian Dispersed Phase (EDP) model to simulate the water injected from the flame deflector and its interaction with supersonic rocket exhaust from a proposed Space Launch System (SLS) vehicle. The Eulerian formulation, as part of the multi-phase framework, is described. The simulations show that water cooling is only effective over the region under the liquid engines. Likewise, the water injection provides only minor effects over the surface area under the solid engines.

Micro-matrix solid-phase dispersion coupled with MEEKC for quantitative analysis of lignans in Schisandrae Chinensis Fructus using molecular sieve TS-1 as a sorbent.

PubMed

Chu, Chu; Wei, Mengmeng; Wang, Shan; Zheng, Liqiong; He, Zheng; Cao, Jun; Yan, Jizhong

2017-09-15

A simple and effective method was developed for determining lignans in Schisandrae Chinensis Fructus by using a micro-matrix solid phase dispersion (MSPD) technique coupled with microemulsion electrokinetic chromatography (MEEKC). Molecular sieve, TS-1, was applied as a solid supporting material in micro MSPD extraction for the first time. Parameters that affect extraction efficiency, such as type of dispersant, mass ratio of the sample to the dispersant, grinding time, elution solvent and volume were optimized. The optimal extraction conditions involve dispersing 25mg of powdered Schisandrae samples with 50mg of TS-1 by a mortar and pestle. A grinding time of 150s was adopted. The blend was then transferred to a solid-phase extraction cartridge and the target analytes were eluted with 500μL of methanol. Moreover, several parameters affecting MEEKC separation were studied, including the type of oil, SDS concentration, type and concentration of cosurfactant, and concentration of organic modifier. A satisfactory linearity (R>0.9998) was obtained, and the calculated limits of quantitation were less than 2.77μg/mL. Finally, the micro MSPD-MEEKC method was successfully applied to the analysis of lignans in complex Schisandrae fructus samples. Copyright © 2017 Elsevier B.V. All rights reserved.

Investigating the Interaction Pattern and Structural Elements of a Drug-Polymer Complex at the Molecular Level.

PubMed

Nie, Haichen; Mo, Huaping; Zhang, Mingtao; Song, Yang; Fang, Ke; Taylor, Lynne S; Li, Tonglei; Byrn, Stephen R

2015-07-06

Strong associations between drug and polymeric carriers are expected to contribute to higher drug loading capacities and better physical stability of amorphous solid dispersions. However, molecular details of the interaction patterns and underlying mechanisms are still unclear. In the present study, a series of amorphous solid dispersions of clofazimine (CLF), an antileprosy drug, were prepared with different polymers by applying the solvent evaporation method. When using hypromellose phthalate (HPMCP) as the carrier, the amorphous solid dispersion system exhibits not only superior drug loading capacity (63% w/w) but also color change due to strong drug-polymer association. In order to further explain these experimental observations, the interaction between CLF and HPMCP was investigated in a nonpolar volatile solvent system (chloroform) prior to forming the solid dispersion. We observed significant UV/vis and (1)H NMR spectral changes suggesting the protonation of CLF and formation of ion pairs between CLF and HPMCP in chloroform. Furthermore, nuclear Overhauser effect spectroscopy (NOESY) and diffusion order spectroscopy (DOSY) were employed to evaluate the strength of associations between drug and polymers, as well as the molecular mobility of CLF. Finally, by correlating the experimental values with quantum chemistry calculations, we demonstrate that the protonated CLF is binding to the carboxylate group of HPMCP as an ion pair and propose a possible structural model of the drug-polymer complex. Understanding the drug and carrier interaction patterns from a molecular perspective is critical for the rational design of new amorphous solid dispersions.

Using Flory-Huggins phase diagrams as a pre-formulation tool for the production of amorphous solid dispersions: a comparison between hot-melt extrusion and spray drying.

PubMed

Tian, Yiwei; Caron, Vincent; Jones, David S; Healy, Anne-Marie; Andrews, Gavin P

2014-02-01

Amorphous drug forms provide a useful method of enhancing the dissolution performance of poorly water-soluble drugs; however, they are inherently unstable. In this article, we have used Flory-Huggins theory to predict drug solubility and miscibility in polymer candidates, and used this information to compare spray drying and melt extrusion as processes to manufacture solid dispersions. Solid dispersions were prepared using two different techniques (hot-melt extrusion and spray drying), and characterised using a combination of thermal (thermogravimetric analysis and differential scanning calorimetry), spectroscopic (Fourier transform infrared spectroscopy (FTIR) and X-ray diffraction methods. Spray drying permitted generation of amorphous solid dispersions across a wider drug concentration than melt extrusion. Melt extrusion provided sufficient energy for more intimate mixing to be achieved between drug and polymer, which may improve physical stability. It was also confirmed that stronger drug-polymer interactions might be generated through melt extrusion. Remixing and dissolution of recrystallised felodipine into the polymeric matrices did occur during the modulated differential scanning calorimetry analysis, but the complementary information provided from FTIR confirms that all freshly prepared spray-dried samples were amorphous with the existence of amorphous drug domains within high drug-loaded samples. Using temperature-composition phase diagrams to probe the relevance of temperature and drug composition in specific polymer candidates facilitates polymer screening for the purpose of formulating solid dispersions. © 2013 Royal Pharmaceutical Society.

One decade of research into the fate and transport of carbon-based nanomaterials - Lessons learnt and future perspectives

NASA Astrophysics Data System (ADS)

Hüffer, Thorsten; Hofmann, Thilo

2016-04-01

Carbon-based nanomaterials (CNM) exhibit unique physico-chemical properties (e.g., large surface area to volume ratios, electron delocalization), which make them promising for a great number of applications. The production, use, and disposal of CNM and CNM-containing products will inevitably result in the release of these materials into the environment. The fate and transport of CNM greatly depends on their physico-chemical properties and surrounding environmental conditions. This field of research has constantly increased over recent years. Yet little is known on how transformation processes such as changes in surface properties or aggregation influence their interaction with other environmental species (i.e., solid surfaces or contaminants). For example, changes in redox chemistry in combination with irradiation have shown to significantly alter the surface chemistry of C60 fullerenes and consequently decreased their sorption affinity towards non-polar organic contaminants [1]. The presence of natural organic matter (NOM) seems to play a major role on the aggregation of CNM; however, the results are not consistent whether this leads to an increase or decrease in interactions with solid surfaces or contaminants. Either increased interactions resulting from a higher dispersion of CNM or decreased interactions of CNM, which was assigned to an offset of "creating" new sorption sites due to increased dispersion by a reduced accessibility of polar moieties. For the latter effect, NOM was proposed to either directly compete for sorption sites on CNM surface or a blocking of CNM pores by large NOM molecules [2]. The potential consequences of these changes in surface properties of CNM on their toxic effects on microorganisms have only been partially examined. For an environmental risk assessment, data on the occurrence of CNM is obligatory but to date the environmental concentrations of CNM are still difficult to assess due to still unsolved analytical issues in matrix separation and the discrimination of CNM from naturally present particles with similar dimensions and properties (e.g., soot or colloids). Recently, progress has been made to characterize the aggregation and to determine the occurrence of (functionalized) fullerenes using asymmetrical flow field-flow fractionation coupled to a LC-HR-MS [3]. In this contribution, the major results during the last decade of environmental research into CNM will be reviewed with the focus on their analyses and characterization, and interactions with solid surfaces. References: [1] Hüffer, T., Kah, M., Hofmann, T., Schmidt, T.C. (2013) How Redox Conditions and Irradiation Affect Sorption of PAHs by Dispersed Fullerenes (nC60). Environmental Science & Technology, 47(13), 6935-6942. [2] Hüffer, T., Schroth, S., Schmidt, T.C. (2015) Influence of humic acids on sorption of alkanes by carbon nanotubes - Implications for the dominant sorption mode. Chemosphere, 119, 1169-1175. [3] Kolkman, A., Emke, E., Bauerlein, P.S., Carboni, A., Tran, D.T., terLaak, T.L., vanWezel, A.P., deVoogt, P. (2013) Analysis of (Functionalized) Fullerenes in Water Samples by Liquid Chromatography Coupled to High-Resolution Mass Spectrometry. Analytical Chemistry, 85(12), 5867-5874.

Solid-solution CrCoCuFeNi high-entropy alloy thin films synthesized by sputter deposition

DOE PAGES

An, Zhinan; Jia, Haoling; Wu, Yueying; ...

2015-05-04

The concept of high configurational entropy requires that the high-entropy alloys (HEAs) yield single-phase solid solutions. However, phase separations are quite common in bulk HEAs. A five-element alloy, CrCoCuFeNi, was deposited via radio frequency magnetron sputtering and confirmed to be a single-phase solid solution through the high-energy synchrotron X-ray diffraction, energy-dispersive spectroscopy, wavelength-dispersive spectroscopy, and transmission electron microscopy. The formation of the solid-solution phase is presumed to be due to the high cooling rate of the sputter-deposition process.

Analysis of Rayleigh-Lamb Modes in Soft-solids with Application to Surface Wave Elastography

NASA Astrophysics Data System (ADS)

Benech, Nicolás; Grinspan, Gustavo; Aguiar, Sofía; Brum, Javier; Negreira, Carlos; tanter, Mickäel; Gennisson, Jean-Luc

The goal of Surface Wave Elastography (SE) techniques is to estimate the shear elasticity of the sample by measuring the surface wave speed. In SE the thickness of the sample is often assumed to be infinite, in this way, the surface wave speed is directly linked to the sample's shear elasticity. However for many applications this assumption is not true. In this work, we study experimentally the Rayleigh-Lamb modes in soft solids of finite thickness to explore the optimal conditions for SWE. Experiments were carried out in three tissue mimicking phantoms of different thicknesses (10 mm, 20 mm and 60 mm) and same shear elasticity. The surface waves were generated at the surface of the phantom using piston attached to a mechanical vibrator. The central frequency of the excitation was varied between 60 Hz to 160 Hz. One component of the displacement field generated by the piston was measured at the surface and in the bulk of the sample trough a standard speckle tracking technique using a 256 element, 7.5 MHz central frequency linear array and an ultrasound ultrafast electronics. Finally, by measuring the phase velocity at each excitation frequency, velocity dispersion curves were obtained for each phantom. The results show that instead of a Rayleigh wave, zero order symmetric (S0) and antisymmetric (A0) Lamb modes are excited with this type of source. Moreover, in this study we show that due to the near field effects of the source, which are appreciable only in soft solids at low frequencies, both Lamb modes are separable in time and space. We show that while the Ao mode dominates close the source, the S0 mode dominates far away.

[Pharmacokinetics and relative bioavailability of THC and THC-solid dispersion orally to mice at single dose].

PubMed

Liao, Li; Hua, Hua; Zhao, Jun-Ning; Luo, Heng; Yang, An-Dong

2014-03-01

To establish a fast sensitive, reproducible LC-MS/MS method to study pharmacokinetic properties of THC, and compare relative bioavailability of THC and its solid dispersion in mice. 200 mice were divided randomly into two groups, and administered orally with THC and THC-solid dispersion after fasting (calculate on THC:400 mg x kg(-1)), used HPLC-MS/MS method to determine the THC concentration of each period at the following times: baseline ( predose ), 15, 30, 45 min, 1, 1.5, 2, 3, 4, 6, 24 h after dosing. Calculating the pharmacokinetic parameters according to the C-t curv, and then use the Phoenix WinNonlin software for data analysis. The calibration curves were linear over the range 9.06-972 microg x L(-1) for THC (R2 = 0.999). The limit of detection (LOD) was 0.7 microg x L(-1), respectively. The average extraction recoveries for THC was above 75%, The methodology recoveries were between 79% and 108%. The intra-day and inter-day RSD were less than 13%, the stability test showed that the plasma samples was stable under different conditions (RSD < 15%). The precision, accuracy, recovery and applicability were found to be adequate for pharmacokinetic studies. Pharmacokinetic parameters of THC and THC-solid dispersion orally to mice shows as fllows: T(max), were 60 and 15 min, AUC(0-t) were 44 500.43 and 57 497.81 mg x L(-1) x min, AUC(0-infinity) were 51 226.00 and 68 031.48 mg x L(-1) x min, MRT(0-infinity) were 596.915 6, 661.747 7 min, CL(z)/F were 0.007 809 and 0.005 88 L x min(-1) x kg(-1). Compared with THC, the MRT and t1/2 of the THC-solid dispersion were all slightly extended, the t(max) was significantly reduced, AUC(0-24 h), AUC(0-infinity) and C(max) were all significantly higher, the relative bioavailability of THC-solid dispersion is 1.34 times of THC. The results of the experiment shows that the precision, accuracy, recovery and applicability were found to be adequate for the pharmacokinetic studies. After oral administration to mice, the relative bioavailability of THC-solid dispersion show significant improvement compared to THC.

Trapped-mode-induced Fano resonance and acoustical transparency in a one-dimensional solid-fluid phononic crystal

NASA Astrophysics Data System (ADS)

Quotane, Ilyasse; El Boudouti, El Houssaine; Djafari-Rouhani, Bahram

2018-01-01

We investigate theoretically and numerically the possibility of existence of Fano and acoustic-induced transparency (AIT) resonances in a simple though realistic one-dimensional acoustic structure made of solid-fluid layers inserted between two fluids. These resonances are obtained by combining appropriately the zeros of transmission (antiresonance) induced by the solid layers and the local resonances induced by the solid or combined solid-fluid layers with surface free boundary conditions. In particular, we show the possibility of trapped modes, also called bound states in continuum, which have recently found a high renewal interest. These modes appear as resonances with zero width in the transmission spectra as well as in the density of states (DOS). We consider three different structures: (i) a single solid layer inserted between two fluids. This simple structure shows the possibility of existence of trapped modes, which are discrete modes of the solid layer that lie in the continuum modes of the surrounding fluids. We give explicit analytical expressions of the dispersion relation of these eigenmodes of the solid layer which are found independent of the nature of the surrounding fluids. By slightly detuning the angle of incidence from that associated to the trapped mode, we get a well-defined Fano resonance characterized by an asymmetric Fano profile in the transmission spectra. (ii) The second structure consists of a solid-fluid-solid triple layer embedded between two fluids. This structure is found more appropriate to show both Fano and acoustic-induced transparency resonances. We provide detailed analytical expressions for the transmission and reflection coefficients that enable us to deduce a closed-form expression of the dispersion relation giving the trapped modes. Two situations can be distinguished in the triple-layer system: in the case of a symmetric structure (i.e., the same solid layers) we show, by detuning the incidence angle θ , the possibility of existence of Fano resonances that can be fitted following a Fano-type expression. The variation of the Fano parameter that describes the asymmetry of such resonances as well as their width versus θ is studied in detail. In the case of an asymmetric structure (i.e., different solid layers), we show the existence of an incidence angle that enables to squeeze a resonance between two transmission zeros induced by the two solid layers. This resonance behaves like an AIT resonance, its position and width depend on the nature of the fluid and solid layers as well as on the difference between the thicknesses of the solid layers. (iii) In the case of a periodic structure (phononic crystal), we show that trapped modes and Fano resonances give rise, respectively, to dispersionless flat bands with zero group velocity and nearly flat bands with negative or positive group velocities. The analytical results presented here are obtained by means of the Green's function method which enables to deduce in closed form: dispersion curves, transmission and reflection coefficients, DOS, as well as the displacement fields. The proposed solid-fluid layered structures should have important applications for designing acoustic mirrors and acoustic filters as well as supersonic and subsonic materials.

Matrix solid-phase dispersion extraction of sulfonamides from blood.

PubMed

Zhang, Yupu; Xu, Xu; Liu, He; Zhai, Yujuan; Sun, Ye; Sun, Shuo; Zhang, Hanqi; Yu, Aimin; Wang, Yinghua

2012-02-01

Matrix solid-phase dispersion extraction was applied to the extraction of sulfadiazine, sulfamerazine, and sulfamethazine from human and animal bloods. The separation and determination of the analytes were carried out by high-performance liquid chromatography. The effects of the types of the dispersion adsorbents and elution solvents were investigated, and the highest recovery was obtained when diatomaceous earth was used as the dispersion adsorbent, while acetone was used as the elution solvent. Under the optimal conditions, the linear range for determining the sulfonamides in blood samples was 0.020-10.0 µg/mL, and the average recoveries of the three sulfonamides were higher than 87.5%.

Solid dispersions of the penta-ethyl ester prodrug of diethylenetriaminepentaacetic acid (DTPA): Formulation design and optimization studies

PubMed Central

Yang, Yu-Tsai; Di Pasqua, Anthony J.; Zhang, Yong; Sueda, Katsuhiko; Jay, Michael

2015-01-01

The penta-ethyl ester prodrug of diethylenetriaminepentaacetic acid (DTPA), which exists as an oily liquid, was incorporated into a solid dispersion for oral administration by the solvent evaporation method using blends of polyvinylpyrrolidone (PVP), Eudragit® RL PO and α-tocopherol. D-optimal mixture design was used to optimize the formulation. Formulations that had a high concentration of both Eudragit® RL PO and α-tocopherol exhibited low water absorption and enhanced stability of the DTPA prodrug. Physicochemical properties of the optimal formulation were evaluated using Fourier transform infrared (FTIR) spectroscopy and differential scanning calorimetry (DSC). In vitro release of the prodrug was evaluated using the USP Type II apparatus dissolution method. DSC studies indicated that the matrix had an amorphous structure, while FTIR spectrometry showed that DTPA penta-ethyl ester and excipients did not react with each other during formation of the solid dispersion.. Dissolution testing showed that the optimized solid dispersion exhibited a prolonged release profile, which could potentially result in a sustained delivery of DTPA penta-ethyl to enhance bioavailability. In conclusion, DTPA penta-ethyl ester was successfully incorporated into a solid matrix with high drug loading and improved stability compared to prodrug alone. PMID:24047113

Molecularly designed lipid microdomains for solid dispersions using a polymer/inorganic carrier matrix produced by hot-melt extrusion.

PubMed

Adler, Camille; Schönenberger, Monica; Teleki, Alexandra; Kuentz, Martin

2016-02-29

Amorphous solid dispersions have for many years been a focus in oral formulations, especially in combination with a hot-melt extrusion process. The present work targets a novel approach with a system based on a fatty acid, a polymer and an inorganic carrier. It was intended to adsorb the acidic lipid by specific molecular interactions onto the solid carrier to design disorder in the alkyl chains of the lipid. Such designed lipid microdomains (DLM) were created as a new microstructure to accommodate a compound in a solid dispersion. Vibrational spectroscopy, X-ray powder diffraction, atomic force microscopy as well as electron microscopic imaging were employed to study a system of stearic acid, hydroxypropylcellulose and aluminum magnesium silicate. β-carotene was used as a poorly water-soluble model substance that is difficult to formulate with conventional solid dispersion formulations. The results indicated that the targeted molecular excipient interactions indeed led to DLMs for specific compositions. The different methods provided complementary aspects and important insights into the created microstructure. The novel delivery system appeared to be especially promising for the formulation of oral compounds that exhibit both high crystal energy and lipophilicity. Copyright © 2015 Elsevier B.V. All rights reserved.

Solid-state, triboelectrostatic and dissolution characteristics of spray-dried piroxicam-glucosamine solid dispersions.

PubMed

Adebisi, Adeola O; Kaialy, Waseem; Hussain, Tariq; Al-Hamidi, Hiba; Nokhodchi, Ali; Conway, Barbara R; Asare-Addo, Kofi

2016-10-01

This work explores the use of both spray drying and d-glucosamine HCl (GLU) as a hydrophilic carrier to improve the dissolution rate of piroxicam (PXM) whilst investigating the electrostatic charges associated with the spray drying process. Spray dried PXM:GLU solid dispersions were prepared and characterised (XRPD, DSC, SEM). Dissolution and triboelectric charging were also conducted. The results showed that the spray dried PXM alone, without GLU produced some PXM form II (DSC results) with no enhancement in solubility relative to that of the parent PXM. XRPD results also showed the spray drying process to decrease the crystallinity of GLU and solid dispersions produced. The presence of GLU improved the dissolution rate of PXM. Spray dried PXM: GLU at a ratio of 2:1 had the most improved dissolution. The spray drying process generally yielded PXM-GLU spherical particles of around 2.5μm which may have contributed to the improved dissolution. PXM showed a higher tendency for charging in comparison to the carrier GLU (-3.8 versus 0.5nC/g for untreated material and -7.5 versus 3.1nC/g for spray dried materials). Spray dried PXM and spray dried GLU demonstrated higher charge densities than untreated PXM and untreated GLU, respectively. Regardless of PXM:GLU ratio, all spray dried PXM:GLU solid dispersions showed a negligible charge density (net-CMR: 0.1-0.3nC/g). Spray drying of PXM:GLU solid dispersions can be used to produce formulation powders with practically no charge and thereby improving handling as well as dissolution behaviour of PXM. Copyright © 2016 Elsevier B.V. All rights reserved.

Relating hydrogen-bonding interactions with the phase behavior of naproxen/PVP K 25 solid dispersions: evaluation of solution-cast and quench-cooled films.

PubMed

Paudel, Amrit; Nies, Erik; Van den Mooter, Guy

2012-11-05

In this work, we investigated the relationship between various intermolecular hydrogen-bonding (H-bonding) interactions and the miscibility of the model hydrophobic drug naproxen with the hydrophilic polymer polyvinylpyrrolidone (PVP) across an entire composition range of solid dispersions prepared by quasi-equilibrium film casting and nonequilibrium melt quench cooling. The binary phase behavior in solid dispersions exhibited substantial processing method dependence. The solid state solubility of crystalline naproxen in PVP to form amorphous solid dispersions was 35% and 70% w/w naproxen in solution-cast films and quench-cooled films, respectively. However, the presence of a single mixed phase glass transition indicated the amorphous miscibility to be 20% w/w naproxen for the films, beyond which amorphous-amorphous and/or crystalline phase separations were apparent. This was further supported by the solution state interactions data such as PVP globular size distribution and solution infrared spectral profiles. The borderline melt composition showed cooling rate dependence of amorphization. The glass transition and melting point depression profiles of the system were treated with the analytical expressions based on Flory-Huggins mixing theory to interpolate the equilibrium solid solubility. FTIR analysis and subsequent spectral deconvolution revealed composition and miscibility dependent variations in the strength of drug-polymer intermolecular H-bonding. Two types of H-bonded populations were evidenced from 25% w/w and 35% w/w naproxen in solution-cast films and quench-cooled films, respectively, with the higher fraction of strongly H-bonded population in the drug rich domains of phase separated amorphous film compositions and highly drug loaded amorphous quench-cooled dispersions.

Trace matrix solid phase dispersion using a molecular sieve as the sorbent for the determination of flavonoids in fruit peels by ultra-performance liquid chromatography.

PubMed

Cao, Wan; Hu, Shuai-Shuai; Ye, Li-Hong; Cao, Jun; Pang, Xiao-Qing; Xu, Jing-Jing

2016-01-01

A simple, rapid, and highly selective trace matrix solid phase dispersion (MSPD) technique, coupled with ultra-performance liquid chromatography-ultraviolet detection, was proposed for extracting flavonoids from orange fruit peel matrices. Molecular sieve SBA-15 was applied for the first time as a solid support in trace MSPD. Parameters, such as the type of dispersant, mass ratio of the sample to the dispersant, grinding time, and elution pH, were optimized in detail. The optimal extraction conditions involved dispersing a powdered fruit peel sample (25 mg) into 25mg of SBA-15 and then eluting the target analytes with 500 μL of methanol. A satisfactory linearity (r(2) > 0.9990) was obtained, and the calculated limits of detection reached 0.02-0.03 μg/mL for the compounds. The results showed that the method developed was successfully applied to determine the content of flavonoids in complex fruit peel matrices. Copyright © 2015 Elsevier Ltd. All rights reserved.

Polymer-functionalized nanoparticles for improving oil displacement

NASA Astrophysics Data System (ADS)

Fossati, Ana B.; Martins Alho, Miriam; Jacobo, Silvia E.

2018-03-01

This work focuses on the synthesis, functionalization, and characterization of magnetic nanoparticles to be used for improving the oil recovery in the oil exploitation industry. In this manuscript we explore three different types of hydrophobic/hydrophilic functionalization through a silanized particle: with styrene, with acrylic acid and with a copolymer of styrene and maleic acid. Further application of such nanoparticles dispersions (nanofluid) are discussed as the wetting and spreading behaviour of liquids on the solid surfaces change if the wettability of solid surface is altered. In order to investigate the influence of wettability alternation on enhancing oil recovery after nanofluid treatment, flushing oil experiment and contact angle measurement were conducted in our laboratory. The results indicated that nanofluid can produce a better flushing efficiency compared with brine solution, and the contact angles of oil phase increased from 13° to 37° after nanofluid treatment (0.005% w/w). We focus on the synthesis of magnetic iron oxide nanoparticles considering recovering possibility.

Accurate description of charged excitations in molecular solids from embedded many-body perturbation theory

NASA Astrophysics Data System (ADS)

Li, Jing; D'Avino, Gabriele; Duchemin, Ivan; Beljonne, David; Blase, Xavier

2018-01-01

We present a novel hybrid quantum/classical approach to the calculation of charged excitations in molecular solids based on the many-body Green's function G W formalism. Molecules described at the G W level are embedded into the crystalline environment modeled with an accurate classical polarizable scheme. This allows the calculation of electron addition and removal energies in the bulk and at crystal surfaces where charged excitations are probed in photoelectron experiments. By considering the paradigmatic case of pentacene and perfluoropentacene crystals, we discuss the different contributions from intermolecular interactions to electronic energy levels, distinguishing between polarization, which is accounted for combining quantum and classical polarizabilities, and crystal field effects, that can impact energy levels by up to ±0.6 eV. After introducing band dispersion, we achieve quantitative agreement (within 0.2 eV) on the ionization potential and electron affinity measured at pentacene and perfluoropentacene crystal surfaces characterized by standing molecules.

The Process of Nanostructuring of Metal (Iron) Matrix in Composite Materials for Directional Control of the Mechanical Properties

PubMed Central

Zemtsova, Elena

2014-01-01

We justified theoretical and experimental bases of synthesis of new class of highly nanostructured composite nanomaterials based on metal matrix with titanium carbide nanowires as dispersed phase. A new combined method for obtaining of metal iron-based composite materials comprising the powder metallurgy processes and the surface design of the dispersed phase is considered. The following stages of material synthesis are investigated: (1) preparation of porous metal matrix; (2) surface structuring of the porous metal matrix by TiC nanowires; (3) pressing and sintering to give solid metal composite nanostructured materials based on iron with TiC nanostructures with size 1–50 nm. This material can be represented as the material type “frame in the frame” that represents iron metal frame reinforcing the frame of different chemical compositions based on TiC. Study of material functional properties showed that the mechanical properties of composite materials based on iron with TiC dispersed phase despite the presence of residual porosity are comparable to the properties of the best grades of steel containing expensive dopants and obtained by molding. This will solve the problem of developing a new generation of nanostructured metal (iron-based) materials with improved mechanical properties for the different areas of technology. PMID:24695459

The process of nanostructuring of metal (iron) matrix in composite materials for directional control of the mechanical properties.

PubMed

Zemtsova, Elena; Yurchuk, Denis; Smirnov, Vladimir

2014-01-01

We justified theoretical and experimental bases of synthesis of new class of highly nanostructured composite nanomaterials based on metal matrix with titanium carbide nanowires as dispersed phase. A new combined method for obtaining of metal iron-based composite materials comprising the powder metallurgy processes and the surface design of the dispersed phase is considered. The following stages of material synthesis are investigated: (1) preparation of porous metal matrix; (2) surface structuring of the porous metal matrix by TiC nanowires; (3) pressing and sintering to give solid metal composite nanostructured materials based on iron with TiC nanostructures with size 1-50 nm. This material can be represented as the material type "frame in the frame" that represents iron metal frame reinforcing the frame of different chemical compositions based on TiC. Study of material functional properties showed that the mechanical properties of composite materials based on iron with TiC dispersed phase despite the presence of residual porosity are comparable to the properties of the best grades of steel containing expensive dopants and obtained by molding. This will solve the problem of developing a new generation of nanostructured metal (iron-based) materials with improved mechanical properties for the different areas of technology.

Surface functionalization of WS2 fullerene-like nanoparticles.

PubMed

Shahar, Chen; Zbaida, David; Rapoport, Lev; Cohen, Hagai; Bendikov, Tatyana; Tannous, Johny; Dassenoy, Fabrice; Tenne, Reshef

2010-03-16

WS(2) belongs to a family of layered metal dichalcogenide compounds that are known to form cylindrical (inorganic nanotubes-INT) and polyhedral nanostructures--onion or nested fullerene-like (IF) particles. The outermost layers of these IF nanoparticles can be peeled under shear stress, thus IF nanoparticles have been studied for their use as solid lubricants. However, the IF nanoparticles tend to agglomerate, presumably because of surface structural defects induced by elastic strain and curvature, a fact that has a deleterious effect on their tribological properties. In the present work, chemical modification of the IF-WS(2) surface with alkyl-silane molecules is reported. The surface-modified IF nanoparticles display improved dispersion in oil-based suspensions. The alkyl-silane coating reduces the IF-WS(2) nanoparticles' tendency to agglomerate and consequently improves the long-term tribological behavior of oil formulated with the IF additive.

Effect of SiO2 grafted MWCNTs on the mechanical and dielectric properties of PEN composite films

NASA Astrophysics Data System (ADS)

Jin, Fei; Feng, Mengna; Huang, Xu; Long, Cheng; Jia, Kun; Liu, Xiaobo

2015-12-01

In this study, the functional poly (arylene ether nitrile) (PEN)/multiwall carbon nanotubes (MWCNTs)/SiO2 nanocomposite with high mechanical and good electrical properties were fabricated through a simple and effective method. Specifically, the surface modification using highly ordered and porous SiO2 not only improves the dispersion of the MWCNTs in polymer matrix, but also combines the excellent properties of SiO2 and MWCNTs. Transmission electron microscopy (TEM), Fourier transform infrared spectra (FTIR), and scanning electron microscope (SEM) were employed to confirm the surface functionalization of MWCNTs. As a result, all the composite films exhibited good dielectric properties with high dielectric constant of 7 as well as low dielectric loss of 0.04. Besides, the results of mechanical tests showed that the tensile strength and modulus reached their highest values at the 2 wt% MWCNTs-SiO2 loading content (125 MPa and 2950 MPa, respectively). The rheological results showed that MWCNTs-SiO2/PEN composites have a typical solid-like viscoelastic response as frequencies changes. Therefore, all the results revealed that surface functionalization has strong influence on the dispersion state of MWCNTs in PEN matrix.

Fracture surfaces of granular pastes.

PubMed

Mohamed Abdelhaye, Y O; Chaouche, M; Van Damme, H

2013-11-01

Granular pastes are dense dispersions of non-colloidal grains in a simple or a complex fluid. Typical examples are the coating, gluing or sealing mortars used in building applications. We study the cohesive rupture of thick mortar layers in a simple pulling test where the paste is initially confined between two flat surfaces. After hardening, the morphology of the fracture surfaces was investigated, using either the box counting method to analyze fracture profiles perpendicular to the mean fracture plane, or the slit-island method to analyze the islands obtained by cutting the fracture surfaces at different heights, parallel to the mean fracture plane. The fracture surfaces were shown to exhibit scaling properties over several decades. However, contrary to what has been observed in the brittle or ductile fracture of solid materials, the islands were shown to be mass fractals. This was related to the extensive plastic flow involved in the fracture process.

Propagation of ultrasonic Love waves in nonhomogeneous elastic functionally graded materials.

PubMed

Kiełczyński, P; Szalewski, M; Balcerzak, A; Wieja, K

2016-02-01

This paper presents a theoretical study of the propagation behavior of ultrasonic Love waves in nonhomogeneous functionally graded elastic materials, which is a vital problem in the mechanics of solids. The elastic properties (shear modulus) of a semi-infinite elastic half-space vary monotonically with the depth (distance from the surface of the material). The Direct Sturm-Liouville Problem that describes the propagation of Love waves in nonhomogeneous elastic functionally graded materials is formulated and solved by using two methods: i.e., (1) Finite Difference Method, and (2) Haskell-Thompson Transfer Matrix Method. The dispersion curves of phase and group velocity of surface Love waves in inhomogeneous elastic graded materials are evaluated. The integral formula for the group velocity of Love waves in nonhomogeneous elastic graded materials has been established. The effect of elastic non-homogeneities on the dispersion curves of Love waves is discussed. Two Love wave waveguide structures are analyzed: (1) a nonhomogeneous elastic surface layer deposited on a homogeneous elastic substrate, and (2) a semi-infinite nonhomogeneous elastic half-space. Obtained in this work, the phase and group velocity dispersion curves of Love waves propagating in the considered nonhomogeneous elastic waveguides have not previously been reported in the scientific literature. The results of this paper may give a deeper insight into the nature of Love waves propagation in elastic nonhomogeneous functionally graded materials, and can provide theoretical guidance for the design and optimization of Love wave based devices. Copyright © 2015 Elsevier B.V. All rights reserved.

Distribution of Captured Planetesimals in Circumplanetary Gas Disks and Implications for Accretion of Regular Satellites

NASA Astrophysics Data System (ADS)

Suetsugu, Ryo; Ohtsuki, Keiji

2017-04-01

Regular satellites of giant planets are formed by accretion of solid bodies in circumplanetary disks. Planetesimals that are moving on heliocentric orbits and are sufficiently large to be decoupled from the flow of the protoplanetary gas disk can be captured by gas drag from the circumplanetary disk. In the present work, we examine the distribution of captured planetesimals in circumplanetary disks using orbital integrations. We find that the number of captured planetesimals reaches an equilibrium state as a balance between continuous capture and orbital decay into the planet. The number of planetesimals captured into retrograde orbits is much smaller than that into prograde orbits, because the former experience a strong headwind and spiral into the planet rapidly. We find that the surface number density of planetesimals at the current radial location of regular satellites can be significantly enhanced by gas drag capture, depending on the velocity dispersions of the planetesimals and the width of the gap in the protoplanetary disk. Using a simple model, we examine the ratio of the surface densities of dust and captured planetesimals in the circumplanetary disk and find that solid material at the current location of regular satellites can be dominated by captured planetesimals when the velocity dispersion of those planetesimals is rather small and a wide gap is not formed in the protoplanetary disk. In this case, captured planetesimals in such a region can grow by mutual collision before spiraling into the planet and would contribute to the growth of regular satellites.

Synthesis of surface Cr (VI)-imprinted magnetic nanoparticles for selective dispersive solid-phase extraction and determination of Cr (VI) in water samples.

PubMed

Qi, Xue; Gao, Shuang; Ding, Guosheng; Tang, An-Na

2017-01-01

A facile, rapid and selective magnetic dispersed solid-phase extraction (dSPE) method for the extraction and enrichment of Cr (VI) prior to flame atomic absorption spectrometry (AAS) was introduced. For highly selective and efficient extraction, magnetic Cr (VI)-imprinted nanoparticles (Fe 3 O 4 @ Cr (VI) IIPs) were prepared by hyphenating surface ion-imprinted with sol-gel techniques. In the preparation process, chromate (Cr(VI)) was used as the template ion; vinylimidazole and 3-aminopropyltriethoxysilane were selected as organic functional monomer and co-monomer respectively. Another reagent, methacryloxypropyltrimethoxysilane was adopted as coupling agent to form the stable covalent bonding between organic and inorganic phases. The effects of various parameters on the extraction efficiency, such as pH of sample solution, the amount of adsorbent, extraction time, the type and concentration of eluent were systematically investigated. Furthermore, the thermodynamic and kinetic properties of the adsorption process were studied to explore the internal adsorption mechanism. Under optimized conditions, the preconcentration factor, limit of detection and linear range of the established dSPE-AAS method for Cr (VI) were found to be 98, 0.29μgL -1 and 4-140μgL -1 , respectively. The developed method was also successfully applied to the analysis of Cr (VI) in different water samples with satisfactory results, proving its reliability and feasibility in real sample analysis. Copyright © 2016 Elsevier B.V. All rights reserved.

Characterization of two polymorphs of salmeterol xinafoate crystallized from supercritical fluids.

PubMed

Tong, H H; Shekunov, B Y; York, P; Chow, A H

2001-06-01

To characterize two polymorphs of salmeterol xinafoate (SX-I and SX-II) produced by supercritical fluid crystallization. SX-I and SX-II were crystallized as fine powders using Solution Enhanced Dispersion by Supercritical Fluids (SEDS). The two polymorphs and a reference micronized SX sample (MSX) were characterized using powder X-ray diffractometry (PXRD), Fourier transform infrared spectroscopy (FTIR), differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), aqueous solubility (and dissolution) determination at 5-40 degrees C, BET adsorption analysis, and inverse gas chromatography (IGC). Compared with SX-I, SX-II exhibited a lower enthalpy of fusion, a higher equilibrium solubility, a higher intrinsic dissolution rate, a lower enthalpy of solution (based on van't Hoff solubility plots), and a different FTIR spectrum (reflecting differences in intermolecular hydrogen bonding). Solubility ratio plot yielded a transition temperature (-99 degrees C) below the melting points of both polymorphs. MSX showed essentially the same crystal form as SX-I (confirmed by PXRD and FTIR), but a distinctly different thermal behaviour. Mild trituration of SX-I afforded a similar DSC profile to MSX while prolonged grinding of SX-I gave rise to an endotherm at -109 degrees C, corresponding to solid-solid transition of SX-I to SX-II. Surface analysis of MSX, SX-I, and SX-II by IGC revealed significant differences in surface free energy in terms of both dispersive (nonpolar) interactions and specific (polar) acid-base properties. The SEDS-processed SX-I and SX-II display high polymorphic purity and distinctly different physical and surface properties. The polymorphs are related enantiotropically with SX-I being the thermodynamically stable form at room temperature.

Polypyrrole-magnetite dispersive micro-solid-phase extraction combined with ultraviolet-visible spectrophotometry for the determination of rhodamine 6G and crystal violet in textile wastewater.

PubMed

Kamaruddin, Amirah Farhan; Sanagi, Mohd Marsin; Wan Ibrahim, Wan Aini; Md Shukri, Dyia S; Abdul Keyon, Aemi S

2017-11-01

Polypyrrole-magnetite dispersive micro-solid-phase extraction method combined with ultraviolet-visible spectrophotometry was developed for the determination of selected cationic dyes in textile wastewater. Polypyrrole-magnetite was used as adsorbent due to its thermal stability, magnetic properties, and ability to adsorb Rhodamine 6G and crystal violet. Dispersive micro-solid-phase extraction parameters were optimized, including sample pH, adsorbent amount, extraction time, and desorption solvent. The optimum polypyrrole-magnetite dispersive micro-solid phase-extraction conditions were sample pH 8, 60 mg polypyrrole-magnetite adsorbent, 5 min of extraction time, and acetonitrile as the desorption solvent. Under the optimized conditions, the polypyrrole-magnetite dispersive micro-solid-phase extraction with ultraviolet-visible method showed good linearity in the range of 0.05-7 mg/L (R 2  > 0.9980). The method also showed a good limit of detection for the dyes (0.05 mg/L) and good analyte recoveries (97.4-111.3%) with relative standard deviations < 10%. The method was successfully applied to the analysis of dyes in textile wastewater samples where the concentration found was 1.03 mg (RSD ±7.9%) and 1.13 mg/L (RSD ± 4.6%) for Rhodamine 6G and crystal violet, respectively. It can be concluded that this method can be adopted for the rapid extraction and determination of dyes at trace concentration levels. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Oral bioavailability and intestinal absorption of candesartan cilexetil: role of naringin as P-glycoprotein inhibitor.

PubMed

Gurunath, Surampalli; Nanjwade, Basavaraj K; Patil, P A

2015-01-01

The aim of the study is to explore the pharmacokinetic behavior of candesartan solid dispersions prepared by different pharmaceutical interventions using P-gp inhibitor in rabbits to validate the effectiveness of naringin as a pharmaceutical excipient in enhancing the oral delivery of lipophilic candesartan cilexetil. Male albino rabbits (1-1.5 kg) were orally administered pure CAN suspensions and various candesartan solid dispersions (10 mg/kg) with and without naringin (15 mg/kg) and blood samples were collected at specified time points. CAN plasma samples were measured using HPLC. After oral dosing of pure CAN suspension, the mean AUC0-8 h was found to be 0.14 ± 0.09 μgh/ml which was increased significantly, i.e. 0.52 ± 0.13 μgh/ml with freeze-dried solid dispersions in the presence of naringin (p < 0.01). Similarly, the mean Cmax of pure CAN suspension increased from 35.81 ± 0.13 μg/ml (without naringin) to 112.23 ± 0.13 μg/ml (freeze-dried solid dispersions with naringin) (p < 0.01). A 3.7-folds increase in apparent bioavailability was noticed with freeze-dried solid dispersions with naringin as compared to free CAN suspension administered alone. These results are quite stimulating for further development of a clinically useful oral formulation of candesartan cilexetil based on P-gp inhibition using naringin, a natural flavonoid as a pharmaceutical excipient.

Dispersion of cellulose nanofibers in biopolymer based nanocomposites

NASA Astrophysics Data System (ADS)

Wang, Bei

The focus of this work was to understand the fundamental dispersion mechanism of cellulose based nanofibers in bionanocomposites. The cellulose nanofibers were extracted from soybean pod and hemp fibers by chemo-mechanical treatments. These are bundles of cellulose nanofibers with a diameter ranging between 50 to 100 nm and lengths of thousands of nanometers which results in very high aspect ratio. In combination with a suitable matrix polymer, cellulose nanofiber networks show considerable potential as an effective reinforcement for high quality specialty applications of bio-based nanocomposites. Cellulose fibrils have a high density of --OH groups on the surface, which have a tendency to form hydrogen bonds with adjacent fibrils, reducing interaction with the surrounding matrix. The use of nanofibers has been mostly restricted to water soluble polymers. This thesis is focused on synthesizing the nanocomposite using a solid phase matrix polypropylene (PP) or polyethylene (PE) by hot compression and poly (vinyl alcohol) (PVA) in an aqueous phase by film casting. The mechanical properties of nanofiber reinforced PVA film demonstrated a 4-5 fold increase in tensile strength, as compared to the untreated fiber-blend-PVA film. It is necessary to reduce the entanglement of the fibrils and improve their dispersion in the matrix by surface modification of fibers without deteriorating their reinforcing capability. Inverse gas chromatography (IGC) was used to explore how various surface treatments would change the dispersion component of surface energy and acid-base character of cellulose nanofibers and the effect of the incorporation of these modified nanofibers into a biopolymer matrix on the properties of their nano-composites. Poly (lactic acid) (PLA) and polyhydroxybutyrate (PHB) based nanocomposites using cellulose nanofibers were prepared by extrusion, injection molding and hot compression. The IGC results indicated that styrene maleic anhydride coated and ethylene-acrylic acid coated fibers improved their potential to interact with both acidic and basic resins. From transmission electron micrograph, it was shown that the nanofibers were partially dispersed in the polymer matrix. The mechanical properties of the nanocomposites were lower than those predicted by theoretical calculations for both nanofiber reinforced biopolymers.

The investigation of solid slag obtained by neutralization of sewage sludge.

PubMed

Kavaliauskas, Zydrunas; Valincius, Vitas; Stravinskas, Giedrius; Milieska, Mindaugas; Striugas, Nerijus

2015-11-01

The purpose of this research is to investigate the feasibility of utilizing the slag collected after gasification of organic fuel combined with sewage sludge. The residue left after gasification process is likely usable as raw material for production of supercondensers. The sewage sludge neutralization system consists of a dosing system (fuel tank), gasifier, plasma reactor, electrostatic filter, and heat exchangers. For the gasification process, dried solid sewage is supplied in proportion of 70% to biomass 30% by weight. The slag is collected in a specially designed chamber beneath the gasifier. A scanning electron microscope (SEM) was used to evaluate surface morphology of the samples. Elemental analysis of the sewage sludge slag was performed using the energy-dispersive spectroscopy (EDS) method, which showed different solid-state elements contained in the porous structure of the solid phase: carbon 29%, aluminum 26%, potassium 20%, chlorine 1%, and others. The specific surface area of the sewage sludge slag is 6.15 m(2)/g as the BET analysis shows. In order to use the slag as a secondary raw material, detailed analysis of the structure and properties is necessary for a decision on whether the slag left after gasification of sewage sludge is suitable for any further usages. Initial results indicate that the slag may be used for production of electrodes for supercapacitors. Every year thousands of tons of sewage sludge are formed in Lithuania. Sewage sludge consists of organic and inorganic compounds. Partial combustion, plasma decomposition, and other methods are used to neutralize the sewage sludge. The incineration of sewage sludge results in generation of solid-phase slag. In this paper the material structure and composition of a solid slag (formed during neutralization of sewage sludge) is considered. Also, the impact the ambient temperature on structure and composition of solid slag is analyzed.

Disk Dispersal: Theoretical Understanding and Observational Constraints

NASA Astrophysics Data System (ADS)

Gorti, U.; Liseau, R.; Sándor, Z.; Clarke, C.

2016-12-01

Protoplanetary disks dissipate rapidly after the central star forms, on time-scales comparable to those inferred for planet formation. In order to allow the formation of planets, disks must survive the dispersive effects of UV and X-ray photoevaporation for at least a few Myr. Viscous accretion depletes significant amounts of the mass in gas and solids, while photoevaporative flows driven by internal and external irradiation remove most of the gas. A reasonably large fraction of the mass in solids and some gas get incorporated into planets. Here, we review our current understanding of disk evolution and dispersal, and discuss how these might affect planet formation. We also discuss existing observational constraints on dispersal mechanisms and future directions.

WOx supported on γ-Al2O3 with different morphologies as model catalysts for alkanol dehydration

DOE Office of Scientific and Technical Information (OSTI.GOV)

Shi, Dachuan; Wang, Huamin; Kovarik, Libor

2018-04-21

The distinctive morphological and surface characteristics of platelet-like γ-Al2O3 were compared to a regular, commercial γ-Al2O3. γ-Al2O3 platelets display dominant (110) surface facets and higher densities of coordinative unsaturated penta-coordinate Al3+ (Al3+penta) sites than regular γ-Al2O3, as measured by solid-state magic-angle spinning nuclear magnetic resonance spectroscopy (MAS NMR). Such Al3+penta sites are also the preferred surface anchoring sites for tungsten oxide (WOx) species consistent with NMR analysis indicating that these sites are consumed upon WOx adsorption. The higher Al3+penta density on γ-Al2O3 platelets leads to greater WOx dispersion (or smaller WOx clusters), as demonstrated by scanning transmission electron microscopy andmore » ultraviolet–visible spectroscopy, and WOx species at intermediate WOx surface concentration are the most active for the probe reaction of 2-butanol dehydration. WOx on γ-Al2O3 platelets approaches the highest turnover rates at higher surface densities than WOx on regular γ-Al2O3, yet with similar highest rate values for both series of catalysts. This indicates that different Al2O3 supports mainly affect the dispersion of supported WOx rather than the intrinsic reactivity of individual WOx clusters with similar size.« less

WO x supported on γ-Al 2 O 3 with different morphologies as model catalysts for alkanol dehydration

DOE Office of Scientific and Technical Information (OSTI.GOV)

Shi, Dachuan; Wang, Huamin; Kovarik, Libor

The distinctive morphological and surface characteristics of platelet-like γ-Al2O3 were compared to a regular, commercial γ-Al2O3. γ-Al2O3 platelets display dominant (110) surface facets and higher densities of coordinative unsaturated penta-coordinate Al3+ (Al3+penta) sites than regular γ-Al2O3, as measured by solid-state magic-angle spinning nuclear magnetic resonance spectroscopy (MAS NMR). Such Al3+penta sites are also the preferred surface anchoring sites for tungsten oxide (WOx) species consistent with NMR analysis indicating that these sites are consumed upon WOx adsorption. The higher Al3+penta density on γ-Al2O3 platelets leads to greater WOx dispersion (or smaller WOx clusters), as demonstrated by scanning transmission electron microscopy andmore » ultraviolet–visible spectroscopy, and WOx species at intermediate WOx surface concentration are the most active for the probe reaction of 2-butanol dehydration. WOx on γ-Al2O3 platelets approaches the highest turnover rates at higher surface densities than WOx on regular γ-Al2O3, yet with similar highest rate values for both series of catalysts. This indicates that different Al2O3 supports mainly affect the dispersion of supported WOx rather than the intrinsic reactivity of individual WOx clusters with similar size.« less

Effect of aminoalkyl methacrylate copolymer E/HCl on in vivo absorption of poorly water-soluble drug.

PubMed

Yoshida, Takatsune; Kurimoto, Ippei; Yoshihara, Keiichi; Umejima, Hiroyuki; Ito, Naoki; Watanabe, Shunsuke; Sako, Kazuhiro; Kikuchi, Akihiko

2013-11-01

This study aimed to investigate in vivo absorption of tacrolimus formulated as a solid dispersion using Eudragit E®/HCl (E-SD). E-SD is an aminoalkyl methacrylate copolymer that can be dissolved under neutral pH conditions. E-SD was used alone as a solid dispersion carrier and/or was mixed with tacrolimus primarily dispersed with hydroxypropylmethylcellulose (HPMC). Tacrolimus was formulated with E-SD at several different ratios. Formulations with tacrolimus/E-SD ratio of 1/3 showed higher in vivo absorption, compared to tacrolimus dispersed in the excipients (primarily HPMC) found in commercially available tacrolimus capsules, using a rat in situ closed loop method. Good correlation was observed between in vitro drug solubility and in vivo drug absorption. In vitro solubility tests and rat oral absorption studies of tacrolimus/HPMC solid dispersion formulations were also conducted after mixing the HPMC dispersion with several ratios of E-SD. E-SD/tacrolimus/HPMC formulations yielded high in vitro drug solubility but comparatively low in vivo absorption. Dog oral absorption studies were conducted using capsules containing a formulation of tacrolimus/E-SD at a ratio of 1/5. The E-SD formulation-containing capsule showed higher in vivo drug absorption than tacrolimus dispersed in the standard HPMC capsule. These studies report enhancement of the in vivo absorption of a poorly water-soluble drug following dispersion with E-SD when compared to formulation in HPMC.

Optical system for determining physical characteristics of a solar cell

DOEpatents

Sopori, Bhushan L.

2001-01-01

The invention provides an improved optical system for determining the physical characteristics of a solar cell. The system comprises a lamp means for projecting light in a wide solid-angle onto the surface of the cell; a chamber for receiving the light through an entrance port, the chamber having an interior light absorbing spherical surface, an exit port for receiving a beam of light reflected substantially normal to the cell, a cell support, and an lower aperture for releasing light into a light absorbing baffle; a means for dispersing the reflection into monochromatic components; a means for detecting an intensity of the components; and a means for reporting the determination.

Sensitive determination of three aconitum alkaloids and their metabolites in human plasma by matrix solid-phase dispersion with vortex-assisted dispersive liquid-liquid microextraction and HPLC with diode array detection.

PubMed

Wang, Xiaozhong; Li, Xuwen; Li, Lanjie; Li, Min; Liu, Ying; Wu, Qian; Li, Peng; Jin, Yongri

2016-05-01

A simple and sensitive method for determination of three aconitum alkaloids and their metabolites in human plasma was developed using matrix solid-phase dispersion combined with vortex-assisted dispersive liquid-liquid microextraction and high-performance liquid chromatography with diode array detection. The plasma sample was directly purified by matrix solid-phase dispersion and the eluate obtained was concentrated and further clarified by vortex-assisted dispersive liquid-liquid microextraction. Some important parameters affecting the extraction efficiency, such as type and amount of dispersing sorbent, type and volume of elution solvent, type and volume of extraction solvent, salt concentration as well as sample solution pH, were investigated in detail. Under optimal conditions, the proposed method has good repeatability and reproducibility with intraday and interday relative standard deviations lower than 5.44 and 5.75%, respectively. The recoveries of the aconitum alkaloids ranged from 73.81 to 101.82%, and the detection limits were achieved within the range of 1.6-2.1 ng/mL. The proposed method offered the advantages of good applicability, sensitivity, simplicity, and feasibility, which makes it suitable for the determination of trace amounts of aconitum alkaloids in human plasma samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Highly dispersed SiO x/Al 2O 3 catalysts illuminate the reactivity of isolated silanol sites

DOE PAGES

Mouat, Aidan R.; George, Cassandra; Kobayashi, Takeshi; ...

2015-09-23

The reaction of γ-alumina with tetraethylorthosilicate (TEOS) vapor at low temperatures selectively yields monomeric SiO x species on the alumina surface. These isolated (-AlO) 3Si(OH) sites are characterized by PXRD, XPS, DRIFTS of adsorbed NH 3, CO, and pyridine, and 29Si and 27Al DNP-enhanced solid-state NMR spectroscopy. The formation of isolated sites suggests that TEOS reacts preferentially at strong Lewis acid sites on the γ-Al 2O 3 surface, functionalizing the surface with “mild” Brønsted acid sites. As a result, for liquid-phase catalytic cyclohexanol dehydration, these SiO x sites exhibit up to 3.5-fold higher specific activity than the parent alumina withmore » identical selectivity.« less

Wavelength dispersion characteristics of integrated silicon avalanche LEDs: potential applications in futuristic on-chip micro- and nano-biosensors

NASA Astrophysics Data System (ADS)

Okhai, Timothy A.; Snyman, Lukas W.; Polleux, Jean-Luc

2016-02-01

Si Av LEDs are easily integrated in on-chip integrated circuitry. They have high modulation frequencies into the GHz range and can be fabricated to sub-micron dimensions. Due to subsurface light generation in the silicon device itself, and the high refractive index differences between silicon and the device environment, the exiting light radiation has interesting dispersion characteristics. Three junction micro p+-np+ Silicon Avalanche based Light Emitting Devices (Si Av LEDs) have been analyzed in terms of dispersion characteristics, generally resulting in different wavelengths of light (colors) being emitted at different angles and solid angles from the surfaces of these devices. The emission wavelength is in the 450 - 850 nm range. The devices are of micron dimension and operate at 8 - 10V, 1μA - 2mA. The emission spot sizes are about 1 micron square. Emission intensities are up to 500 nW.μm-2. The observed dispersion characteristics range from 0.05 degrees per nm per degree at emission angle of 5 degrees, to 0.15 degrees per nm at emission angles of 30 degrees. It is believed that the dispersion characteristics can find interesting and futuristic on-chip electro-optic applications involving particularly a ranging from on chip micro optical wavelength dispersers, communication de-multiplexers, and novel bio-sensor applications. All of these could penetrate into the nanoscale dimensions.

Turmeric powder and starch: selected physical, physicochemical, and microstructural properties.

PubMed

Kuttigounder, Dhanalakshmi; Lingamallu, Jaganmohan Rao; Bhattacharya, Suvendu

2011-01-01

Turmeric powder and its starch were characterized for physical, physicochemical, and microstructural characteristics. X-ray diffractogram indicated that turmeric starch to be of B type. Dried and cured-dried turmeric powder samples showed higher water-holding capacity (3.62 and 4.78 g/g, respectively) compared to isolated starch (1.07 g/g) at 30 °C. Non-Newtonian shear-thinning characteristics were observed with turmeric powder dispersion containing 10% (w/w) solids. A power law model fitted well to correlate the shear-rate and shear-stress data (r= 0.993 to 0.999, P≤ 0.01) for both samples. Apparent viscosities of isolated turmeric starch and cured-dried turmeric powder dispersion containing 10% (w/w) solids were 1.29 ± 0.03 and 7.57 ± 0.39 mPa s, respectively. Microstructure of starch particles showed a smooth flat outer surface. The approximate length and breadth of isolated elliptical starches were 25 and 10 μm while the thickness was about 5 μm. Isolation and characterization of starch from an unconventional source like turmeric rhizome indicate a potential application as a functional ingredient in foods and pharmaceutical industries including agglomerated products. © 2011 Institute of Food Technologists®

Effervescence-assisted dispersive solid-phase extraction using ionic-liquid-modified magnetic β-cyclodextrin/attapulgite coupled with high-performance liquid chromatography for fungicide detection in honey and juice.

PubMed

Wu, Xiaoling; Yang, Miyi; Zeng, Haozhe; Xi, Xuefei; Zhang, Sanbing; Lu, Runhua; Gao, Haixiang; Zhou, Wenfeng

2016-11-01

In this study, a simple effervescence-assisted dispersive solid-phase extraction method was developed to detect fungicides in honey and juice. Most significantly, an innovative ionic-liquid-modified magnetic β-cyclodextrin/attapulgite sorbent was used because its large specific surface area enhanced the extraction capacity and also led to facile separation. A one-factor-at-a-time approach and orthogonal design were employed to optimize the experimental parameters. Under the optimized conditions, the entire extraction procedure was completed within 3 min. In addition, the calibration curves exhibited good linearity, and high enrichment factors were achieved for pure water and honey samples. For the honey samples, the extraction efficiencies for the target fungicides ranged from 77.0 to 94.3% with relative standard deviations of 2.3-5.44%. The detection and quantitation limits were in the ranges of 0.07-0.38 and 0.23-1.27 μg/L, respectively. Finally, the developed technique was successfully applied to real samples, and satisfactory results were achieved. This analytical technique is cost-effective, environmentally friendly, and time-saving. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Simultaneous Determination of Oleanolic Acid and Ursolic Acid by in Vivo Microdialysis via UHPLC-MS/MS Using Magnetic Dispersive Solid Phase Extraction Coupling with Microwave-Assisted Derivatization and Its Application to a Pharmacokinetic Study of Arctiumlappa L. Root Extract in Rats.

PubMed

Zheng, Zhenjia; Zhao, Xian-En; Zhu, Shuyun; Dang, Jun; Qiao, Xuguang; Qiu, Zhichang; Tao, Yanduo

2018-04-18

Simultaneous detection of oleanolic acid and ursolic acid in rat blood by in vivo microdialysis can provide important pharmacokinetics information. Microwave-assisted derivatization coupled with magnetic dispersive solid phase extraction was established for the determination of oleanolic acid and ursolic acid by liquid chromatography tandem mass spectrometry. 2'-Carbonyl-piperazine rhodamine B was first designed and synthesized as the derivatization reagent, which was easily adsorbed onto the surface of Fe 3 O 4 /graphene oxide. Simultaneous derivatization and extraction of oleanolic acid and ursolic acid were performed on Fe 3 O 4 /graphene oxide. The permanent positive charge of the derivatization reagent significantly improved the ionization efficiencies. The limits of detection were 0.025 and 0.020 ng/mL for oleanolic acid and ursolic acid, respectively. The validated method was shown to be promising for sensitive, accurate, and simultaneous determination of oleanolic acid and ursolic acid. It was used for their pharmacokinetics study in rat blood after oral administration of Arctiumlappa L. root extract.

One pot synthesis of magnetic graphene/carbon nanotube composites as magnetic dispersive solid-phase extraction adsorbent for rapid determination of oxytetracycline in sewage water.

PubMed

Sun, Yunyun; Tian, Jing; Wang, Lu; Yan, Hongyuan; Qiao, Fengxia; Qiao, Xiaoqiang

2015-11-27

A simple and time-saving one pot synthesis of magnetic graphene/carbon nanotube composites (M-G/CNTs) was developed that could avoid the tedious drying process of graphite oxide, and G/CNTs were modified by Fe3O4 nanoparticles in the reduction procedure. It contributed to a shorten duration of the synthesis process of M-G/CNTs. The obtained M-G/CNTs were characterized and the results indicated that CNTs and Fe3O4 nanoparticles were served as spacer distributing to the layers of graphene, which was beneficial for enlarging surface area and improving extraction efficiency. Moreover, M-G/CNTs showed good magnetic property and outstanding thermal stability. Then M-G/CNTs were applied as adsorbent of magnetic dispersive solid-phase extraction for rapid extraction and determination of oxytetracycline in sewage water. Under the optimum conditions, good linearity was obtained in the range of 20-800ngmL(-1) and the recoveries were ranged from 95.5% to 112.5% with relative standard deviations less than 5.8%. Copyright © 2015 Elsevier B.V. All rights reserved.

High performance preconcentration of inorganic Se species by dispersive micro-solid phase extraction with a nanosilica-ionic liquid hybrid material

NASA Astrophysics Data System (ADS)

Llaver, Mauricio; Coronado, Eduardo A.; Wuilloud, Rodolfo G.

2017-12-01

A highly sensitive and efficient dispersive micro-solid phase extraction (D-μ-SPE) method was developed for inorganic Se speciation analysis. A novel ionic liquid (IL)-nanomaterial hybrid consisting of 1-dodecyl-3-methylimidazolium bromide-functionalized nanosilica was used for the efficient retention of Se(IV) complexed with ammonium pyrrolidine dithiocarbamate, followed by elution with an ethyl acetate/Triton X-114 mixture and determination by electrothermal atomic absorption spectroscopy. The Se(VI) species was selectively determined by difference between total inorganic Se and Se(IV) after pre-reduction. The IL-nanomaterial hybrid was characterized by Fourier transform infrared spectroscopy and transmission electronic microscopy. Likewise, Se(IV) sorption capacity of the retention material and maximum amount of IL loaded on its surface were determined. Several factors concerning the functionalization, extraction and elution steps were optimized, yielding a 100% extraction efficiency for Se(IV) under optimal conditions. A limit of detection of 1.1 ng L- 1, a relative standard deviation of 5.7% and a 110-fold enhancement factor were obtained. The D-μ-SPE method was successfully applied to several water samples from different origins and compositions, including rain, tap, underground, river and sea.

Tribological Properties of Nanodiamonds in Aqueous Suspensions: Effect of the Surface Charge

NASA Astrophysics Data System (ADS)

Krim, J.; Liu, Zijian; Leininger, D. A.; Kooviland, A.; Smirnov, A. I.; Shendarova, O.; Brenner, D. W.

The presence of granular nanoparticulates, be they wear particles created naturally by frictional rubbing at a geological fault line or products introduced as lubricant additives, can dramatically alter friction at solid-liquid interfaces. Given the complexity of such systems, understanding system properties at a fundamental level is particularly challenging. The Quartz Crystal Microbalance (QCM) is an ideal tool for studies of material-liquid-nanoparticulate interfaces. We have employed it here to study the uptake and nanotribological properties of positively and negatively charged 5-15 nm diameter nanodiamonds dispersed in water[1] in the both the presence and absence of a macroscopic contact with the QCM electrode. The nanodiamonds were found to impact tribological performance at both nanometer and macroscopic scales. The tribological effects were highly sensitive to the sign of the charge: negatively (positively) charged particles were more weakly (strongly) bound and reduced (increased) frictional drag at the solid-liquid interface. For the macroscopic contacts, negatively charged nanodiamonds appeared to be displaced from the contact, while the positively charged ones were not. Overall, the negatively charged nanodiamonds were more stable in an aqueous dispersion for extended time periods. Work supported by NSF and DOE.

A facile synthesis of Zn(x)Cd(1-x)S/CNTs nanocomposite photocatalyst for H2 production.

PubMed

Wang, Lei; Yao, Zhongping; Jia, Fangzhou; Chen, Bin; Jiang, Zhaohua

2013-07-21

The sulfide solid solution has become a promising and important visible-light-responsive photocatalyst for hydrogen production nowadays. Zn(x)Cd(1-x)S/CNT nanocomposites were synthesized to improve the dispersion, adjust the energy band gap, and enhance the separation of the photogenerated electrons and holes. The as-prepared photocatalysts were characterized by scanning electron-microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and UV-visible diffuse reflectance spectra (UV-visible), respectively. And the effects of CNTs on structure, composition and optical absorption property of the sulfide solid solutions were investigated along with their inherent relationships. For Zn0.83Cd0.17S/CNTs, sulfide solid solution is assembled along the CNTs orderly, with a diameter of 100 nm or so. XPS analysis shows that there is bonding effect between the solid solutions and the CNTs due to the strong adsorption of Zn(2+) and Cd(2+) on the surface of CNTs. There are two obvious absorption edges for Zn0.83Cd0.17S/CNTs, corresponding to two kinds of sulfide solid solutions with different molar ratios of Zn/Cd. The hybridization of solid solutions with CNTs makes the absorption spectrum red shift. The photocatalytic property was evaluated by splitting Na2S + Na2SO3 solution into H2, and the highest rate of H2 evolution of 6.03 mmol h(-1) g(-1) was achieved over Zn0.83Cd0.17S/CNTs. The high activity of photocatalytic H2 production is attributed to the following factors: (1) the optimum band gap and a moderate position of the conduction band (which needs to match the irradiation spectrum of the Xe lamp best), (2) the efficient separation of photogenerated electrons and holes by hybridization, and (3) the improvement of the dispersion of nanocomposites by assembling along the CNTs as well.

Investigating the Dissolution Performance of Amorphous Solid Dispersions Using Magnetic Resonance Imaging and Proton NMR.

PubMed

Tres, Francesco; Coombes, Steven R; Phillips, Andrew R; Hughes, Leslie P; Wren, Stephen A C; Aylott, Jonathan W; Burley, Jonathan C

2015-09-10

We have investigated the dissolution performance of amorphous solid dispersions of poorly water-soluble bicalutamide in a Kollidon VA64 polymeric matrix as a function of the drug loading (5% vs. 30% bicalutamide). A combined suite of state-of-the-art analytical techniques were employed to obtain a clear picture of the drug release, including an integrated magnetic resonance imaging UV-Vis flow cell system and 1H-NMR. Off-line 1H-NMR was used for the first time to simultaneously measure the dissolution profiles and rates of both the drug and the polymer from a solid dispersion. MRI and 1H-NMR data showed that the 5% drug loading compact erodes linearly, and that bicalutamide and Kollidon VA64 are released at approximately the same rate from the molecular dispersion. For the 30% extrudate, data indicated a slower water ingress into the compact which corresponds to a slower dissolution rate of both bicalutamide and Kollidon VA64.

Drop Printing of Pharmaceuticals: Effect of Molecular Weight on PEG Coated-Naproxen/PEG3350 Solid Dispersions

PubMed Central

Hsu, Hsin-Yun; Toth, Scott; Simpson, Garth J.; Harris, Michael T.

2016-01-01

Solid dispersions have been used to enhance the bioavailability of poorly water-soluble active pharmaceutical ingredients (APIs). However, the solid state phase, compositional uniformity, and scale-up problems are issues that need to be addressed. To allow for highly controllable products, the Drop Printing (DP) technique can provide precise dosages and predictable compositional uniformity of APIs in two/three dimensional structures. In this study, DP was used to prepare naproxen (NAP)/polyethylene glycol 3350 (PEG3350) solid dispersions with PEG coatings of different molecular weights (MW). A comparison of moisture-accelerated crystallization inhibition by different PEG coatings was assessed. Scanning electron microscopy (SEM), second harmonic generation (SHG) microscopy, and differential scanning calorimetry (DSC) analysis were performed to characterize the morphology and quantify the apparent crystallinity of NAP within the solid dispersions. Thermogravimetric analysis (TGA) was employed to measure the water content within each sample. The results suggest that the moisture-accelerated crystallization inhibition capability of the PEG coatings increased with increasing MW of the PEG coating. Besides, to demonstrate the flexibility of DP technology on manufacturing formulation, multilayer tablets with different PEG serving as barrier layers were also constructed, and their dissolution behavior was examined. By applying DP and appropriate materials, it is possible to design various carrier devices used to control the release dynamics of the API. PMID:27041744

Drop Printing of Pharmaceuticals: Effect of Molecular Weight on PEG Coated-Naproxen/PEG3350 Solid Dispersions.

PubMed

Hsu, Hsin-Yun; Toth, Scott; Simpson, Garth J; Harris, Michael T

2015-12-01

Solid dispersions have been used to enhance the bioavailability of poorly water-soluble active pharmaceutical ingredients (APIs). However, the solid state phase, compositional uniformity, and scale-up problems are issues that need to be addressed. To allow for highly controllable products, the Drop Printing (DP) technique can provide precise dosages and predictable compositional uniformity of APIs in two/three dimensional structures. In this study, DP was used to prepare naproxen (NAP)/polyethylene glycol 3350 (PEG3350) solid dispersions with PEG coatings of different molecular weights (MW). A comparison of moisture-accelerated crystallization inhibition by different PEG coatings was assessed. Scanning electron microscopy (SEM), second harmonic generation (SHG) microscopy, and differential scanning calorimetry (DSC) analysis were performed to characterize the morphology and quantify the apparent crystallinity of NAP within the solid dispersions. Thermogravimetric analysis (TGA) was employed to measure the water content within each sample. The results suggest that the moisture-accelerated crystallization inhibition capability of the PEG coatings increased with increasing MW of the PEG coating. Besides, to demonstrate the flexibility of DP technology on manufacturing formulation, multilayer tablets with different PEG serving as barrier layers were also constructed, and their dissolution behavior was examined. By applying DP and appropriate materials, it is possible to design various carrier devices used to control the release dynamics of the API.

Dispersion analysis of passive surface-wave noise generated during hydraulic-fracturing operations

USGS Publications Warehouse

Forghani-Arani, Farnoush; Willis, Mark; Snieder, Roel; Haines, Seth S.; Behura, Jyoti; Batzle, Mike; Davidson, Michael

2014-01-01

Surface-wave dispersion analysis is useful for estimating near-surface shear-wave velocity models, designing receiver arrays, and suppressing surface waves. Here, we analyze whether passive seismic noise generated during hydraulic-fracturing operations can be used to extract surface-wave dispersion characteristics. Applying seismic interferometry to noise measurements, we extract surface waves by cross-correlating several minutes of passive records; this approach is distinct from previous studies that used hours or days of passive records for cross-correlation. For comparison, we also perform dispersion analysis for an active-source array that has some receivers in common with the passive array. The active and passive data show good agreement in the dispersive character of the fundamental-mode surface-waves. For the higher mode surface waves, however, active and passive data resolve the dispersive properties at different frequency ranges. To demonstrate an application of dispersion analysis, we invert the observed surface-wave dispersion characteristics to determine the near-surface, one-dimensional shear-wave velocity.

Design, characterization, and aerosol dispersion performance modeling of advanced spray-dried microparticulate/nanoparticulate mannitol powders for targeted pulmonary delivery as dry powder inhalers.

PubMed

Li, Xiaojian; Vogt, Frederick G; Hayes, Don; Mansour, Heidi M

2014-04-01

The purpose was to design and characterize inhalable microparticulate/nanoparticulate dry powders of mannitol with essential particle properties for targeted dry powder delivery for cystic fibrosis mucolytic treatment by dilute organic solution spray drying, and, in addition, to tailor and correlate aerosol dispersion performance delivered as dry powder inhalers based on spray-drying conditions and solid-state physicochemical properties. Organic solution advanced spray drying from dilute solution followed by comprehensive solid-state physicochemical characterization and in vitro dry powder aerosolization were used. The particle size distribution of the spray-dried (SD) powders was narrow, unimodal, and in the range of ∼500 nm to 2.0 μm. The particles possessed spherical particle morphology, relatively smooth surface morphology, low water content and vapor sorption (crystallization occurred at exposure above 65% relative humidity), and retention of crystallinity by polymorphic interconversion. The emitted dose, fine particle fraction (FPF), and respirable fraction (RF) were all relatively high. The mass median aerodynamic diameters were below 4 μm for all SD mannitol aerosols. The in vitro aerosol deposition stage patterns could be tailored based on spray-drying pump rate. Positive linear correlation was observed between both FPF and RF values with spray-drying pump rates. The interplay between various spray-drying conditions, particle physicochemical properties, and aerosol dispersion performance was observed and examined, which enabled tailoring and modeling of high aerosol deposition patterns.

Core-shell indium (III) sulfide@metal-organic framework nanocomposite as an adsorbent for the dispersive solid-phase extraction of nitro-polycyclic aromatic hydrocarbons.

PubMed

Jia, Yuqian; Zhao, Yanfang; Zhao, Mei; Wang, Zhenhua; Chen, Xiangfeng; Wang, Minglin

2018-05-25

A core-shell discoid shaped indium (III) sulfide@metal-organic framework (MIL-125(Ti)) nanocomposite was synthesized by a solvothermal method and explored as an adsorbent material for dispersive solid-phase extraction (d-SPE). The as-synthesized sorbent was characterized by scanning electron microscopy, energy-dispersive spectroscopy, transmission electron microscopy, powder X-ray diffraction, N 2 adsorption-desorption analysis, and Fourier transform infrared spectroscopy. The extraction performance was evaluated by the d-SPE of 16 nitro-polycyclic aromatic hydrocarbons (NPAHs) from water samples. The analysis was carried out by gas chromatography (GC) coupled with triple quadruple mass spectrometer in negative chemical ionization (NCI) mode. The selected ion monitoring (SIM) was used in the quantification of the target NPAHs. Extraction factors affecting the d-SPE, including the ionic strength, extraction temperature, and extraction time were optimized by the response surface methodology. The developed d-SPE method showed good linear correlations from 10 to 1000 ng L -1 (r > 0.99), low detection limits (2.9-83.0 ng L -1 ), satisfactory repeatability (relative standard deviation of <10%, n = 6), and acceptable recoveries (71.3%-112.2%) for water samples. The developed method was used for the food and environmental sample analysis. The results demonstrated that the method could be used for sample preparation of trace NPAHs in real samples. Copyright © 2018. Published by Elsevier B.V.

Design, Characterization, and Aerosol Dispersion Performance Modeling of Advanced Spray-Dried Microparticulate/Nanoparticulate Mannitol Powders for Targeted Pulmonary Delivery as Dry Powder Inhalers

PubMed Central

Li, Xiaojian; Vogt, Frederick G.; Hayes, Don

2014-01-01

Abstract Background: The purpose was to design and characterize inhalable microparticulate/nanoparticulate dry powders of mannitol with essential particle properties for targeted dry powder delivery for cystic fibrosis mucolytic treatment by dilute organic solution spray drying, and, in addition, to tailor and correlate aerosol dispersion performance delivered as dry powder inhalers based on spray-drying conditions and solid-state physicochemical properties. Methods: Organic solution advanced spray drying from dilute solution followed by comprehensive solid-state physicochemical characterization and in vitro dry powder aerosolization were used. Results: The particle size distribution of the spray-dried (SD) powders was narrow, unimodal, and in the range of ∼500 nm to 2.0 μm. The particles possessed spherical particle morphology, relatively smooth surface morphology, low water content and vapor sorption (crystallization occurred at exposure above 65% relative humidity), and retention of crystallinity by polymorphic interconversion. The emitted dose, fine particle fraction (FPF), and respirable fraction (RF) were all relatively high. The mass median aerodynamic diameters were below 4 μm for all SD mannitol aerosols. Conclusion: The in vitro aerosol deposition stage patterns could be tailored based on spray-drying pump rate. Positive linear correlation was observed between both FPF and RF values with spray-drying pump rates. The interplay between various spray-drying conditions, particle physicochemical properties, and aerosol dispersion performance was observed and examined, which enabled tailoring and modeling of high aerosol deposition patterns. PMID:24502451

Controlling the metal to semiconductor transition of MoS 2 and WS 2 in solution

DOE PAGES

Chou, Stanley Shihyao; Yi-Kai Huang; Kim, Jaemyung; ...

2015-01-22

Lithiation-exfoliation produces single to few-layered MoS 2 and WS 2 sheets dispersible in water. However, the process transforms them from the pristine semiconducting 2H phase to a distorted metallic phase. Recovery of the semiconducting properties typically involves heating of the chemically exfoliated sheets at elevated temperatures. Therefore, it has been largely limited to sheets deposited on solid substrates. We report the dispersion of chemically exfoliated MoS 2 sheets in high boiling point organic solvents enabled by surface functionalization and the controllable recovery of their semiconducting properties directly in solution. Ultimately, this process connects the scalability of chemical exfoliation with themore » simplicity of solution processing, enabling a facile method for tuning the metal to semiconductor transitions of MoS 2 and WS 2 within a liquid medium.« less

Kinetics of microbial reduction of Solid phase U(VI).

PubMed

Liu, Chongxuan; Jeon, Byong-Hun; Zachara, John M; Wang, Zheming; Dohnalkova, Alice; Fredrickson, James K

2006-10-15

Sodium boltwoodite (NaUO2SiO3OH x 1.5 H2O) was used to assess the kinetics of microbial reduction of solid-phase U(VI) by a dissimilatory metal-reducing bacterium (DMRB), Shewanella oneidensis strain MR-1. The bioreduction kinetics was studied with Na-boltwoodite in suspension or within alginate beads in a nongrowth medium with lactate as electron donor at pH 6.8 buffered with PIPES. Concentrations of U(VI)tot and cell number were varied to evaluate the coupling of U(VI) dissolution, diffusion, and microbial activity. Microscopic and spectroscopic analyses with transmission electron microscopy (TEM), energy dispersive spectroscopy (EDS), and laser-induced fluorescence spectroscopy (LIFS) collectively indicated that solid-phase U(VI) was first dissolved and diffused out of grain interiors before it was reduced on bacterial surfaces and/or within the periplasm. The kinetics of solid-phase U(VI) bioreduction was well described by a coupled model of bicarbonate-promoted dissolution of Na-boltwoodite, intragrain uranyl diffusion, and Monod type bioreduction kinetics with respect to dissolved U(VI) concentration. The results demonstrated that microbial reduction of solid-phase U(VI) is controlled by coupled biological, chemical, and physical processes.

Streamlined sample cleanup using combined dispersive solid-phase extraction and in-vial filtration for analysis of pesticides and environmental pollutants in shrimp

USDA-ARS?s Scientific Manuscript database

A new method of sample preparation was developed and is reported for the first time. The approach combines in-vial filtration with dispersive solid-phase extraction (d-SPE) in a fast and convenient cleanup of QuEChERS (quick, easy, cheap, effective, rugged, and safe) extracts. The method was appli...

Natural organic UV-absorbent coatings based on cellulose and lignin: designed effects on spectroscopic properties.

PubMed

Hambardzumyan, Arayik; Foulon, Laurence; Chabbert, Brigitte; Aguié-Béghin, Véronique

2012-12-10

Novel nanocomposite coatings composed of cellulose nanocrystals (CNCs) and lignin (either synthetic or fractionated from spruce and corn stalks) were prepared without chemical modification or functionalization (via covalent attachment) of one of the two biopolymers. The spectroscopic properties of these coatings were investigated by UV-visible spectrophotometry and spectroscopic ellipsometry. When using the appropriate weight ratio of CNC/lignin (R), these nanocomposite systems exhibited high-performance optical properties, high transmittance in the visible spectrum, and high blocking in the UV spectrum. Atomic force microscopy analysis demonstrated that these coatings were smooth and homogeneous, with visible dispersed lignin nodules in a cellulosic matrix. It was also demonstrated that the introduction of nanoparticles into the medium increases the weight ratio and the CNC-specific surface area, which allows better dispersion of the lignin molecules throughout the solid film. Consequently, the larger molecular expansion of these aromatic polymers on the surface of the cellulosic nanoparticles dislocates the π-π aromatic aggregates, which increases the extinction coefficient and decreases the transmittance in the UV region. These nanocomposite coatings were optically transparent at visible wavelengths.

The sand bag model of the dispersion of the cosmic body in the atmosphere

NASA Technical Reports Server (NTRS)

Teterev, A. V.; Nemchinov, I. V.

1993-01-01

The strength of the extraterrestrial bodies depends on their structure, composition, dimensions, and the history of this body. The fragmentation of the body due to aerodynamic stresses begins at sufficiently large heights above the surface of the Earth. The process of fragmentation and dispersion of the fragments usually is studied by the hydrodynamic or even gasdynamic models. If the fragmentation process begins due to the initial cracks and faults of the body, or this body consists of large boulders glued by ice, the strength of these boulders after fragmentation remains higher than the aerodynamic stresses exerted at the remaining part of the body. It is supposed that fragmentation occurs at initial moment t = 0 at some height z(sub o) above the surface of the air, these fragments remain solid. The possibility of further fragmentation during the remaining part of the trajectory is not taken into account. If the number of these parts is large enough and their size is small in comparison to the initial radius of the body than we can use the sand bag model proposed in qualitative form.

Melt dispersion granules: formulation and evaluation to improve oral delivery of poorly soluble drugs - a case study with valsartan.

PubMed

Chella, Naveen; Tadikonda, Ramarao

2015-06-01

Solid dispersion (SD) technique is a promising strategy to improve the solubility and dissolution of BCS class II drugs. However, only few products are marketed till today based on SD technology due to poor flow properties and stability. The present work was intended to solve these problems by using combination approach, melt dispersion and surface adsorption technologies. The main aim of the present work is to improve the absorption in the stomach (at lower pH) where the absorption window exists for the drug by improving the dissolution, resulting in the enhancement of oral bioavailability of poorly soluble, weakly acidic drug with pH dependant solubility, i.e. valsartan. Melt dispersion granules were prepared in different ratios using different carriers (Gelucire 50/13, PEG 8000 and Pluronic F-68) and lactose as an adsorbent. Similarly, physical mixtures were also prepared at corresponding ratios. The prepared dispersion granules and physical mixtures were characterized by FTIR, DSC and in vitro dissolution studies. DSC studies revealed reduction in the crystallinity with a possibility of presence of amorphous character of drug in the dispersion granules. From dissolution studies, valsartan Gelucire dispersion (GSD4; 1:4 ratio) showed complete drug release in 30 min against the plain drug which showed only 11.31% of drug release in 30 min. Pharmacokinetic studies of optimized formulation in male Wistar rats showed 2.65-fold higher bioavailability and 1.47-fold higher Cmax compared to pure drug. The melt dispersion technology has the potential to improve dissolution and the bioavailability of BCS class II drugs.

Solubility and dissolution performances of spray-dried solid dispersion of Efavirenz in Soluplus.

PubMed

Lavra, Zênia Maria Maciel; Pereira de Santana, Davi; Ré, Maria Inês

2017-01-01

Efavirenz (EFV), a first-line anti-HIV drug largely used as part of antiretroviral therapies, is practically insoluble in water and belongs to BCS class II (low solubility/high permeability). The aim of this study was to improve the solubility and dissolution performances of EFV by formulating an amorphous solid dispersion of the drug in polyvinyl caprolactam-polyvinyl acetate-polyethylene glycol graft copolymer (Soluplus ® ) using spray-drying technique. To this purpose, spray-dried dispersions of EFV in Soluplus ® at different mass ratios (1:1.25, 1:7, 1:10) were prepared and characterized using particle size measurements, SEM, XRD, DSC, FTIR and Raman microscopy mapping. Solubility and dissolution were determined in different media. Stability was studied at accelerated conditions (40 °C/75% RH) and ambient conditions for 12 months. DSC and XRD analyses confirmed the EFV amorphous state. FTIR spectroscopy analyses revealed possible drug-polymer molecular interaction. Solubility and dissolution rate of EFV was enhanced remarkably in the developed spray-dried solid dispersions, as a function of the polymer concentration. Spray-drying was concluded to be a proper technique to formulate a physically stable dispersion of amorphous EFV in Soluplus ® , when protected from moisture.

Characterization of solid dispersions of itraconazole and hydroxypropylmethylcellulose prepared by melt extrusion, Part II.

PubMed

Six, Karel; Berghmans, Hugo; Leuner, Christian; Dressman, Jennifer; Van Werde, Kristof; Mullens, Jules; Benoist, Luc; Thimon, Mireille; Meublat, Laurent; Verreck, Geert; Peeters, Jef; Brewster, Marcus; Van den Mooter, Guy

2003-07-01

This study was done to elucidate the physical and pharmaceutical properties of itraconazole-HPMC dispersions and the influence of water on the phase separation. Extrudates were prepared using a corotating twin-screw hot-stage extruder with fixed process parameters. Modulated-temperature differential scanning calorimetry (MTDSC) and DSC 111 were used to examine the mixing behavior of itraconazole and the carrier by evaluation of the glass transition region. High temperature diffuse reflectance infrared transform spectroscopy (HT-DRIFT) was performed to reveal interactions between itraconazole and HPMC. Dissolution was performed to investigate the pharmaceutical performance of the dispersions. Although the dissolution rate of itraconazole significantly increased, we found that the solid dispersions do not form a homogeneous system. A different picture was obtained depending on the way MTDSC analysis was performed, i.e., using open or closed sample pans. Water can evaporate in open pans, which allows itraconazole to interact with HPMC and leads to a partially mixed phase. Analysis in hermetically closed pans revealed a further phase separation as water remains on the sample and impedes the interaction between drug and polymer. Solid dispersions of itraconazole and HPMC do not form a homogeneous phase.

Chemoselective Hydrogenation with Supported Organoplatinum(IV) Catalyst on Zn(II)-Modified Silica

DOE Office of Scientific and Technical Information (OSTI.GOV)

Camacho-Bunquin, Jeffrey; Ferrandon, Magali; Sohn, Hyuntae

For this research, well-defined organoplatinum(IV) sites were grafted on a Zn(II)-modified SiO 2 support via surface organometallic chemistry in toluene at room temperature. Solid-state spectroscopies including XAS, DRIFTS, DRUV–vis, and solid-state (SS) NMR enhanced by dynamic nuclear polarization (DNP), as well as TPR-H 2 and TEM techniques revealed highly dispersed (methylcyclopentadienyl)methylplatinum(IV) sites on the surface ((MeCp)PtMe/Zn/SiO 2, 1). In addition, computational modeling suggests that the surface reaction of (MeCp)PtMe 3 with Zn(II)-modified SiO 2 support is thermodynamically favorable (ΔG = -12.4 kcal/mol), likely due to the increased acidity of the hydroxyl group, as indicated by NH 3-TPD and DNP-enhanced 17O{more » 1H} SSNMR. In situ DRIFTS and XAS hydrogenation experiments reveal the probable formation of a surface Pt(IV)-H upon hydrogenolysis of Pt-Me groups. The heterogenized organoplatinum(IV)-hydride sites catalyze the selective partial hydrogenation of 1,3-butadiene to butenes (up to 95%) and the reduction of nitrobenzene derivatives to anilines (up to 99%) with excellent tolerance of reduction-sensitive functional groups (olefin, carbonyl, nitrile, halogens) under mild reaction conditions.« less

Chemoselective Hydrogenation with Supported Organoplatinum(IV) Catalyst on Zn(II)-Modified Silica

DOE Office of Scientific and Technical Information (OSTI.GOV)

Camacho-Bunquin, Jeffrey; Ferrandon, Magali; Sohn, Hyuntae

Well-defined organoplatinum(IV) sites were grafted on a Zn(II)-modified SiO2 support via surface organometallic chemistry in toluene at room temperature. Solid-state spectroscopies including XAS, DRIFTS, DRUV-Vis, and solid-state (SS)NMR enhanced by dynamic nuclear polarization (DNP), as well as TPR-H2 and TEM techniques revealed highly dispersed (methylcyclopentadi-enyl)methylplatinum(IV) sites on the surface ((MeCp)PtMe/Zn/SiO2, 1). In addition, computational modelling suggests that the surface reaction of (MeCp)PtMe3 with Zn(II)-modified SiO2 support is thermodynamically favorable (ΔG = -12.4 kcal/mol), likely due to the increased acidity of the hydroxyl group, as confirmed by NH3-TPD and DNP-enhanced 17O{1H} SSNMR. In situ DRIFTS and XAS hydrogenation experiments reveal themore » formation of a surface Pt(IV)-H upon hydrogenolysis of Pt-Me groups. The heterogenized organoplatinum(IV)-H sites catalyze the selective partial hydrogenation of 1,3-butadiene to butenes (up to 95%) and the reduction of nitrobenzene derivatives to anilines (up to 100%) with excellent tolerance of reduction-sensitive func-tional groups (olefin, carbonyl, nitrile, halogens) under mild reaction conditions.« less

Interfacial friction and adhesion of cross-linked polymer thin films swollen with linear chains.

PubMed

Zhang, Qing; Archer, Lynden A

2007-07-03

The preparation and interfacial properties of a new type of tethered, thin-film lubricant coating are presented. These coatings are composed of three components: a dense self-assembled monolayer (SAM) underlayer that presents reactive vinyl groups at its surface; a cross-linked polydimethylsiloxane (PDMS) overlayer that is covalently tethered to the SAM; and free, mobile linear PDMS chains dispersed in the network. We investigate the influence of the molecular weight (Ms) and concentration of the free PDMS chains on the structure and equilibrium swelling properties of the cross-linked films. Using a bead-probe lateral force microscopy measurement technique, we also quantify the interfacial friction and adhesion characteristics of surfaces functionalized with these coatings. We find that both the volume fraction and the molecular weight of free PDMS molecules in the coatings influence their interfacial friction and adhesion properties. For example, the addition of short PDMS chains in dry, cross-linked PDMS thin films yields tethered surface coatings with ultralow friction coefficients (mu = 5.2 x 10(-3)). An analysis based on classical lubrication theory suggests that the reduction in friction force produced by free polymer is a consequence of the gradual separation of asperities on opposing surfaces and the consequent substitution of solid-solid friction by viscous drag of the free polymer chains in the network.

Chemoselective Hydrogenation with Supported Organoplatinum(IV) Catalyst on Zn(II)-Modified Silica

DOE PAGES

Camacho-Bunquin, Jeffrey; Ferrandon, Magali; Sohn, Hyuntae; ...

2018-02-27

For this research, well-defined organoplatinum(IV) sites were grafted on a Zn(II)-modified SiO 2 support via surface organometallic chemistry in toluene at room temperature. Solid-state spectroscopies including XAS, DRIFTS, DRUV–vis, and solid-state (SS) NMR enhanced by dynamic nuclear polarization (DNP), as well as TPR-H 2 and TEM techniques revealed highly dispersed (methylcyclopentadienyl)methylplatinum(IV) sites on the surface ((MeCp)PtMe/Zn/SiO 2, 1). In addition, computational modeling suggests that the surface reaction of (MeCp)PtMe 3 with Zn(II)-modified SiO 2 support is thermodynamically favorable (ΔG = -12.4 kcal/mol), likely due to the increased acidity of the hydroxyl group, as indicated by NH 3-TPD and DNP-enhanced 17O{more » 1H} SSNMR. In situ DRIFTS and XAS hydrogenation experiments reveal the probable formation of a surface Pt(IV)-H upon hydrogenolysis of Pt-Me groups. The heterogenized organoplatinum(IV)-hydride sites catalyze the selective partial hydrogenation of 1,3-butadiene to butenes (up to 95%) and the reduction of nitrobenzene derivatives to anilines (up to 99%) with excellent tolerance of reduction-sensitive functional groups (olefin, carbonyl, nitrile, halogens) under mild reaction conditions.« less

The adsorption of argon on ZnO at 77K

NASA Astrophysics Data System (ADS)

Marinelli, Francis; Grillet, Yves; Pellenq, Roland J.-M.

We have studied the adsorption of argon onto ZnO surfaces at 77K by means of quasiequilibrium adsorption volumetry coupled with high resolution microcalorimetry and Grand Canonical Monte-Carlo (GCMC) simulations. The adsorbate/surface adsorption potential function (PN type) used in the simulations, was determined on the basis of ab initio calculations (corrected for dispersion interactions). The first aspect of this work was to test the ability of a standard solid-state Hartree-Fock technique coupled with a perturbative semiempirical approach in deriving a reliable adsorption potential function. The dispersion part of the adsorbate/surface interatomic potential was derived by using perturbation theory-based equations while the repulsive and induction interactions were derived from periodic HartreeFock (CRYSTAL92) calculations. GCMC simulations based on this adsorption potential allow one to calculate adsorption isotherms and isosteric heat versus loading curves as well as singlet distribution functions at 77K for each type of ZnO (neutral and polar) faces. The combined analysis of the simulation data for all surfaces gives a good insight of the adsorption mechanism of argon onto ZnO surfaces at 77K in agreement with experiment. As far as neutral surfaces are concerned, it is shown that adsorption first takes place within the 'troughs' which cover ZnO neutral surfaces. At low chemical potentials, these semi-channels are preferential adsorption sites in which we could detect a nearly one-dimensional adsorbate freezing in a commensurate phase at 77K. The polar O faces are the most favourable surfaces for adsorption at higher chemical potentials.

PREFACE: Vibrations at surfaces Vibrations at surfaces

NASA Astrophysics Data System (ADS)

Rahman, Talat S.

2011-12-01

This special issue is dedicated to the phenomenon of vibrations at surfaces—a topic that was indispensible a couple of decades ago, since it was one of the few phenomena capable of revealing the nature of binding at solid surfaces. For clean surfaces, the frequencies of modes with characteristic displacement patterns revealed how surface geometry, as well as the nature of binding between atoms in the surface layers, could be different from that in the bulk solid. Dispersion of the surface phonons provided further measures of interatomic interactions. For chemisorbed molecules on surfaces, frequencies and dispersion of the vibrational modes were also critical for determining adsorption sites. In other words, vibrations at surfaces served as a reliable means of extracting information about surface structure, chemisorption and overlayer formation. Experimental techniques, such as electron energy loss spectroscopy and helium-atom-surface scattering, coupled with infra-red spectroscopy, were continually refined and their resolutions enhanced to capture subtleties in the dynamics of atoms and molecules at surfaces. Theoretical methods, whether based on empirical and semi-empirical interatomic potential or on ab initio electronic structure calculations, helped decipher experimental observations and provide deeper insights into the nature of the bond between atoms and molecules in regions of reduced symmetry, as encountered on solid surfaces. Vibrations at surfaces were thus an integral part of the set of phenomena that characterized surface science. Dedicated workshops and conferences were held to explore the variety of interesting and puzzling features revealed in experimental and theoretical investigations of surface vibrational modes and their dispersion. One such conference, Vibrations at Surfaces, first organized by Harald Ibach in Juelich in 1980, continues to this day. The 13th International Conference on Vibrations at Surfaces was held at the University of Central Florida, Orlando, in March 2010. Several speakers at this meeting were invited to contribute to the special section in this issue. As is clear from the articles in this special section, the phenomenon of vibrations at surfaces continues to be a dynamic field of investigation. In fact, there is a resurgence of effort because the insights provided by surface dynamics are still fundamental to the development of an understanding of the microscopic factors that control surface structure formation, diffusion, reaction and structural stability. Examination of dynamics at surfaces thus complements and supplements the wealth of information that is obtained from real-space techniques such as scanning tunneling microscopy. Vibrational dynamics is, of course, not limited to surfaces. Surfaces are important since they provide immediate deviation from the bulk. They display how lack of symmetry can lead to new structures, new local atomic environments and new types of dynamical modes. Nanoparticles, large molecules and nanostructures of all types, in all kinds of local environments, provide further examples of regions of reduced symmetry and coordination, and hence display characteristic vibrational modes. Given the tremendous advance in the synthesis of a variety of nanostructures whose functionalization would pave the way for nanotechnology, there is even greater need to engage in experimental and theoretical techniques that help extract their vibrational dynamics. Such knowledge would enable a more complete understanding and characterization of these nanoscale systems than would otherwise be the case. The papers presented here provide excellent examples of the kind of information that is revealed by vibrations at surfaces. Vibrations at surface contents Poisoning and non-poisoning oxygen on Cu(410)L Vattuone, V Venugopal, T Kravchuk, M Smerieri, L Savio and M Rocca Modifying protein adsorption by layers of glutathione pre-adsorbed on Au(111)Anne Vallée, Vincent Humblot, Christophe Méthivier, Paul Dumas and Claire-Marie Pradier Relating temperature dependence of atom scattering spectra to surface corrugationW W Hayes and J R Manson Effects of the commensurability and disorder on friction for the system Xe/CuA Franchini, V Bortolani, G Santoro and K Xheka Switching ability of nitro-spiropyran on Au(111): electronic structure changes as a sensitive probe during a ring-opening reactionChristopher Bronner, Gunnar Schulze, Katharina J Franke, José Ignacio Pascual and Petra Tegeder High-resolution phonon study of the Ag(100) surfaceK L Kostov, S Polzin and W Widdra On the interpretation of IETS spectra of a small organic molecule Karina Morgenstern

Time-Dependent Changes in Morphology and Composition of Solid Particles Collected From Heavy Water Electrolyte after Electrolysis with a Palladium Cathode

NASA Astrophysics Data System (ADS)

Dash, John; Wang, Q.

2009-03-01

Recently, we have observed particles floating on the surfaces of electrolytes after electrolysis, in four cells, each of which contained a heavy water electrolyte and a Pd cathode. Solid particles were unexpected from electrolysis, so it seemed important to characterize these particles. Cu grids were used to collect particles from the electrolyte surface. Then, a scanning electron microscope ( SEM ) and an energy dispersive spectrometer ( EDS ) were used to study the surfaces of these particles and to record time-dependent changes which were occurring. The morphology and composition of the particles were determined . After storage at ambient for 11 days, there were large changes in the morphology and composition of the particles. For example, one portion of the particles contained a large number of microspheres. A typical microsphere contained mostly carbon and palladium, whereas the matrix near the microsphere contained mostly palladium with less carbon and a significant amount of silver. One day later the same microsphere had increased carbon and reduced palladium, but there was no significant change in the composition of the matrix. Results for other particles from other cells will also be presented.

ELECTROMAGNETIC STIRRING IN ZONE REFINING

DOE Office of Scientific and Technical Information (OSTI.GOV)

Braun, I.; Frank, F.C.; Marshall, S.

1958-02-01

The efficiency of the zone refining process can obviously be increased by stirring the molten zone to disperse the impurity-rich layer at the solid- liquid surface. Induction heating is sometimes preferred to radiant heat because it produces more convection, but no marked improvement has been reported. Pfann and Dorsi(1967) have described a method of stirring the melt by passing an electric current through the ingot and compressing a magnetic field across the molten zone. Preliminary results obtained by using a rotating magnetic field us the stirring agent during the purification of aluminum are described. (A.C.)

Determination of perfluorinated compounds in mollusks by matrix solid-phase dispersion and liquid chromatography-tandem mass spectrometry.

PubMed

Villaverde-de-Sáa, Eugenia; Quintana, José Benito; Rodil, Rosario; Ferrero-Refojos, Raúl; Rubí, Elisa; Cela, Rafael

2012-01-01

Perfluorinated compounds (PFCs) have been used for over 40 years in different commercial and industrial applications mainly as surfactants and surface protectors and have become an important class of marine emerging pollutants. This study presents the development and validation of a new analytical method to determine the simultaneous presence of eight PFCs in different kinds of mollusks using matrix solid-phase dispersion (MSPD) followed by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Simplicity of the analytical procedure, low volume of solvent and quantity of sample required, low global price, and integration of extraction and clean-up into a single step, are the most important advantages of the developed methodology. Solvent, solid support (dispersing agent), clean-up sorbent, and their amounts were optimized by means of an experimental design. In the final method, 0.5 g of sample are dispersed with 0.2 g of diatomaceous earth and transferred into a polypropylene syringe containing 4 g of silica as clean-up sorbent. Then, analytes are eluted with 20 mL of acetonitrile. The extract is finally concentrated to a final volume of 0.5 mL in methanol, avoiding extract dryness in order to prevent evaporation losses and injected in the LC-MS/MS. The combination of this MSPD protocol with LC-MS/MS afforded detection limits from 0.05 to 0.3 ng g(-1). Also, a good linearity was established for the eight PFCs in the range from limit of quantification (LOQ) to 500 ng mL(-1) with R(2) > 0.9917. The recovery of the method was studied with three types of spiked mollusk and was in the 64-126% range. Moreover, a mussel sample was spiked and aged for more than 1 month and analyzed by the developed method and a reference method, ion-pair extraction, for comparison, producing both methods statistically equal concentration values. The method was finally applied to the determination of PFCs in different kinds of mollusks revealing concentrations up to 8.3 ng g(-1) for perfluoroundecanoic acid.

Magnetic Memory from Site Isolated Dy(III) on Silica Materials

PubMed Central

2017-01-01

Achieving magnetic remanence at single isolated metal sites dispersed at the surface of a solid matrix has been envisioned as a key step toward information storage and processing in the smallest unit of matter. Here, we show that isolated Dy(III) sites distributed at the surface of silica nanoparticles, prepared with a simple and scalable two-step process, show magnetic remanence and display a hysteresis loop open at liquid 4He temperature, in contrast to the molecular precursor which does not display any magnetic memory. This singular behavior is achieved through the controlled grafting of a tailored Dy(III) siloxide complex on partially dehydroxylated silica nanoparticles followed by thermal annealing. This approach allows control of the density and the structure of isolated, “bare” Dy(III) sites bound to the silica surface. During the process, all organic fragments are removed, leaving the surface as the sole ligand, promoting magnetic remanence. PMID:28386602

Magnetic memory from site isolated Dy(III) on silica materials

DOE Office of Scientific and Technical Information (OSTI.GOV)

Allouche, Florian; Lapadula, Giuseppe; Siddiqi, Georges

Achieving magnetic remanence at single isolated metal sites dispersed at the surface of a solid matrix has been envisioned as a key step toward information storage and processing in the smallest unit of matter. Here, we show that isolated Dy(III) sites distributed at the surface of silica nanoparticles, prepared with a simple and scalable two-step process, show magnetic remanence and display a hysteresis loop open at liquid 4He temperature, in contrast to the molecular precursor which does not display any magnetic memory. This singular behavior is achieved through the controlled grafting of a tailored Dy(III) siloxide complex on partially dehydroxylatedmore » silica nanoparticles followed by thermal annealing. This approach allows control of the density and the structure of isolated, “bare” Dy(III) sites bound to the silica surface. Throughout the process, all organic fragments are removed, leaving the surface as the sole ligand, promoting magnetic remanence.« less

Magnetic memory from site isolated Dy(III) on silica materials

DOE PAGES

Allouche, Florian; Lapadula, Giuseppe; Siddiqi, Georges; ...

2017-02-22

Achieving magnetic remanence at single isolated metal sites dispersed at the surface of a solid matrix has been envisioned as a key step toward information storage and processing in the smallest unit of matter. Here, we show that isolated Dy(III) sites distributed at the surface of silica nanoparticles, prepared with a simple and scalable two-step process, show magnetic remanence and display a hysteresis loop open at liquid 4He temperature, in contrast to the molecular precursor which does not display any magnetic memory. This singular behavior is achieved through the controlled grafting of a tailored Dy(III) siloxide complex on partially dehydroxylatedmore » silica nanoparticles followed by thermal annealing. This approach allows control of the density and the structure of isolated, “bare” Dy(III) sites bound to the silica surface. Throughout the process, all organic fragments are removed, leaving the surface as the sole ligand, promoting magnetic remanence.« less

Multiscale Computational Modeling of the Nanostructure of Solid Dispersions of Hydroxypropyl Methylcellulose Acetate Succinate (HPMCAS) and Phenytoin.

PubMed

Huang, Wenjun; Mandal, Taraknath; Larson, Ronald G

2017-10-02

We recently developed coarse-grained (CG) force fields for hydroxypropyl methylcellulose acetate succinate (HPMCAS) polymers and the model drug molecule phenytoin, and a continuum transport model to study the polymer-drug nanostructures presented during a dissolution test after solvation of solid dispersion particles. We model the polymer-drug interactions that contribute to suppression of drug aggregation, release, and crystal growth during the dissolution process, and we take these as indicators of polymer effectiveness. We find that the size and the intermolecular interaction strength of the functional group and the drug loading concentration are the major factors that impact the effectiveness of the polymeric excipient. The hydroxypropyl acetyl group is the most effective functional group, followed by the acetyl group, while the deprotonated succinyl group is the least effective functional group, except that the deprotonated succinyl group at the 6-position is very effective in slowing down the phenytoin crystal growth. Our simulation results thus suggest HPMCAS with higher acetyl and lower succinyl content is more effective in promoting phenytoin solubility in dissolution media, and polymers become less effective when drug loading becomes high (i.e., 50% of the mass of the polymer/drug solid dispersion), agreeing with previous experimental studies. In addition, our transport model indicates that the drug release time from a solid dispersion particle of 2 μm diameter is less than 10 min, correlating well with the experimental time scale for a typical dissolution profile to reach maximum peak concentration. Our modeling effort, therefore, provides new avenues to understand the dissolution behavior of complex HPMCAS-phenytoin solid dispersions and offers a new design tool to optimize the formulation. Moreover, the systematic and robust approach used in our computational models can be extended to other polymeric excipients and drug candidates.

Solubilization of the poorly water soluble drug, telmisartan, using supercritical anti-solvent (SAS) process.

PubMed

Park, Junsung; Cho, Wonkyung; Cha, Kwang-Ho; Ahn, Junhyun; Han, Kang; Hwang, Sung-Joo

2013-01-30

Telmisartan is a biopharmaceutical classification system (BCS) class II drug that has extremely low water solubility but is freely soluble in highly alkalized solutions. Few organic solvents can dissolve telmisartan. This solubility problem is the main obstacle achieving the desired bioavailability. Because of its unique characteristics, the supercritical anti-solvent (SAS) process was used to BCS class II drug in a variety of ways including micronization, amorphization and solid dispersion. Solid dispersions were prepared using hydroxypropylmethylcellulose/polyvinylpyrrolidone (HPMC/PVP) at 1:0.5, 1:1, and 1:2 weight ratios of drug to polymer, and pure telmisartan was also treated using the SAS process. Processed samples were characterized for morphology, particle size, crystallinity, solubility, dissolution rate and polymorphic stability. After the SAS process, all samples were converted to the amorphous form and were confirmed to be hundreds nm in size. Solubility and dissolution rate were increased compared to the raw material. Solubility tended to increase with increases in the amount of polymer used. However, unlike the solubility results, the dissolution rate decreased with increases in polymer concentration due to gel layer formation of the polymer. Processed pure telmisartan showed the best drug release even though it had lower solubility compared to other solid dispersions; however, because there were no stabilizers in processed pure telmisartan, it recrystallized after 1 month under severe conditions, while the other solid dispersion samples remained amorphous form. We conclude that after controlling the formulation of solid dispersion, the SAS process could be a promising approach for improving the solubility and dissolution rate of telmisartan. Copyright © 2012 Elsevier B.V. All rights reserved.

Thermal Processing of PVP- and HPMC-Based Amorphous Solid Dispersions.

PubMed

LaFountaine, Justin S; Prasad, Leena Kumari; Brough, Chris; Miller, Dave A; McGinity, James W; Williams, Robert O

2016-02-01

Thermal processing technologies continue to gain interest in pharmaceutical manufacturing. However, the types and grades of polymers that can be utilized in common thermal processing technologies, such as hot-melt extrusion (HME), are often limited by thermal or rheological factors. The objectives of the present study were to compare and contrast two thermal processing methods, HME and KinetiSol® Dispersing (KSD), and investigate the influence of polymer type, polymer molecular weight, and drug loading on the ability to produce amorphous solid dispersions (ASDs) containing the model compound griseofulvin (GRIS). Dispersions were analyzed by a variety of imaging, solid-state, thermal, and solution-state techniques. Dispersions were prepared by both HME and KSD using polyvinylpyrrolidone (PVP) K17 or hydroxypropyl methylcellulose (HPMC) E5. Dispersions were only prepared by KSD using higher molecular weight grades of HPMC and PVP, as these could not be extruded under the conditions selected. Powder X-ray diffraction (PXRD) analysis showed that dispersions prepared by HME were amorphous at 10% and 20% drug load; however, it showed significant crystallinity at 40% drug load. PXRD analysis of KSD samples showed all formulations and drug loads to be amorphous with the exception of trace crystallinity seen in PVP K17 and PVP K30 samples at 40% drug load. These results were further supported by other analytical techniques. KSD produced amorphous dispersions at higher drug loads than could be prepared by HME, as well as with higher molecular weight polymers that were not processable by HME, due to its higher rate of shear and torque output.

Increased dissolution rates of tranilast solid dispersions extruded with inorganic excipients.

PubMed

Maniruzzaman, Mohammed; Ross, Steven A; Islam, Muhammad Tariqul; Scoutaris, Nikolaos; Nair, Arun; Douroumis, Dennis

2017-06-01

The purpose of this study was to evaluate the performance of Neusilin® (NEU) a synthetic magnesium aluminometasilicate as an inorganic drug carrier co-processed with the hydrophilic surfactants Labrasol and Labrafil to develop Tranilast (TLT)-based solid dispersions using continuous melt extrusion (HME) processing. Twin-screw extrusion was optimized to develop various TLT/excipient/surfactant formulations followed by continuous capsule filling in the absence of any downstream equipment. Physicochemical characterization showed the existence of TLT in partially crystalline state in the porous network of inorganic NEU for all extruded formulations. Furthermore, in-line NIR studies revealed a possible intermolecular H-bonding formation between the drug and the carrier resulting in the increase of TLT dissolution rates. The capsules containing TLT-extruded solid dispersions showed enhanced dissolution rates and compared with the marketed Rizaben ® product.

Dispersive solid-phase extraction followed by vortex-assisted dispersive liquid-liquid microextraction based on the solidification of a floating organic droplet for the determination of benzoylurea insecticides in soil and sewage sludge.

PubMed

Peng, Guilong; He, Qiang; Mmereki, Daniel; Lu, Ying; Zhong, Zhihui; Liu, Hanyang; Pan, Weiliang; Zhou, Guangming; Chen, Junhua

2016-04-01

A novel dispersive solid-phase extraction combined with vortex-assisted dispersive liquid-liquid microextraction based on solidification of floating organic droplet was developed for the determination of eight benzoylurea insecticides in soil and sewage sludge samples before high-performance liquid chromatography with ultraviolet detection. The analytes were first extracted from the soil and sludge samples into acetone under optimized pretreatment conditions. Clean-up of the extract was conducted by dispersive solid-phase extraction using activated carbon as the sorbent. The vortex-assisted dispersive liquid-liquid microextraction based on solidification of floating organic droplet procedure was performed by using 1-undecanol with lower density than water as the extraction solvent, and the acetone contained in the solution also acted as dispersive solvent. Under the optimum conditions, the linearity of the method was in the range 2-500 ng/g with correlation coefficients (r) of 0.9993-0.9999. The limits of detection were in the range of 0.08-0.56 ng/g. The relative standard deviations varied from 2.16 to 6.26% (n = 5). The enrichment factors ranged from 104 to 118. The extraction recoveries ranged from 81.05 to 97.82% for all of the analytes. The good performance has demonstrated that the proposed methodology has a strong potential for application in the multiresidue analysis of complex matrices. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Crystallization Kinetics of Indomethacin/Polyethylene Glycol Dispersions Containing High Drug Loadings.

PubMed

Duong, Tu Van; Van Humbeeck, Jan; Van den Mooter, Guy

2015-07-06

The reproducibility and consistency of physicochemical properties and pharmaceutical performance are major concerns during preparation of solid dispersions. The crystallization kinetics of drug/polyethylene glycol solid dispersions, an important factor that is governed by the properties of both drug and polymer has not been adequately explored, especially in systems containing high drug loadings. In this paper, by using standard and modulated differential scanning calorimetry and X-ray powder diffraction, we describe the influence of drug loading on crystallization behavior of dispersions made up of indomethacin and polyethylene glycol 6000. Higher drug loading increases the amorphicity of the polymer and inhibits the crystallization of PEG. At 52% drug loading, polyethylene glycol was completely transformed to the amorphous state. To the best of our knowledge, this is the first detailed investigation of the solubilization effect of a low molecular weight drug on a semicrystalline polymer in their dispersions. In mixtures containing up to 55% indomethacin, the dispersions exhibited distinct glass transition events resulting from amorphous-amorphous phase separation which generates polymer-rich and drug-rich domains upon the solidification of supercooled polyethylene glycol, whereas samples containing at least 60% drug showed a single amorphous phase during the period in which crystallization normally occurs. The current study demonstrates a wide range in physicochemical properties of drug/polyethylene glycol solid dispersions as a result of the complex nature in crystallization of this system, which should be taken into account during preparation and storage.

Evaluating the ready biodegradability of two poorly water-soluble substances: comparative approach of bioavailability improvement methods (BIMs).

PubMed

Sweetlove, Cyril; Chenèble, Jean-Charles; Barthel, Yves; Boualam, Marc; L'Haridon, Jacques; Thouand, Gérald

2016-09-01

Difficulties encountered in estimating the biodegradation of poorly water-soluble substances are often linked to their limited bioavailability to microorganisms. Many original bioavailability improvement methods (BIMs) have been described, but no global approach was proposed for a standardized comparison of these. The latter would be a valuable tool as part of a wider strategy for evaluating poorly water-soluble substances. The purpose of this study was to define an evaluation strategy following the assessment of different BIMs adapted to poorly water-soluble substances with ready biodegradability tests. The study was performed with two poorly water-soluble chemicals-a solid, anthraquinone, and a liquid, isodecyl neopentanoate-and five BIMs were compared to the direct addition method (reference method), i.e., (i) ultrasonic dispersion, (ii) adsorption onto silica gel, (iii) dispersion using an emulsifier, (iv) dispersion with silicone oil, and (v) dispersion with emulsifier and silicone oil. A two-phase evaluation strategy of solid and liquid chemicals was developed involving the selection of the most relevant BIMs for enhancing the biodegradability of tested substances. A description is given of a BIM classification ratio (R BIM), which enables a comparison to be made between the different test chemical sample preparation methods used in the various tests. Thereby, using this comparison, the BIMs giving rise to the greatest biodegradability were ultrasonic dispersion and dispersion with silicone oil or with silicone oil and emulsifier for the tested solid chemical, adsorption onto silica gel, and ultrasonic dispersion for the liquid one.

Dispersion relations of elastic waves in one-dimensional piezoelectric/piezomagnetic phononic crystal with initial stresses.

PubMed

Guo, Xiao; Wei, Peijun

2016-03-01

The dispersion relations of elastic waves in a one-dimensional phononic crystal formed by periodically repeating of a pre-stressed piezoelectric slab and a pre-stressed piezomagnetic slab are studied in this paper. The influences of initial stress on the dispersive relation are considered based on the incremental stress theory. First, the incremental stress theory of elastic solid is extended to the magneto-electro-elasto solid. The governing equations, constitutive equations, and boundary conditions of the incremental stresses in a magneto-electro-elasto solid are derived with consideration of the existence of initial stresses. Then, the transfer matrices of a pre-stressed piezoelectric slab and a pre-stressed piezomagnetic slab are formulated, respectively. The total transfer matrix of a single cell in the phononic crystal is obtained by the multiplication of two transfer matrixes related with two adjacent slabs. Furthermore, the Bloch theorem is used to obtain the dispersive equations of in-plane and anti-plane Bloch waves. The dispersive equations are solved numerically and the numerical results are shown graphically. The oblique propagation and the normal propagation situations are both considered. In the case of normal propagation of elastic waves, the analytical expressions of the dispersion equation are derived and compared with other literatures. The influences of initial stresses, including the normal initial stresses and shear initial stresses, on the dispersive relations are both discussed based on the numerical results. Copyright © 2015 Elsevier B.V. All rights reserved.

Effect of solid state fermentation of peanut shell on its dye adsorption performance.

PubMed

Liu, Jiayang; Wang, Zhixin; Li, Hongyan; Hu, Changwei; Raymer, Paul; Huang, Qingguo

2018-02-01

The effect of solid state fermentation of peanut shell to produce beneficial laccase and on its dye adsorption performance was evaluated. The resulting residues from solid fermentation were tested as sorbents (designated as SFs) in comparison to the raw peanut shell (RPS) for their ability to remove crystal violet from water. The fermentation process reduced the adsorption capacity (q m ) of SF by about 50%, and changed the sorptive behavior when compared to the RPS. The Langmuir model was more suitable for fitting adsorption by SFs. q m was positively correlated with the surface area of peanut shell, but negatively correlated with acid detergent lignin content. For all the sorbents tested, the process was spontaneous and endothermic, and the adsorption followed both the pseudo 1st and 2nd order kinetic model and the film diffusion model. Dye adsorption efficiency was greater when SFs dispersed solution than when placed in filter packets. Copyright © 2017 Elsevier Ltd. All rights reserved.

Synthesis of methyl esters from waste cooking oil using construction waste material as solid base catalyst.

PubMed

Balakrishnan, K; Olutoye, M A; Hameed, B H

2013-01-01

The current research investigates synthesis of methyl esters by transesterification of waste cooking oil in a heterogeneous system, using barium meliorated construction site waste marble as solid base catalyst. The pretreated catalyst was calcined at 830 °C for 4h prior to its activity test to obtained solid oxide characterized by scanning electron microscopy/energy dispersive spectroscopy, BET surface area and pore size measurement. It was found that the as prepared catalyst has large pores which contributed to its high activity in transesterification reaction. The methyl ester yield of 88% was obtained when the methanol/oil molar ratio was 9:1, reaction temperature at 65 °C, reaction time 3h and catalyst/oil mass ratio of 3.0 wt.%. The catalyst can be reused over three cycles, offer low operating conditions, reduce energy consumption and waste generation in the production of biodiesel. Copyright © 2012 Elsevier Ltd. All rights reserved.

Enhancement of carvedilol solubility by solid dispersion technique using cyclodextrins, water soluble polymers and hydroxyl acid.

PubMed

Yuvaraja, K; Khanam, Jasmina

2014-08-05

Aim of the present work is to enhance aqueous solubility of carvedilol (CV) by solid dispersion technique using wide variety of carriers such as: β-cyclodextrin (βCD), hydroxypropyl-β-cyclodextrin (HPβCD), tartaric acid (TA), polyvinyl pyrrolidone K-30 (PVP K-30) and poloxamer-407 (PLX-407). Various products of 'CV-solid dispersion' had been studied extensively in various pH conditions to check enhancement of solubility and dissolution characteristics of carvedilol. Any physical change upon interaction between CV and carriers was confirmed by instrumental analysis: XRD, DSC, FTIR and SEM. Negative change of Gibb's free energy and complexation constants (Kc, 75-240M(-1), for cyclodextrins and 1111-20,365M(-1), for PVP K-30 and PLX-407) were the evidence of stable nature of the binding between CV and carriers. 'Solubility enhancement factor' of ionized-CV was found high enough (340 times) with HPβCD in presence of TA. TA increases the binding efficiency of cyclodextrin and changing the pH of microenvironment in dissolution medium. In addition, ionization process was used to increase the apparent intrinsic solubility of drug. In vitro, dissolution time of CV was remarkably reduced in the solid dispersion system compared to that of pure drug. This may be attributed to increased wettability, dispersing ability and transformation of crystalline state of drug to amorphous one. Copyright © 2014 Elsevier B.V. All rights reserved.

New environmentally friendly MSPD solid support based on golden mussel shell: characterization and application for extraction of organic contaminants from mussel tissue.

PubMed

Rombaldi, Caroline; de Oliveira Arias, Jean Lucas; Hertzog, Gabriel Ianzer; Caldas, Sergiane Souza; Vieira, João P; Primel, Ednei Gilberto

2015-06-01

The use of golden mussel shells as a solid support in vortex-assisted matrix solid-phase dispersion (MSPD) was evaluated for the first time for extraction of residues of 11 pesticides and nine pharmaceutical and personal care products from mussel tissue samples. After they had been washed, dried, and milled, the mussel shells were characterized by scanning electron microscopy, energy-dispersive X-ray spectroscopy, infrared spectroscopy, and Brunauer-Emmett-Teller analysis. The MSPD procedure with analysis by liquid chromatography-tandem mass spectrometry allowed the determination of target analytes at trace concentrations (nanograms per gram), with mean recoveries ranging from 61 to 107 % and relative standard deviations lower than 18 %. The optimized method consisted of dispersion of 0.5 g of mussel tissue, 0.5 g of NaSO4, and 0.5 g of golden mussel shell for 5 min, and subsequent extraction with 5 mL of ethyl acetate. The matrix effect was evaluated, and a low effect was found for all compounds. The results showed that mussel shell is an effective material and a less expensive material than materials that have traditionally been used, i.e., it may be used in the MSPD dispersion step during the extraction of pesticides and pharmaceutical and personal care products from golden mussel tissues. Graphical Abstract Vortex-assited matrix solid-phase dispersion for extraction of 11 pesticides and 9 PPCPs care products from mussel tissue samples.

Topological semimetals with Riemann surface states

NASA Astrophysics Data System (ADS)

Fang, Chen; Lu, Ling; Liu, Junwei; Fu, Liang

Topological semimetals have robust bulk band crossings between the conduction and the valence bands. Among them, Weyl semimetals are so far the only class having topologically protected signatures on the surface known as the ``Fermi arcs''. Here we theoretically find new classes of topological semimetals protected by nonsymmorphic glide reflection symmetries. On a symmetric surface, there are multiple Fermi arcs protected by nontrivial Z2 spectral flows between two high-symmetry lines (or two segments of one line) in the surface Brillouin zone. We observe that so far topological semimetals with protected Fermi arcs have surface dispersions that can be mapped to noncompact Riemann surfaces representing simple holomorphic functions. We propose perovskite superlattice [(SrIrO3)2m, (CaIrO3)2n] as a nonsymmorphic Dirac semimetal. C.F. and L.F. were supported by the S3TEC Solid State Solar Thermal Energy Conversion Center, an Energy Frontier Research Center funded by the U.S. Department of Energy (DOE), Office of Science, Basic Energy Sciences (BES), under Award No. DE-SC0001299/DE.

X-ray fluorescence surface contaminant analyzer: A feasibility study

NASA Technical Reports Server (NTRS)

Eldridge, Hudson B.

1988-01-01

The bonding of liner material to the inner metal surfaces of solid rocket booster cases is adversely affected by minute amounts of impurities on the metal surface. Suitable non-destructive methods currently used for detecting these surface contaminants do not provide the means of identifying their elemental composition. The feasibility of using isotopic source excited energy dispersive X-ray fluorescence as a possible technique for elemental analysis of such contaminants is investigated. A survey is made of the elemental compositions of both D-6ac steel, a common construction material for the booster cases, and Conoco HD-2 grease, a common surface contamination. Source and detector choices that maximize signal to noise ratio in a Recessed Source Geometry are made. A Monte Carlo simulation is then made of the optimized device incorporating the latest available X-ray constants at the energy of the chosen source to determine the device's response to a D-6ac steel surface contained with Conoco HD-2 grease.

Application of ethyl cellulose, microcrystalline cellulose and octadecanol for wax based floating solid dispersion pellets.

PubMed

Yan, Hong-Xiang; Zhang, Shuang-Shuang; He, Jian-Hua; Liu, Jian-Ping

2016-09-05

The present study aimed to develop and optimize the wax based floating sustained-release dispersion pellets for a weakly acidic hydrophilic drug protocatechuic acid to achieve prolonged gastric residence time and improved bioavailability. This low-density drug delivery system consisted of octadecanol/microcrystalline cellulose mixture matrix pellet cores prepared by extrusion-spheronization technique, coated with drug/ethyl cellulose 100cp solid dispersion using single-step fluid-bed coating method. The formulation-optimized pellets could maintain excellent floating state without lag time and sustain the drug release efficiently for 12h based on non-Fickian transport mechanism. Observed by SEM, the optimized pellet was the dispersion-layered spherical structure containing a compact inner core. DSC, XRD and FTIR analysis revealed drug was uniformly dispersed in the amorphous molecule form and had no significant physicochemical interactions with the polymer dispersion carrier. The stability study of the resultant pellets further proved the rationality and integrity of the developed formulation. Copyright © 2016 Elsevier Ltd. All rights reserved.

Magnetic dispersive solid-phase extraction based on modified magnetic nanoparticles for the detection of cocaine and cocaine metabolites in human urine by high-performance liquid chromatography-mass spectrometry.

PubMed

Yang, Feiyu; Zou, Yun; Ni, Chunfang; Wang, Rong; Wu, Min; Liang, Chen; Zhang, Jiabin; Yuan, Xiaoliang; Liu, Wenbin

2017-11-01

An easy-to-handle magnetic dispersive solid-phase extraction procedure was developed for preconcentration and extraction of cocaine and cocaine metabolites in human urine. Divinyl benzene and vinyl pyrrolidone functionalized silanized Fe 3 O 4 nanoparticles were synthesized and used as adsorbents in this procedure. Scanning electron microscopy, vibrating sample magnetometry, and infrared spectroscopy were employed to characterize the modified adsorbents. A high-performance liquid chromatography with mass spectrometry method for determination of cocaine and its metabolites in human urine sample has been developed with pretreatment of the samples by magnetic dispersive solid-phase extraction. The obtained results demonstrated the higher extraction capacity of the prepared nanoparticles with recoveries between 75.1 to 105.7% and correlation coefficients higher than 0.9971. The limits of detection for the cocaine and cocaine metabolites were 0.09-1.10 ng/mL. The proposed magnetic dispersive solid-phase extraction method provided a rapid, environmentally friendly and magnetic stuff recyclable approach and it was confirmed that the prepared adsorbents material was a kind of highly effective extraction materials for the trace cocaine and cocaine metabolites analyses in human urine. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Determination of haloacetic acids in water using layered double hydroxides as a sorbent in dispersive solid-phase extraction followed by liquid chromatography with tandem mass spectrometry.

PubMed

Alsharaa, Abdulnaser; Sajid, Muhammad; Basheer, Chanbasha; Alhooshani, Khalid; Lee, Hian Kee

2016-09-01

In the present study, highly efficient and simple dispersive solid-phase extraction procedure for the determination of haloacetic acids in water samples has been established. Three different types of layered double hydroxides were synthesized and used as a sorbent in dispersive solid-phase extraction. Due to the interesting behavior of layered double hydroxides in an acidic medium (pH˂4), the analyte elution step was not needed; the layered double hydroxides are simply dissolved in acid immediately after extraction to release the analytes which are then directly introduced into a liquid chromatography with tandem mass spectrometry system for analysis. Several dispersive solid-phase extraction parameters were optimized to increase the extraction efficiency of haloacetic acids such as temperature, extraction time and pH. Under optimum conditions, good linearity was achieved over the concentration range of 0.05-100 μg/L with detection limits in the range of 0.006-0.05 μg/L. The relative standard deviations were 0.33-3.64% (n = 6). The proposed method was applied to different water samples collected from a drinking water plant to determine the concentrations of haloacetic acids. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A Molecular-Level View of the Physical Stability of Amorphous Solid Dispersions

NASA Astrophysics Data System (ADS)

Yuan, Xiaoda

Many pharmaceutical compounds being developed in recent years are poorly soluble in water. This has led to insufficient oral bioavailability of many compounds in vitro. The amorphous formulation is one of the promising techniques to increase the oral bioavailability of these poorly water-soluble compounds. However, an amorphous drug substance is inherently unstable because it is a high energy form. In order to increase the physical stability, the amorphous drug is often formulated with a suitable polymer to form an amorphous solid dispersion. Previous research has suggested that the formation of an intimately mixed drug-polymer mixture contributes to the stabilization of the amorphous drug compound. The goal of this research is to better understand the role of miscibility, molecular interactions and mobility on the physical stability of amorphous solid dispersions. Methods were developed to detect different degrees of miscibility on nanometer scale and to quantify the extent of hydrogen-bonding interactions between the drug and the polymer. Miscibility, hydrogen-bonding interactions and molecular mobility were correlated with physical stability during a six-month period using three model systems. Overall, this research provides molecular-level insights into many factors that govern the physical stability of amorphous solid dispersions which can lead to a more effective design of stable amorphous formulations.

Recrystallization of nifedipine and felodipine from amorphous molecular level solid dispersions containing poly(vinylpyrrolidone) and sorbed water.

PubMed

Marsac, Patrick J; Konno, Hajime; Rumondor, Alfred C F; Taylor, Lynne S

2008-03-01

To compare the physical stability of amorphous molecular level solid dispersions of nifedipine and felodipine, in the presence of poly(vinylpyrrolidone) (PVP) and small amounts of moisture. Thin amorphous films of nifedipine and felodipine and amorphous molecular level solid dispersions with PVP were stored at various relative humidities (RH) and the nucleation rate was measured. The amount of water sorbed at each RH was measured using isothermal vapor sorption and glass transition temperatures (Tg) were determined using differential scanning calorimetry. The solubility of each compound in methyl pyrrolidone was measured as a function of water content. Nifedipine crystallizes more easily than felodipine at any given polymer concentration and in the presence of moisture. The glass transition temperatures of each compound, alone and in the presence of PVP, are statistically equivalent at any given water content. The nifedipine systems are significantly more hygroscopic than the corresponding felodipine systems. Variations in the physical stability of the two compounds could not be explained by differences in Tg. However, the relative physical stability is consistent with differences in the degree of supersaturation of each drug in the solid dispersion, treating the polymer and water as a co-solvent system for each drug compound.

Determination of sulfonamides in livers using matrix solid-phase dispersion extraction high-performance liquid chromatography.

PubMed

Zhang, Yupu; Xu, Xu; Qi, Xiao; Gao, Wenquan; Sun, Shuo; Li, Xiaotian; Jiang, Chengfei; Yu, Aimin; Zhang, Hanqi; Yu, Yong

2012-01-01

The matrix solid-phase dispersion (MSPD) was applied for extracting seven sulfonamides (SAs) in liver samples. The separation and determination were carried out by high-performance liquid chromatography. The analytes were derivated with fluorescamine and detected with fluorescence detector. The types of dispersion adsorbents for MSPD were examined and the highest recovery was obtained when the diatomaceous earth was used as the dispersion adsorbent and the mass ratio of dispersion adsorbent to sample was 3:1. The acetone was used as the elution solvent. Under the optimal conditions, the linear range for determining the SAs in liver samples was 5.0-1000.0 ng/g. The porcine, chicken and cattle liver samples were analyzed and the average recoveries of seven SAs were higher than 84.6%. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A novel solid digestate-derived biochar-Cu NP composite activating H2O2 system for simultaneous adsorption and degradation of tetracycline.

PubMed

Fu, Dun; Chen, Zheng; Xia, Dong; Shen, Liang; Wang, Yuanpeng; Li, Qingbiao

2017-02-01

Solid digestate, a by-product of anaerobic digestion systems, has led to a range of environmental issues. In the present study, a novel composite based on a solid digestate-biochar-Cu NP composite was synthesized for tetracycline removal from an aqueous medium. The removal efficiency values for tetracycline (200 mg L -1 ) were 31.5% and 97.8%, respectively, by the biochar-Cu NP composite (0.5 g L -1 ) in the absence and presence of hydrogen peroxide (H 2 O 2 , 20 mM) within 6 h of reaction time. The possible degradation pathway of tetracycline was investigated using liquid chromatography-mass spectrometry. The desorption experiment results suggested that no significant concentration of tetracycline was detected on the composite after the reaction, but a small amount of intermediates in terms of total organic carbon (TOC) accounting for 3.1%, and 23.3% of the end-product NH 4 + was adsorbed onto the biochar sheets. The dispersive Cu NPs on the biochar resulted in an increase in the surface area and pore volume of the biochar-Cu NP composite, which enhanced tetracycline adsorption as well as the degradation efficiency. Relative tetracycline removal mechanisms were dominantly ascribed to ·OH generation from the Cu(II)/Cu(I) redox reaction with H 2 O 2 and the electron-transfer process of free radicals (FRs) in biochar. The proposed approach serves dual purposes of waste digestate reuse and treatment of antibiotic pollutants. This study highlights the activation of H 2 O 2 by the dispersive Cu NPs coupling with biochar derived from a waste solid digestate for tetracycline treatment. Copyright © 2016. Published by Elsevier Ltd.

Shall we upgrade one-dimensional secondary settler models used in WWTP simulators? - An assessment of model structure uncertainty and its propagation.

PubMed

Plósz, Benedek Gy; De Clercq, Jeriffa; Nopens, Ingmar; Benedetti, Lorenzo; Vanrolleghem, Peter A

2011-01-01

In WWTP models, the accurate assessment of solids inventory in bioreactors equipped with solid-liquid separators, mostly described using one-dimensional (1-D) secondary settling tank (SST) models, is the most fundamental requirement of any calibration procedure. Scientific knowledge on characterising particulate organics in wastewater and on bacteria growth is well-established, whereas 1-D SST models and their impact on biomass concentration predictions are still poorly understood. A rigorous assessment of two 1-DSST models is thus presented: one based on hyperbolic (the widely used Takács-model) and one based on parabolic (the more recently presented Plósz-model) partial differential equations. The former model, using numerical approximation to yield realistic behaviour, is currently the most widely used by wastewater treatment process modellers. The latter is a convection-dispersion model that is solved in a numerically sound way. First, the explicit dispersion in the convection-dispersion model and the numerical dispersion for both SST models are calculated. Second, simulation results of effluent suspended solids concentration (XTSS,Eff), sludge recirculation stream (XTSS,RAS) and sludge blanket height (SBH) are used to demonstrate the distinct behaviour of the models. A thorough scenario analysis is carried out using SST feed flow rate, solids concentration, and overflow rate as degrees of freedom, spanning a broad loading spectrum. A comparison between the measurements and the simulation results demonstrates a considerably improved 1-D model realism using the convection-dispersion model in terms of SBH, XTSS,RAS and XTSS,Eff. Third, to assess the propagation of uncertainty derived from settler model structure to the biokinetic model, the impact of the SST model as sub-model in a plant-wide model on the general model performance is evaluated. A long-term simulation of a bulking event is conducted that spans temperature evolution throughout a summer/winter sequence. The model prediction in terms of nitrogen removal, solids inventory in the bioreactors and solids retention time as a function of the solids settling behaviour is investigated. It is found that the settler behaviour, simulated by the hyperbolic model, can introduce significant errors into the approximation of the solids retention time and thus solids inventory of the system. We demonstrate that these impacts can potentially cause deterioration of the predictive power of the biokinetic model, evidenced by an evaluation of the system's nitrogen removal efficiency. The convection-dispersion model exhibits superior behaviour, and the use of this type of model thus is highly recommended, especially bearing in mind future challenges, e.g., the explicit representation of uncertainty in WWTP models.

Graphene oxide decorated with silver nanoparticles as a coating on a stainless-steel fiber for solid-phase microextraction.

PubMed

Wang, Licheng; Hou, Xiudan; Li, Jubai; Liu, Shujuan; Guo, Yong

2015-07-01

A novel graphene oxide decorated with silver nanoparticles coating on a stainless-steel fiber for solid-phase microextraction was prepared. Scanning electron microscopy and X-ray photoelectron spectroscopy were used to characterize the coating surface and showed that silver nanoparticles were dispersed on the wrinkled graphene oxide surface. Coupled to gas chromatography with flame ionization detection, the extraction abilities of the fiber for polycyclic aromatic hydrocarbons were examined in the headspace solid-phase microextraction mode. The extraction parameters including adsorption time, adsorption temperature, salt concentration, desorption time and desorption temperature were investigated. Under the optimized condition, wide linearity with low limits of detection from 2 to 10 ng/L was obtained. The relative standard deviations for single-fiber repeatability and fiber-to-fiber reproducibility were less than 10.6 and 17.5%, respectively. The enrichment factors were from 1712.5 to 4503.7, showing the fiber has good extraction abilities. Moreover, the fiber exhibited a good stability and could be reused for more than 120 times. The established method was also applied for determination of polycyclic aromatic hydrocarbons in two real water samples and the recoveries of analytes ranged from 84.4-116.3% with relative standard deviations less than 16.2%. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Wetting properties of phospholipid dispersion on tunable hydrophobic SiO2-glass plates.

PubMed

Alexandrova, Lidia; Karakashev, Stoyan I; Grigorov, L; Phan, Chi M; Smoukov, Stoyan K

2015-06-01

We study the wetting properties of very small droplets of salty aqueous suspensions of unilamellar liposomes of DMPC (dimyristoylphosphatidylcholine), situated on SiO2-glass surfaces with different levels of hydrophobicity. We evaluated two different measures of hydrophobicity of solid surfaces - receding contact angles and the thickness of wetting films trapped between an air bubble and the solid surface at different levels of hydrophobicity. We established a good correlation between methods which differ significantly in measurement difficulty and experimental setup. We also reveal details of the mechanism of wetting of different surfaces by the DMPC liposome suspension. Hydrophilic surfaces with water contact angles in the range of 0° to 35° are readily hydrophobized by the liposomes and only showed corresponding contact angles in the range 27°-43°. For same range of surface hydrophobicities, there was a clear reduction of the thickness of the wetting films between the surface and a bubble, reaching a minimum in the 35°-40° range. At higher levels of hydrophobicity both pure water and the liposome suspension show similar contact angles, and the thickness of wetting films between a bubble and those surfaces increases in parallel. Our analysis showed that the only force able to stabilize the film under these experimental conditions is steric repulsion. The latter suggests that nanobubbles adsorbed on hydrophobic parts of the surface, and coated with a DMPC layer, may be the cause of the 40-70 nm thickness of wetting films we observe. Copyright © 2014 Elsevier B.V. All rights reserved.

Wave dispersion and propagation in state-based peridynamics

NASA Astrophysics Data System (ADS)

Butt, Sahir N.; Timothy, Jithender J.; Meschke, Günther

2017-11-01

Peridynamics is a nonlocal continuum model which offers benefits over classical continuum models in cases, where discontinuities, such as cracks, are present in the deformation field. However, the nonlocal characteristics of peridynamics leads to a dispersive dynamic response of the medium. In this study we focus on the dispersion properties of a state-based linear peridynamic solid model and specifically investigate the role of the peridynamic horizon. We derive the dispersion relation for one, two and three dimensional cases and investigate the effect of horizon size, mesh size (lattice spacing) and the influence function on the dispersion properties. We show how the influence function can be used to minimize wave dispersion at a fixed lattice spacing and demonstrate it qualitatively by wave propagation analysis in one- and two-dimensional models of elastic solids. As a main contribution of this paper, we propose to associate peridynamic non-locality expressed by the horizon with a characteristic length scale related to the material microstructure. To this end, the dispersion curves obtained from peridynamics are compared with experimental data for two kinds of sandstone.

Derivation of Hamaker Dispersion Energy of Amorphous Carbon Surfaces in Contact with Liquids Using Photoelectron Energy-Loss Spectra

NASA Astrophysics Data System (ADS)

Godet, Christian; David, Denis

2017-12-01

Hamaker interaction energies and cutoff distances have been calculated for disordered carbon films, in contact with purely dispersive (diiodomethane) or polar (water) liquids, using their experimental dielectric functions ɛ ( q, ω) obtained over a broad energy range. In contrast with previous works, a q-averaged < ɛ ( q, ω) > q is derived from photoelectron energy-loss spectroscopy (XPS-PEELS) where the energy loss function (ELF) < Im[-1/ ɛ ( q, ω)] > q is a weighted average over allowed transferred wave vector values, q, given by the physics of bulk plasmon excitation. For microcrystalline diamond and amorphous carbon films with a wide range of (sp3/sp2 + sp3) hybridization, non-retarded Hamaker energies, A 132 ( L < 1 nm), were calculated in several configurations, and distance and wavenumber cutoff values were then calculated based on A 132 and the dispersive work of adhesion obtained from contact angles. A geometric average approximation, H 0 CVL = ( H 0 CVC H 0 LVL )1/2, holds for the cutoff separation distances obtained for carbon-vacuum-liquid (CVL), carbon-vacuum-carbon (CVC) and liquid-vacuum-liquid (LVL) equilibrium configurations. The linear dependence found for A CVL, A CLC and A CLV values as a function of A CVC, for each liquid, allows predictive relationships for Hamaker energies (in any configuration) using experimental determination of the dispersive component of the surface tension, {γ}_{CV}^d , and a guess value of the cutoff distance H 0 CVC of the solid. [Figure not available: see fulltext.

Influence of type and level of water-soluble additives on drug release and surface and mechanical properties of Surelease films.

PubMed

Rohera, Bhagwan D; Parikh, Nilesh H

2002-11-01

Ethylcellulose in combination with water-soluble additives has been used in the development of microporous membrane-coated dosage forms. In the present study, application of three types of water-soluble additives, namely polyethylene glycols (PEG 400, 3350, and 8000), maltodextrins (Maltrin M150, M100, and M040 in the order of lower to higher average polymer size and molecular weight; dextrose equivalence 16.9, 11.1, and 4.8, respectively), and xylitol, as porosity modifiers in the films of a commercially available aqueous ethylcellulose dispersion (Surelease/E-7-7060 plasticized with glyceryl tricaprylate/caprate) was investigated. The effect of type and level of these additives on drug release characteristics and surface and mechanical properties of the polymeric films was studied. Each additive was incorporated at 20 and 30% levels in the polymeric dispersion based on its solids content. Ibuprofen tablets were coated using the polymeric dispersion with and without additive at 3% w/w coat level in a fluid-bed equipment. The coated tablets were evaluated for their drug release rate, coat reflectivity (gloss), Brinell hardness, and elastic modulus. Differential scanning calorimetric analysis of the films was performed to determine the physico-chemical changes in the applied film-coats. The rate of drug release, hence film porosity, was observed to be dependent on the type and level of the additive added. The molecular weight of the additive and its concentration in the polymeric dispersion had significant influence on the rate of drug release, hardness, and elasticity of the film-coats.

78 FR 22256 - Proposed Information Collection Request; Comment Request; The National Oil and Hazardous...

Federal Register 2010, 2011, 2012, 2013, 2014

2013-04-15

... Chemicals''). The use of bioremediation agents, dispersants, surface washing agents, surface collecting... basic categories: dispersants, surface washing agents, surface collecting agents, bioremediation agents..., manufacturers of bioremediation agents, dispersants, surface collecting agents, surface washing agents...

Viscoelastic love-type surface waves

USGS Publications Warehouse

Borcherdt, Roger D.

2008-01-01

The general theoretical solution for Love-Type surface waves in viscoelastic media provides theoreticalexpressions for the physical characteristics of the waves in elastic as well as anelastic media with arbitraryamounts of intrinsic damping. The general solution yields dispersion and absorption-coefficient curves for the waves as a function of frequency and theamount of intrinsic damping for any chosen viscoelastic model.Numerical results valid for a variety of viscoelastic models provide quantitative estimates of the physicalcharacteristics of the waves pertinent to models of Earth materials ranging from small amounts of damping in the Earth’s crust to moderate and large amounts of damping in soft soils and water-saturated sediments. Numerical results, presented herein, are valid for a wide range of solids and applications.

Characterizing shallow secondary clarifier performance where conventional flux theory over-estimates allowable solids loading rate.

PubMed

Daigger, Glen T; Siczka, John S; Smith, Thomas F; Frank, David A; McCorquodale, J A

The performance characteristics of relatively shallow (3.3 and 3.7 m sidewater depth in 30.5 m diameter) activated sludge secondary clarifiers were extensively evaluated during a 2-year testing program at the City of Akron Water Reclamation Facility (WRF), Ohio, USA. Testing included hydraulic and solids loading stress tests, and measurement of sludge characteristics (zone settling velocity (ZSV), dispersed and flocculated total suspended solids), and the results were used to calibrate computational fluid dynamic (CFD) models of the various clarifiers tested. The results demonstrated that good performance could be sustained at surface overflow rates in excess of 3 m/h, as long as the clarifier influent mixed liquor suspended solids (MLSS) concentration was controlled to below critical values. The limiting solids loading rate (SLR) was significantly lower than the value predicted by conventional solids flux analysis based on the measured ZSV/MLSS relationship. CFD analysis suggested that this resulted because mixed liquor entering the clarifier was being directed into the settled sludge blanket, diluting it and also creating a 'thin' concentration sludge blanket that overlays the thicker concentration sludge blanket typically expected. These results indicate the need to determine the allowable SLR for shallow clarifiers using approaches other than traditional solids flux analysis. A combination of actual testing and CFD analyses are demonstrated here to be effective in doing so.

An investigation into the use of polymer blends to improve the printability of and regulate drug release from pharmaceutical solid dispersions prepared via fused deposition modeling (FDM) 3D printing.

PubMed

Alhijjaj, Muqdad; Belton, Peter; Qi, Sheng

2016-11-01

FDM 3D printing has been recently attracted increasing research efforts towards the production of personalized solid oral formulations. However, commercially available FDM printers are extremely limited with regards to the materials that can be processed to few types of thermoplastic polymers, which often may not be pharmaceutically approved materials nor ideal for optimizing dosage form performance of poor soluble compounds. This study explored the use of polymer blends as a formulation strategy to overcome this processability issue and to provide adjustable drug release rates from the printed dispersions. Solid dispersions of felodipine, the model drug, were successfully fabricated using FDM 3D printing with polymer blends of PEG, PEO and Tween 80 with either Eudragit E PO or Soluplus. As PVA is one of most widely used polymers in FDM 3D printing, a PVA based solid dispersion was used as a benchmark to compare the polymer blend systems to in terms of processability. The polymer blends exhibited excellent printability and were suitable for processing using a commercially available FDM 3D printer. With 10% drug loading, all characterization data indicated that the model drug was molecularly dispersed in the matrices. During in vitro dissolution testing, it was clear that the disintegration behavior of the formulations significantly influenced the rates of drug release. Eudragit EPO based blend dispersions showed bulk disintegration; whereas the Soluplus based blends showed the 'peeling' style disintegration of strip-by-strip. The results indicated that interplay of the miscibility between excipients in the blends, the solubility of the materials in the dissolution media and the degree of fusion between the printed strips during FDM process can be used to manipulate the drug release rate of the dispersions. This brings new insight into the design principles of controlled release formulations using FDM 3D printing. Copyright © 2016 Elsevier B.V. All rights reserved.

Predicting final product properties of melt extruded solid dispersions from process parameters using Raman spectrometry.

PubMed

Vigh, Tamás; Drávavölgyi, Gábor; Sóti, Péter L; Pataki, Hajnalka; Igricz, Tamás; Wagner, István; Vajna, Balázs; Madarász, János; Marosi, György; Nagy, Zsombor K

2014-09-01

Raman spectrometry was utilized to estimate degraded drug percentage, residual drug crystallinity and glass-transition temperature in the case of melt-extruded pharmaceutical products. Tight correlation was shown between the results obtained by confocal Raman mapping and transmission Raman spectrometry, a PAT-compatible potential in-line analytical tool. Immediate-release spironolactone-Eudragit E solid dispersions were the model system, owing to the achievable amorphization and the heat-sensitivity of the drug compound. The deep investigation of the relationship between process parameters, residual drug crystallinity and degradation was performed using statistical tools and a factorial experimental design defining 54 different circumstances for the preparation of solid dispersions. From the examined factors, drug content (10, 20 and 30%), temperature (110, 130 and 150°C) and residence time (2.75, 11.00 and 24.75min) were found to have significant and considerable effect. By forming physically stable homogeneous dispersions, the originally very slow dissolution of the lipophilic and poorly water-soluble spironolactone was reasonably improved, making 3minute release possible in acidic medium. Copyright © 2014 Elsevier B.V. All rights reserved.

Dispersive Solid Phase Extraction for the Analysis of Veterinary Drugs Applied to Food Samples: A Review

PubMed Central

Islas, Gabriela; Hernandez, Prisciliano

2017-01-01

To achieve analytical success, it is necessary to develop thorough clean-up procedures to extract analytes from the matrix. Dispersive solid phase extraction (DSPE) has been used as a pretreatment technique for the analysis of several compounds. This technique is based on the dispersion of a solid sorbent in liquid samples in the extraction isolation and clean-up of different analytes from complex matrices. DSPE has found a wide range of applications in several fields, and it is considered to be a selective, robust, and versatile technique. The applications of dispersive techniques in the analysis of veterinary drugs in different matrices involve magnetic sorbents, molecularly imprinted polymers, carbon-based nanomaterials, and the Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) method. Techniques based on DSPE permit minimization of additional steps such as precipitation, centrifugation, and filtration, which decreases the manipulation of the sample. In this review, we describe the main procedures used for synthesis, characterization, and application of this pretreatment technique and how it has been applied to food analysis. PMID:29181027

Preparation of almost dispersant-free colloidal silica with superb dispersiblility in organic solvents and monomers

NASA Astrophysics Data System (ADS)

Huang, Feng-Hsi; Chang, Chao-Ching; Oyang, Tai-Yueh; Chen, Ching-Chung; Cheng, Liao-Ping

2011-09-01

Surface modification of silica nanoparticles synthesized by the sol-gel process was performed using coupling agents, 3-(trimethoxysilyl) propyl methacrylate (MSMA) and/or trimethyethoxylsilane (TMES). The chemical structures of the formed particles were analyzed by means of Fourier Transform Infrared Spectroscopy (FTIR) and solid-state Si-Nuclear Magnetic Resonance (Si-NMR), and the particle sizes were determined by Transmission Electron Microscopy (TEM) imaging. The latter results indicate that such surface modifications can effectively lessen the serious aggregation being common to pure silica nanoparticles. In some cases, separate particles of ca. 5-10 nm dia. could be obtained, when both MSMA and TMES were employed during the modification process. Dynamic light scattering method was adopted to examine the stability of the prepared silica sols during a long-term storage. It was found that the aggregation phenomenon can essentially be eliminated in case that the surface of silica contained sufficient amount of TMES moiety. Vacuum distillation was used to remove the volatile components such as methanol, ethanol, and water from the silica sol. The condensed product, containing 2 wt% residual solvent, appeared as a uniform transparent paste-like material, which can be dispersed in common organic solvents and monomers within a few seconds.

Isoelectric points and points of zero charge of metal (hydr)oxides: 50years after Parks' review.

PubMed

Kosmulski, Marek

2016-12-01

The pH-dependent surface charging of metal (hydr)oxides is reviewed on the occasion of the 50th anniversary of the publication by G.A. Parks: "Isoelectric points of solid oxides, solid hydroxides, and aqueous hydroxo complex systems" in Chemical Reviews. The point of zero charge (PZC) and isoelectric point (IEP) became standard parameters to characterize metal oxides in aqueous dispersions, and they define adsorption (surface excess) of ions, stability against coagulation, rheological properties of dispersions, etc. They are commonly used in many branches of science including mineral processing, soil science, materials science, geochemistry, environmental engineering, and corrosion science. Parks established standard procedures and experimental conditions which are required to obtain reliable and reproducible values of PZC and IEP. The field is very active, and the number of related papers exceeds 300 a year, and the standards established by Parks remain still valid. Relevant experimental techniques improved over the years, especially the measurements of electrophoretic mobility became easier and more reliable, are the numerical values of PZC and IEP compiled by Parks were confirmed by contemporary publications with a few exceptions. The present paper is an up-to-date compilation of the values of PZC and IEP of metal oxides. Unlike in former reviews by the same author, which were more comprehensive, only limited number of selected results are presented and discussed here. On top of the results obtained by means of classical methods (titration and electrokinetic methods), new methods and correlations found over the recent 50years are presented. Copyright © 2016 Elsevier B.V. All rights reserved.

Aqueous processing of composite lithium ion electrode material

DOEpatents

Li, Jianlin; Armstrong, Beth L.; Daniel, Claus; Wood, III, David L.

2017-06-20

A method of making a battery electrode includes the steps of dispersing an active electrode material and a conductive additive in water with at least one dispersant to create a mixed dispersion; treating a surface of a current collector to raise the surface energy of the surface to at least the surface tension of the mixed dispersion; depositing the dispersed active electrode material and conductive additive on a current collector; and heating the coated surface to remove water from the coating.

Aqueous processing of composite lithium ion electrode material

DOEpatents

Li, Jianlin; Armstrong, Beth L; Daniel, Claus; Wood, III, David L

2015-02-17

A method of making a battery electrode includes the steps of dispersing an active electrode material and a conductive additive in water with at least one dispersant to create a mixed dispersion; treating a surface of a current collector to raise the surface energy of the surface to at least the surface tension of the mixed dispersion; depositing the dispersed active electrode material and conductive additive on a current collector; and heating the coated surface to remove water from the coating.

Bladder stone in a human female: The case of an abnormally located intrauterine contraceptive device

DOE Office of Scientific and Technical Information (OSTI.GOV)

Khan, S.R.; Wilkinson, E.J.

A single 4.7 x 3.3 x 1.5 cm solid nodule was removed from the bladder of a 24 years old white female who had lost an intrauterine contraceptive device (IUD) installed approximately four years ago. The nodule showed no external evidence of an IUD or its string. An examination of the nodular surface by scanning electron microscopy (SEM) showed mostly amorphous material with some adherent filamentous structures. Its energy dispersive x-ray microanalysis revealed the presence of calcium and phosphorus suggesting that the nodule was actually a urolith. Fracturing the nodule exposed an embedded entity consistent with being a copper IUD.more » Apparently, the lost IUD had migrated from the uterus into the bladder where it became mineralized. Thus the solid nodule was actually a foreign body stone.« less

Dispersion Energy Analysis of Rayleigh and Love Waves in the Presence of Low-Velocity Layers in Near-Surface Seismic Surveys

NASA Astrophysics Data System (ADS)

Mi, Binbin; Xia, Jianghai; Shen, Chao; Wang, Limin

2018-03-01

High-frequency surface-wave analysis methods have been effectively and widely used to determine near-surface shear (S) wave velocity. To image the dispersion energy and identify different dispersive modes of surface waves accurately is one of key steps of using surface-wave methods. We analyzed the dispersion energy characteristics of Rayleigh and Love waves in near-surface layered models based on numerical simulations. It has been found that if there is a low-velocity layer (LVL) in the half-space, the dispersion energy of Rayleigh or Love waves is discontinuous and ``jumping'' appears from the fundamental mode to higher modes on dispersive images. We introduce the guided waves generated in an LVL (LVL-guided waves, a trapped wave mode) to clarify the complexity of the dispersion energy. We confirm the LVL-guided waves by analyzing the snapshots of SH and P-SV wavefield and comparing the dispersive energy with theoretical values of phase velocities. Results demonstrate that LVL-guided waves possess energy on dispersive images, which can interfere with the normal dispersion energy of Rayleigh or Love waves. Each mode of LVL-guided waves having lack of energy at the free surface in some high frequency range causes the discontinuity of dispersive energy on dispersive images, which is because shorter wavelengths (generally with lower phase velocities and higher frequencies) of LVL-guided waves cannot penetrate to the free surface. If the S wave velocity of the LVL is higher than that of the surface layer, the energy of LVL-guided waves only contaminates higher mode energy of surface waves and there is no interlacement with the fundamental mode of surface waves, while if the S wave velocity of the LVL is lower than that of the surface layer, the energy of LVL-guided waves may interlace with the fundamental mode of surface waves. Both of the interlacements with the fundamental mode or higher mode energy may cause misidentification for the dispersion curves of surface waves.

Recycling polyethylene terephthalate wastes as short fibers in Strain-Hardening Cementitious Composites (SHCC).

PubMed

Lin, Xiuyi; Yu, Jing; Li, Hedong; Lam, Jeffery Y K; Shih, Kaimin; Sham, Ivan M L; Leung, Christopher K Y

2018-05-26

As an important portion of the total plastic waste bulk but lack of reuse and recycling, the enormous amounts of polyethylene terephthalate (PET) solid wastes have led to serious environmental issues. This study explores the feasibility of recycling PET solid wastes as short fibers in Strain-Hardening Cementitious Composites (SHCCs), which exhibit strain-hardening and multiple cracking under tension, and therefore have clear advantages over conventional concrete for many construction applications. Based on micromechanical modeling, fiber dispersion and alkali resistance, the size of recycled PET fibers was first determined. Then the hydrophobic PET surface was treated with NaOH solution followed by a silane coupling agent to achieve the dual purpose of improving the fiber/matrix interfacial frictional bond (from 0.64 MPa to 0.80 MPa) and enhancing the alkali resistance for applications in alkaline cementitious environment. With surface treatment, recycling PET wastes as fibers in SHCCs is a promising approach to significantly reduce the material cost of SHCCs while disposing hazardous PET wastes in construction industry. Copyright © 2018 Elsevier B.V. All rights reserved.

Distinguishability of N Composition Profiles In SiON Films On Si By Angle-Resolved X-ray Photoelectron Spectroscopy

NASA Astrophysics Data System (ADS)

Powell, C. J.; Werner, W. S. M.; Smekal, W.

2007-09-01

We report on the use of the NIST Database for the Simulation of Electron Spectra for Surface Analysis (SESSA) to determine N 1s, O 1s, and Si 2p3/2 photoelectron intensities for a 25 Å SiON film on a Si substrate with different distributions of N in the film. These simulations were made to assess the distinguishability of angle-resolved x-ray photoelectron spectroscopy (ARXPS) signals for each N distribution. Our approach differs from conventional simulations of ARXPS data in that we do not neglect elastic scattering of the photoelectrons and the finite solid angle of the analyzer. Appreciable dispersion of the photoelectron intensities was found only for the N 1s intensities at an emission angle of 75° (with respect to the surface normal). Conventional analyses of ARXPS data that include such large emission angles are unlikely to be valid due to angle-dependent changes of the attenuation length. We demonstrate the magnitude of elastic-scattering and analyzer solid-angle effects on the calculated angular distributions.

One-step continuous extrusion process for the manufacturing of solid dispersions.

PubMed

Maniruzzaman, M; Nair, A; Scoutaris, N; Bradley, Michael S A; Snowden, M J; Douroumis, D

2015-12-30

The purpose of this study was to evaluate the performance of synthetic magnesium aluminometasilicate (MAS) as a novel inorganic carrier in hot melt extrusion (HME) processing of indomethacin (IND) for the development of solid dispersions. A continuous extrusion process at various IND/excipient blend ratios (20%, 30% and 40%) was performed using a twin-screw extruder. Physicochemical characterization carried out by SEM, DSC, and XRPD demonstrated the presence of IND in amorphous nature within the porous network of the inorganic material for all extruded formulations. Further, AFM and FTIR studies revealed a single-phase amorphous system and intermolecular H-bonding formation. The IND/MAS extrudates showed enhanced INM dissolution rates within 100% been released within 1h. Stability studies under accelerated conditions (40°C, RH 75%) showed that MAS retained the physical stability of the amorphous solid dispersions even at high drug loadings for 12 months. Copyright © 2015 Elsevier B.V. All rights reserved.

The investigation of MCM-48-type and MCM-41-type mesoporous silica as oral solid dispersion carriers for water insoluble cilostazol.

PubMed

Wang, Yanzhu; Sun, Lizhang; Jiang, Tongying; Zhang, Jinghai; Zhang, Chen; Sun, Changshan; Deng, Yihui; Sun, Jin; Wang, Siling

2014-06-01

To explore the suitable application of MCM-41 (Mobil Composition of Matter number forty-one)-type and MCM-48-type mesoporous silica in the oral water insoluble drug delivery system. Cilostazol (CLT) as a model drug was loaded into synthesized MCM-48 (Mobil Composition of Matter number forty-eight) and commercial MCM-41 by three common methods. The obtained MCM-41, MCM-48 and CLT-loaded samples were characterized by means of nitrogen adsorption, thermogravimetric analysis, ultraviolet-visible spectrophotometry, scanning electron microscopy, transmission electron microscopy, differential scanning calorimetry and powder X-ray diffractometer. It was found that solvent evaporation method was preferred according to the drug loading efficiency and the maximum percent cumulative drug dissolution. MCM-48 with 3D cubic pore structure and MCM-41 with 2D long tubular structure are nearly spherical particles in 300-500 nm. Nevertheless, the silica carriers with similar large specific surface areas and concentrating pore size distributions (978.66 m(2)/g, 3.8 nm for MCM-41 and 1108.04 m(2)/g, 3.6 nm for MCM-48) exhibited different adsorption behaviors for CLT. The maximum percent cumulative drug release of the two CLT/silica solid dispersion (CLT-MCM-48 and CLT-MCM-41) was 63.41% and 85.78% within 60 min, respectively; while in the subsequent 12 h release experiment, almost 100% cumulative drug release were both obtained. In the pharmacokinetics aspect, the maximum plasma concentrations of CLT-MCM-48 reached 3.63 mg/L by 0.92 h. The AUC0-∞ values of the CLT-MCM-41 and CLT-MCM-48 were 1.14-fold and 1.73-fold, respectively, compared with the commercial preparation. Our findings suggest that MCM-41-type and MCM-48-type mesoporous silica have great promise as solid dispersion carriers for sustained and immediate release separately.

40 CFR 227.29 - Initial mixing.

Code of Federal Regulations, 2012 CFR

2012-07-01

...) Initial mixing is defined to be that dispersion or diffusion of liquid, suspended particulate, and solid... adequate to predict initial dispersion and diffusion of the waste, these shall be used, if necessary, in.... (2) When field data on the dispersion and diffusion of a waste of characteristics similar to that...

40 CFR 227.29 - Initial mixing.

Code of Federal Regulations, 2011 CFR

2011-07-01

...) Initial mixing is defined to be that dispersion or diffusion of liquid, suspended particulate, and solid... adequate to predict initial dispersion and diffusion of the waste, these shall be used, if necessary, in.... (2) When field data on the dispersion and diffusion of a waste of characteristics similar to that...

40 CFR 227.29 - Initial mixing.

Code of Federal Regulations, 2014 CFR

2014-07-01

...) Initial mixing is defined to be that dispersion or diffusion of liquid, suspended particulate, and solid... adequate to predict initial dispersion and diffusion of the waste, these shall be used, if necessary, in.... (2) When field data on the dispersion and diffusion of a waste of characteristics similar to that...

40 CFR 227.29 - Initial mixing.

Code of Federal Regulations, 2013 CFR

2013-07-01

...) Initial mixing is defined to be that dispersion or diffusion of liquid, suspended particulate, and solid... adequate to predict initial dispersion and diffusion of the waste, these shall be used, if necessary, in.... (2) When field data on the dispersion and diffusion of a waste of characteristics similar to that...

Shear thickening in suspensions: the lubricated-to-frictional contact scenario

NASA Astrophysics Data System (ADS)

Morris, Jeffrey

2017-11-01

Suspensions of solid particles in viscous liquids can vary from low-viscosity liquids to wet granular materials or soft solids depending on the solids loading and the forces acting between particles. When the particles are very concentrated, these mixtures are ''dense suspensions.'' Dense suspensions often exhibit shear thickening, an increase in apparent viscosity as the shear rate is increased. In its most extreme form, order of magnitude increases in viscosity over such a narrow range in shear rate occur that the term discontinuous shear thickening (DST) is applied. DST is particularly striking as it occurs in the relatively simple case of nearly hard spheres in a Newtonian liquid, and is found to take place for submicron particles in colloidal dispersions to much larger particle corn starch dispersions. We focus on simulations of a recently developed ``lubricated-to-frictional'' rheology in which the interplay of viscous lubrication, repulsive surface forces, and contact friction between particle surfaces provides a scenario to explain DST. Our simulation method brings together elements of the discrete-element method from granular flow with a simplified Stokesian Dynamics, and can rationalize not only the abrupt change in properties with imposed shear rate (or shear stress), but also the magnitude of the change. The large change in properties is associated with the breakdown of lubricating films between particles, with activation of Coulomb friction between particles. The rate dependence is caused by the shearing forces driving particles to contact, overwhelming conservative repulsive forces between surfaces; the repulsive forces are representative of colloidal stabilization by surface charge or steric effects, e.g. due to adsorbed polymer. The results of simulation are compared to developments by other groups, including a number of experimental studies and a theory incorporating the same basic elements as the simulation. The comparison to experiments of the predictions of the lubricated-to-frictional rheology is generally good, but discrepancies demand some perspective on the strong simplifying assumptions in the model. Since contact is difficult to both establish and to characterize for surfaces between particles of micron scale or smaller, what is happening in the very close ``contacts'' is not clear, and how changes at this scale give rise to the large-scale force organization is yet to be established. The insight to the elements needed for the abrupt flow induced transition seen in DST thus suggests a need for consideration of both the microscopic physics of contact and the statistical physics governing the macroscopic properties. This work was supported in part by the NSF CBET program, Grant # 1605283.

Coupling between magnetic and optical properties of stable Au-Fe solid solution nanoparticles

NASA Astrophysics Data System (ADS)

de Julián Fernández, C.; Mattei, G.; Paz, E.; Novak, R. L.; Cavigli, L.; Bogani, L.; Palomares, F. J.; Mazzoldi, P.; Caneschi, A.

2010-04-01

Au-Fe nanoparticles constitute one of the simplest prototypes of a multifunctional nanomaterial that can exhibit both magnetic and optical (plasmonic) properties. This solid solution, not feasible in the bulk phase diagram in thermal equilibrium, can be formed as a nanostructure by out-of-equilibrium processes. Here, the novel magnetic, optical and magneto-optical properties of ion-implanted Au-Fe solid solution nanoparticles dispersed in a SiO2 matrix are investigated and correlated. The surface plasmon resonance of the Au-Fe nanoparticles with almost equicomposition is strongly damped when compared to pure Au and to Au-rich Au-Fe nanoparticles. In all cases, the Au atoms are magnetically polarized, as measured by x-ray magnetic circular dichroism, and ferromagnetically coupled with Fe atoms. Although the chemical stability of Au-Fe nanoparticles is larger than that of Fe nanoparticles, both the magnetic moment per Fe atom and the order temperature are smaller. These results suggest that electronic and magnetic properties are more influenced by the hybridization of the electronic bands in the Au-Fe solid solution than by size effects. On the other hand, the magneto-optical transitions allowed in the vis-nIR spectral regions are very similar. In addition, we also observe, after studying the properties of thermally treated samples, that the Au-Fe alloy is stabilized, not by surface effects, but by the combination of the out-of-equilibrium nature of the ion implantation technique and by changes in the properties due to size effects.

Coupling between magnetic and optical properties of stable Au-Fe solid solution nanoparticles.

PubMed

de Julián Fernández, C; Mattei, G; Paz, E; Novak, R L; Cavigli, L; Bogani, L; Palomares, F J; Mazzoldi, P; Caneschi, A

2010-04-23

Au-Fe nanoparticles constitute one of the simplest prototypes of a multifunctional nanomaterial that can exhibit both magnetic and optical (plasmonic) properties. This solid solution, not feasible in the bulk phase diagram in thermal equilibrium, can be formed as a nanostructure by out-of-equilibrium processes. Here, the novel magnetic, optical and magneto-optical properties of ion-implanted Au-Fe solid solution nanoparticles dispersed in a SiO(2) matrix are investigated and correlated. The surface plasmon resonance of the Au-Fe nanoparticles with almost equicomposition is strongly damped when compared to pure Au and to Au-rich Au-Fe nanoparticles. In all cases, the Au atoms are magnetically polarized, as measured by x-ray magnetic circular dichroism, and ferromagnetically coupled with Fe atoms. Although the chemical stability of Au-Fe nanoparticles is larger than that of Fe nanoparticles, both the magnetic moment per Fe atom and the order temperature are smaller. These results suggest that electronic and magnetic properties are more influenced by the hybridization of the electronic bands in the Au-Fe solid solution than by size effects. On the other hand, the magneto-optical transitions allowed in the vis-nIR spectral regions are very similar. In addition, we also observe, after studying the properties of thermally treated samples, that the Au-Fe alloy is stabilized, not by surface effects, but by the combination of the out-of-equilibrium nature of the ion implantation technique and by changes in the properties due to size effects.

Enhancement of solubility and antidiabetic effects of Repaglinide using spray drying technique in STZ-induced diabetic rats.

PubMed

Varshosaz, Jaleh; Minayian, Mohsen; Ahmadi, Mahdieh; Ghassami, Erfaneh

2017-09-01

The purpose of the study was to enhance the solubility of the poorly water-soluble drug, Repaglinide using spray drying based solid dispersion technique by different carriers including Eudragit E100, hydroxyl propyl cellulose Mw 80 000 and poly vinyl pyrollidone K30. Optimization of the best formulation was carried out according to drug solubility, release profile, particle size and angle of repose of the solid dispersions. The optimized sample was characterized using X-ray powder diffraction (XRPD), differential scanning calorimetry (DSC) and Fourier transform infrared spectroscopy (FT-IR). The morphology of the dispersions was studied by SEM. The blood glucose lowering effect of spray dried solid dispersions was studied in normal and streptozocin-induced diabetic rats. The results showed that Eudragit E100 in 1:3 ratio could enhance drug solubility by 100-fold. DSC studies indicated a marked change in melting point of the drug possibly due to strong hydrogen bonds between the drug and Eudragit, while FT-IR study did not show obvious interactions between them. According to XRPD results Repaglinide converted to an amorphous state in the spray dried dispersions. Spray dried Repaglinide reduced the blood glucose level significantly during the 8 h of obtaining blood samples in comparison with untreated drug (p < 0.05).

Silica Modified with Polyaniline as a Potential Sorbent for Matrix Solid Phase Dispersion (MSPD) and Dispersive Solid Phase Extraction (d-SPE) of Plant Samples

PubMed Central

Sowa, Ireneusz; Wójciak-Kosior, Magdalena; Strzemski, Maciej; Sawicki, Jan; Staniak, Michał; Dresler, Sławomir; Szwerc, Wojciech; Mołdoch, Jarosław; Latalski, Michał

2018-01-01

Polyaniline (PANI) is one of the best known conductive polymers with multiple applications. Recently, it was also used in separation techniques, mostly as a component of composites for solid-phase microextraction (SPME). In the present paper, sorbent obtained by in situ polymerization of aniline directly on silica gel particles (Si-PANI) was used for dispersive solid phase extraction (d-SPE) and matrix solid–phase extraction (MSPD). The efficiency of both techniques was evaluated with the use of high performance liquid chromatography with diode array detection (HPLC-DAD) quantitative analysis. The quality of the sorbent was verified by Raman spectroscopy and microscopy combined with automated procedure using computer image analysis. For extraction experiments, triterpenes were chosen as model compounds. The optimal conditions were as follows: protonated Si-PANI impregnated with water, 160/1 sorbent/analyte ratio, 3 min of extraction time, 4 min of desorption time and methanolic solution of ammonia for elution of analytes. The proposed procedure was successfully used for pretreatment of plant samples. PMID:29565297

Supercritical antisolvent versus coevaporation: preparation and characterization of solid dispersions.

PubMed

Majerik, Viktor; Horváth, Géza; Szokonya, László; Charbit, Gérard; Badens, Elisabeth; Bosc, Nathalie; Teillaud, Eric

2007-09-01

The objective of this work was to improve the dissolution rate and aqueous solubility of oxeglitazar. Solid dispersions of oxeglitazar in PVP K17 (polyvinilpyrrolidone) and poloxamer 407 (polyoxyethylene-polyoxypropylene block copolymer) were prepared by supercritical antisolvent (SAS) and coevaporation (CoE) methods. Drug-carrier formulations were characterized by powder X-ray diffraction, Fourier transform infrared spectroscopy, scanning electron microscopy, gas chromatography, UV/VIS spectroscopy and in vitro dissolution tests. The highest dissolution rate (nearly 3-fold higher than raw drug) was achieved by preparation of drug/PVP K17 coevaporate. Oxeglitazar/PVP K17 solid dispersions were stabilized by hydrogen bonding but contained higher amount of residual dichloromethane (DCM) than poloxamer 407 formulations regardless of the method of preparation. SAS prepared oxeglitazar/poloxamer 407 dissolved more than two times faster than raw drug. However, unlike PVP K17, poloxamer 407 did not form a single phase amorphous solid solution with oxeglitazar which has been manifested in higher degrees of crystallinity, too. Among the two techniques, evaluated in this work, conventional coevaporation resulted in higher amorphous content but SAS reduced residual solvent content more efficiently.

Quick, easy, cheap, effective, rugged, and safe sample preparation approach for pesticide residue analysis using traditional detectors in chromatography: A review.

PubMed

Rahman, Md Musfiqur; Abd El-Aty, A M; Kim, Sung-Woo; Shin, Sung Chul; Shin, Ho-Chul; Shim, Jae-Han

2017-01-01

In pesticide residue analysis, relatively low-sensitivity traditional detectors, such as UV, diode array, electron-capture, flame photometric, and nitrogen-phosphorus detectors, have been used following classical sample preparation (liquid-liquid extraction and open glass column cleanup); however, the extraction method is laborious, time-consuming, and requires large volumes of toxic organic solvents. A quick, easy, cheap, effective, rugged, and safe method was introduced in 2003 and coupled with selective and sensitive mass detectors to overcome the aforementioned drawbacks. Compared to traditional detectors, mass spectrometers are still far more expensive and not available in most modestly equipped laboratories, owing to maintenance and cost-related issues. Even available, traditional detectors are still being used for analysis of residues in agricultural commodities. It is widely known that the quick, easy, cheap, effective, rugged, and safe method is incompatible with conventional detectors owing to matrix complexity and low sensitivity. Therefore, modifications using column/cartridge-based solid-phase extraction instead of dispersive solid-phase extraction for cleanup have been applied in most cases to compensate and enable the adaptation of the extraction method to conventional detectors. In gas chromatography, the matrix enhancement effect of some analytes has been observed, which lowers the limit of detection and, therefore, enables gas chromatography to be compatible with the quick, easy, cheap, effective, rugged, and safe extraction method. For liquid chromatography with a UV detector, a combination of column/cartridge-based solid-phase extraction and dispersive solid-phase extraction was found to reduce the matrix interference and increase the sensitivity. A suitable double-layer column/cartridge-based solid-phase extraction might be the perfect solution, instead of a time-consuming combination of column/cartridge-based solid-phase extraction and dispersive solid-phase extraction. Therefore, replacing dispersive solid-phase extraction with column/cartridge-based solid-phase extraction in the cleanup step can make the quick, easy, cheap, effective, rugged, and safe extraction method compatible with traditional detectors for more sensitive, effective, and green analysis. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Optimisation of powders for pulmonary delivery using supercritical fluid technology.

PubMed

Rehman, Mahboob; Shekunov, Boris Y; York, Peter; Lechuga-Ballesteros, David; Miller, Danforth P; Tan, Trixie; Colthorpe, Paul

2004-05-01

Supercritical fluid technology exploited in this work afforded single-step production of respirable particles of terbutaline sulphate (TBS). Different crystal forms of TBS were produced consistently, including two polymorphs, a stoichiometric monohydrate and amorphous material as well as particles with different degrees of crystallinity, size, and morphology. Different solid-state and surface characterisation techniques were applied in conjunction with measurements of powder flow properties using AeroFlow device and aerosol performance by Andersen Cascade Impactor tests. Improved fine particle fraction (FPF) was demonstrated for some powders produced by the SCF process when compared to the micronised material. Such enhanced flow properties and dispersion correlated well with the reduced surface energy parameters demonstrated by these powders. It is shown that semi-crystalline particles exhibited lower specific surface energy leading to a better performance in the powder flow and aerosol tests than crystalline materials. This difference of the surface and bulk crystal structure for selected powder batches is explained by the mechanism of precipitation in SCF which can lead to surface conditioning of particles produced.

Development of clinical dosage forms for a poorly water-soluble drug II: formulation and characterization of a novel solid microemulsion preconcentrate system for oral delivery of a poorly water-soluble drug.

PubMed

Li, Ping; Hynes, Sara R; Haefele, Thomas F; Pudipeddi, Madhu; Royce, Alan E; Serajuddin, Abu T M

2009-05-01

The solution of a poorly water-soluble drug in a liquid lipid-surfactant mixture, which served as a microemulsion preconcentrate, was converted into a solid form by incorporating it in a solid polyethylene glycol (PEG) matrix. The solid microemulsion preconcentrates thus formed consisted of Capmul PG8 (propylene glycol monocaprylate) as oil, Cremophor EL (polyoxyl 35 castor oil) as surfactant, and hydrophilic polymer PEG 3350 as solid matrix. The drug (aqueous solubility: 0.17 microg/mL at pH 1-8 and 25 degrees C) was dissolved in a melt of the mixture at 65-70 degrees C and then the hot solution was filled into hard gelatin capsules; the liquid gradually solidified upon cooling below 55 degrees C. The solid system was characterized by differential scanning calorimetry (DSC), scanning electron microscopy (SEM), confocal Raman microscopy (CRM), and the dispersion testing in water. It was confirmed that a solid microemulsion preconcentrate is a two-phase system, where clusters of crystalline PEG 3350 formed the solid structure (m.p. 55-60 degrees C) and the liquid microemulsion preconcentrate dispersed in between PEG 3350 crystals as a separate phase. The drug remained dissolved in the liquid phase. In vitro release testing showed that the preconcentrate dispersed readily in water forming a microemulsion with the drug dissolved in the oil particles (<150 nm) and the presence of PEG 3350 did not interfere with the process of self-microemulsification.

Trace determination of safranin O dye using ultrasound assisted dispersive solid-phase micro extraction: Artificial neural network-genetic algorithm and response surface methodology.

PubMed

Dil, Ebrahim Alipanahpour; Ghaedi, Mehrorang; Asfaram, Arash; Mehrabi, Fatemeh; Bazrafshan, Ali Akbar; Ghaedi, Abdol Mohammad

2016-11-01

In this study, ultrasound assisted dispersive solid-phase micro extraction combined with spectrophotometry (USA-DSPME-UV) method based on activated carbon modified with Fe2O3 nanoparticles (Fe2O3-NPs-AC) was developed for pre-concentration and determination of safranin O (SO). It is known that the efficiency of USA-DSPME-UV method may be affected by pH, amount of adsorbent, ultrasound time and eluent volume and the extent and magnitude of their contribution on response (in term of main and interaction part) was studied by using central composite design (CCD) and artificial neural network-genetic algorithms (ANN-GA). Accordingly by adjustment of experimental conditions suggested by ANN-GA at pH 6.5, 1.1mg of adsorbent, 10min ultrasound and 150μL of eluent volume led to achievement of best operation performance like low LOD (6.3ngmL(-1)) and LOQ (17.5ngmL(-1)) in the range of 25-3500ngmL(-1). In following stage, the SO content in real water and wastewater samples with recoveries between 93.27-99.41% with RSD lower than 3% was successfully determined. Copyright © 2016 Elsevier B.V. All rights reserved.

Minimum ignition temperature of nano and micro Ti powder clouds in the presence of inert nano TiO2 powder.

PubMed

Yuan, Chunmiao; Amyotte, Paul R; Hossain, Md Nur; Li, Chang

2014-06-30

Minimum ignition temperature (MIT) of micro Ti powder increased gradually with increases in nano-sized TiO2 employed as an inertant. Solid TiO2 inertant significantly reduced ignition hazard of micro Ti powder in contact with hot surfaces. The MIT of nano Ti powder remained low (583 K), however, even with 90% TiO2. The MIT of micro Ti powder, when mixed with nano Ti powder at concentrations as low as 10%, decreased so dramatically that its application as a solid fuel may be possible. A simple MIT model was proposed for aggregate particle size estimation and better understanding of the inerting effect of nano TiO2 on MIT. Estimated particle size was 1.46-1.51 μm larger than that in the 20-L sphere due to poor dispersion in the BAM oven. Calculated MITs were lower than corresponding empirically determined values for micro Ti powder because nano-sized TiO2 coated the micro Ti powder, thereby decreasing its reaction kinetics. In the case of nano Ti powder, nano-sized TiO2 facilitated dispersion of nano Ti powder which resulted in a calculated MIT that was greater than the experimentally determined value. Copyright © 2014 Elsevier B.V. All rights reserved.

Determination of wear metals in engine oil by mild acid digestion and energy dispersive X-ray fluorescence spectrometry using solid phase extraction disks.

PubMed

Yang, Zheng; Hou, Xiandeng; Jones, Bradley T

2003-03-10

A simple, particle size-independent spectrometric method has been developed for the multi-element determination of wear metals in used engine oil. A small aliquot (0.5 ml) of an acid-digested oil sample is spotted onto a C-18 solid phase extraction disk to form a uniform thin film. The dried disk is then analyzed directly by energy dispersive X-ray fluorescence spectrometry. This technique provides a homogeneous and reproducible sample surface to the instrument, thus overcoming the typical problems associated with uneven particle size distribution and sedimentation. As a result, the method provides higher precision and accuracy than conventional methods. Furthermore, the disk sample may be stored and re-analyzed or extracted at a later date. The signals arising from the spotted disks, and the calibration curves constructed from them, are stable for at least 2 months. The limits of detection for Fe, Cu, Zn, Pb, and Cr are 5, 1, 4, 2, and 4 microg g(-1), respectively. Recoveries of these elements from spiked oil samples range from 92 to 110%. The analysis of two standard reference materials and a used oil sample produced results comparable to those found by inductively coupled plasma atomic emission spectrometry.

Reversed phase HPLC analysis of stability and microstructural effects on degradation kinetics of β-carotene encapsulated in freeze-dried maltodextrin-emulsion systems.

PubMed

Harnkarnsujarit, Nathdanai; Charoenrein, Sanguansri; Roos, Yrjö H

2012-09-26

Degradation of dispersed lipophilic compounds in hydrophilic solids depends upon matrix stability and lipid physicochemical properties. This study investigated effects of solid microstructure and size of lipid droplets on the stability of dispersed β-carotene in freeze-dried systems. Emulsions of β-carotene in sunflower oil were dispersed in maltodextrin systems (M040/DE6, M100/DE11, and M250/DE25.5) (8% w/w oil) and prefrozen at various freezing conditions prior to freeze-drying to control nucleation and subsequent pore size and structural collapse of freeze-dried solids. The particle size, physical state, and β-carotene contents of freeze-dried emulsions were measured during storage at various water activity (a(w)) using a laser particle size analyzer, differential scanning calorimeter, and high performance liquid chromatography (HPLC), respectively. The results showed that M040 stabilized emulsions in low temperature freezing exhibited lipid crystallization. Collapse of solids in storage at a(w) which plasticized systems to the rubbery state led to flow and increased the size of oil droplets. Degradation of β-carotene analyzed using a reversed-phase C(30) column followed first-order kinetics. Porosity of solids had a major effect on β-carotene stability; however, the highest stability was found in fully plasticized and collapsed solids.

A new carbon-based magnetic material for the dispersive solid-phase extraction of UV filters from water samples before liquid chromatography-tandem mass spectrometry analysis.

PubMed

Piovesana, Susy; Capriotti, Anna Laura; Cavaliere, Chiara; La Barbera, Giorgia; Samperi, Roberto; Zenezini Chiozzi, Riccardo; Laganà, Aldo

2017-07-01

Magnetic solid-phase extraction is one of the most promising new extraction methods for liquid samples before ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) analysis. Several types of materials, including carbonaceous ones, have been prepared for this purpose. In this paper, for the first time, the preparation, characterization, and sorption capability of Fe 3 O 4 -graphitized carbon black (mGCB) composite toward some compounds of environmental interest were investigated. The synthesized mGCB consisted of micrometric GCB particles with 55 m 2  g -1 surface area bearing some carbonyl and hydroxyl functionalities and the surface partially decorated by Fe 3 O 4 microparticles. The prepared mGCB was firstly tested as an adsorbent for the extraction from surface water of 50 pollutants, including estrogens, perfluoroalkyl compounds, UV filters, and quinolones. The material showed good affinity to many of the tested compounds, except carboxylates and glucoronates; however, some compounds were difficult to desorb. Ten UV filters belonging to the chemical classes of benzophenones and p-aminobenzoates were selected, and parameters were optimized for the extraction of these compounds from surface water before UHPLC-MS/MS determination. Then, the method was validated in terms of linearity, trueness, intra-laboratory precision, and detection and quantification limits. In summary, the method performance (trueness, expressed as analytical recovery, 85-114%; RSD 5-15%) appears suitable for the determination of the selected compounds at the level of 10-100 ng L -1 , with detection limits in the range of 1-5 ng L -1 . Finally, the new method was compared with a published one, based on conventional solid-phase extraction with GCB, showing similar performance in real sample analysis. Graphical Abstract Workflow of the analytical method based on magnetic solid-phase extraction followed by LC-MS/MS determination.

NMR imaging and hydrodynamic analysis of neutrally buoyant non-Newtonian slurry flows

NASA Astrophysics Data System (ADS)

Bouillard, J. X.; Sinton, S. W.

The flow of solids loaded suspension in cylindrical pipes has been the object of intense experimental and theoretical investigations in recent years. These types of flows are of great interest in chemical engineering because of their important use in many industrial manufacturing processes. Such flows are for example encountered in the manufacture of solid-rocket propellants, advanced ceramics, reinforced polymer composites, in heterogeneous catalytic reactors, and in the pipeline transport of liquid-solids suspensions. In most cases, the suspension microstructure and the degree of solids dispersion greatly affect the final performance of the manufactured product. For example, solid propellant pellets need to be extremely-well dispersed in gel matrices for use as rocket engine solid fuels. The homogeneity of pellet dispersion is critical to allow good uniformity of the burn rate, which in turn affects the final mechanical performance of the engine. Today's manufacturing of such fuels uses continuous flow processes rather than batch processes. Unfortunately, the hydrodynamics of such flow processes is poorly understood and is difficult to assess because it requires the simultaneous measurements of liquid/solids phase velocities and volume fractions. Due to the recent development in pulsed Fourier Transform NMR imaging, NMR imaging is now becoming a powerful technique for the non intrusive investigation of multi-phase flows. This paper reports and exposes a state-of-the-art experimental and theoretical methodology that can be used to study such flows. The hydrodynamic model developed for this study is a two-phase flow shear thinning model with standard constitutive fluid/solids interphase drag and solids compaction stresses. this model shows good agreement with experimental data and the limitations of this model are discussed.

One-dimensional filtration of pharmaceutical grade phyllosilicate dispersions.

PubMed

Viseras, C; Cerezo, P; Meeten, G H; Lopez-Galindo, A

2001-04-17

The filtration behaviour of some clay-water dispersions was studied. Two Spanish fibrous phyllosilicates (sepiolite from Vicálvaro and palygorskite from Turón) and a commercial bentonite (Bentopharm UK) with similar sizes and different morphologies (fibrous and/or laminar) were selected as model clays. Sepiolite from Vicálvaro is an almost pure fibrous sample, Bentopharm presents a high amount of laminar particles and palygorskite from Turón is made up of similar percentages of laminar and fibrous particles. The disperse systems were made up using a rotor-stator mixer working at two different mixing rates (1000 and 8000 rpm), for periods of 1 and 10 min. Filtration measurements were taken and the corresponding filtration curves obtained. Finally, the desorptivity (S) of the filtration cakes was calculated and correlated to the textural characteristics of the materials, the solid fraction and mixing conditions. Filtration behaviour of the dispersions depended on all three of these factors. Laminar dispersions presented lower S values than fibrous dispersions. In the 2% w/v dispersions the bridging forces between particles did not permit formation of an interconnected network as in 10% w/v dispersions and, consequently, filtration times increased with the solid fraction (i.e. S values decreased). Regarding stability to pH changes, the results showed that filtration behaviour was highly sensitive to basic pH in the fibrous clay dispersions and almost insensitive in the laminar clay dispersions.

Additional boundary conditions and surface exciton dispersion relations

DOE Office of Scientific and Technical Information (OSTI.GOV)

Rimbey, P.R.

1977-01-15

The surface-exciton dispersion curves in ZnO are derived from the surface impedances developed by Fuchs and Kliewer (FK) and Rimbey and Mahan (RM) including retardation. There exists a distinctive splitting between the two dispersions, the FK additional boundary conditions having longitudinal character, the RM additional boundary conditions being transverse. Surface-mode attenuation due to spatial dispersion is more pronouced in the RM formalism, although inclusion of a phenomenological damping parameter does not alter either dispersion curve. (AIP)

Polymorphic transition of solid-fats dispersed systems — its characterization by a novel method and scanning electron microscopy observation

NASA Astrophysics Data System (ADS)

Hirokawa, Norio; Ueda, Masahiro; Harano, Yoshio

1994-08-01

Solid-fats dispersed systems, such as margarine, butter and cacao-butter, were characterized by a novel method based on liquid permeation under pressure, for the simultaneous measurement of a solid-content ɛ p and an average diameter dp of solid particles (fats crystals) in them. Further, micro-structures of these systems were observed by a scanning electron microscope (SEM). As the result, it has been clarified that the spherical fats crystals of several μm in size appeared in the initial solid-fats products are agglomerates of fine particles of ca. 0.1 μm and that these fine particles are uniformly redispersed during an annealing treatment accompanying the reduction of ɛ p and dp. It is strongly suggested that this phenomenon is caused by a transition of fat crystals into a more stable polymorph.

77 FR 16679 - Emergency Planning and Notification; Emergency Planning and List of Extremely Hazardous...

Federal Register 2010, 2011, 2012, 2013, 2014

2012-03-22

...The U.S. Environmental Protection Agency (EPA or the Agency) is taking final action to revise the manner for applying the threshold planning quantities (TPQs) for those extremely hazardous substances (EHSs) that are non-reactive solid chemicals in solution. This revision allows facilities subject to the Emergency Planning requirements that have a non-reactive solid EHS in solution, to first multiply the amount of the solid chemical in solution on-site by 0.2 before determining if this quantity equals or exceeds the lower published TPQ. This change is based on data that shows less potential for non-reactive solid chemicals in solution to remain airborne and dispersed beyond a facility's fence line in the event of an accidental release. Previously, EPA assumed that 100% of non-reactive solid chemicals in solution could become airborne and dispersed beyond the fenceline in the event of an accidental release.

Solid electrolytes strengthened by metal dispersions

DOEpatents

Lauf, Robert J.; Morgan, Chester S.

1983-01-01

An improvement in solid electrolytes of advanced secondary batteries of the sodium-sulfur, sodium-halogen, and like combinations is achieved by providing said battery with a cermet electrolyte containing a metal dispersion ranging from 0.1 to 10.0 vol. % of a substantially nonreactive metal selected from the group consisting essentially of Pt, Cr, Fe, Co, Ni, Nb, their alloys, and their physical mixtures in the elemental or uncombined state, the remainder of said cermet being an ion-conductive ceramic material.

Solid electrolytes strengthened by metal dispersions

DOEpatents

Lauf, R.J.; Morgan, C.S.

1981-10-05

An improvement in solid electrolytes of advanced secondary batteries of the sodium-sulfur, sodium-halogen, and like combinations is achieved by providing said battery with a cermet electrolyte containing a metal dispersion ranging from 0.1 to 10.0 vol. % of a substantially nonreactive metal selected from the group consisting essentially of Pt, Cr, Fe, Co, Ni, Nb, their alloys, and their physical mixtures in the elemental or uncombined state, the remainder of said cermet being an ion-conductive ceramic material.

Influence of solvent evaporation rate and formulation factors on solid dispersion physical stability.

PubMed

Wu, Jian X; Yang, Mingshi; Berg, Frans van den; Pajander, Jari; Rades, Thomas; Rantanen, Jukka

2011-12-18

New chemical entities (NCEs) often show poor water solubility necessitating solid dispersion formulation. The aim of the current study is to employ design of experiments in investigating the influence of one critical process factor (solvent evaporation rate) and two formulation factors (PVP:piroxicam ratio (PVP:PRX) and PVP molecular weight (P(MW))) on the physical stability of PRX solid dispersion prepared by the solvent evaporation method. The results showed the rank order of an increase in factors contributing to a decrease in the extent of PRX nucleation being evaporation rate>PVP:PRX>P(MW). The same rank order was found for the decrease in the extent of PRX crystal growth in PVP matrices from day 0 up to day 12. However, after 12days the rank became PVP:PRX>evaporation rate>P(MW). The effects of an increase in evaporation rate and PVP:PRX ratio in stabilizing PRX were of the same order of magnitude, while the effect from P(MW) was much smaller. The findings were confirmed by XRPD. FT-IR showed that PRX recrystallization in the PVP matrix followed Ostwald's step rule, and an increase in the three factors all led to increased hydrogen bonding interaction between PRX and PVP. The present study showed the applicability of the Quality by Design approach in solid dispersion research, and highlights the need for multifactorial analysis. Copyright © 2011 Elsevier B.V. All rights reserved.

Soluplus®/TPGS-based solid dispersions prepared by hot-melt extrusion equipped with twin-screw systems for enhancing oral bioavailability of valsartan.

PubMed

Lee, Jae-Young; Kang, Wie-Soo; Piao, Jingpei; Yoon, In-Soo; Kim, Dae-Duk; Cho, Hyun-Jong

2015-01-01

Soluplus(®) (SP) and D-alpha-tocopherol polyethylene glycol 1000 succinate (TPGS)-based solid dispersion (SD) formulations were developed by hot-melt extrusion (HME) to improve oral bioavailability of valsartan (VST). HME process with twin-screw configuration for generating a high shear stress was used to prepare VST SD formulations. The thermodynamic state of the drug and its dispersion in the polymers were evaluated by solid-state studies, including Fourier-transform infrared, X-ray diffraction, and differential scanning calorimetry. Drug release from the SD formulations was assessed at pH values of 1.2, 4.0, and 6.8. Pharmacokinetic study was performed in rats to estimate the oral absorption of VST. HME with a high shear rate produced by the twin-screw system was successfully applied to prepare VST-loaded SD formulations. Drug amorphization and its molecular dispersion in the polymer matrix were verified by several solid-state studies. Drug release from SD formulations was improved, compared to the pure drug, particularly at pH 6.8. Oral absorption of drug in rats was also enhanced in SP and TPGS-based SD groups compared to that in the pure drug group. SP and TPGS-based SDs, prepared by the HME process, could be used to improve aqueous solubility, dissolution, and oral absorption of poorly water-soluble drugs.

Improvement of solubility, dissolution and stability profile of artemether solid dispersions and self emulsified solid dispersions by solvent evaporation method.

PubMed

Tayyab Ansari, Muhammad; Arshad, Muhammad Sohail; Hussain, Altaf; Ahmad, Zeeshan

2016-12-08

The purpose of this study was to investigate changes in the water solubility of artemether; a poorly soluble drug used for the treatment of malaria. Different solid dispersions (SDs) of artemether were prepared using artemether and polyethylene glycol 6000 at ratio 12:88 (Group 1), self-emulsified solid dispersions (SESDs) containing artemether, polyethylene glycol 6000, cremophor-A-25, olive oil, hydroxypropylmethylcellulose and transcutol in the ratio 12:75:5:4:2:2, respectively (Group 2). SESDs were also prepared by substituting cremophor-A-25 in Group 2 with poloxamer 188 (noted as Group 3). Each of these preparations was formulated using physical mixing and the solvent evaporation method. Aqueous solubility of artemether improved 11-, 95- and 102-fold, while dissolution (in simulated gastric fluid) increased 3-, 13- and 14-fold, for formulation groups 1, 2 and 3, respectively. X-ray diffraction patterns of SDs indicated a decrease in peak intensities at 10° implying reduced artemether crystallinity. Scanning electron micrographs invariably revealed embedment of artemether by various excipients and a glassy appearance for solvent evaporated mixtures for all three formulation Groups. Our findings indicate improved hydrophilic interactions for drug particles yield greater solubility and dissolution in the following order for artemether formulating methods: solvent evaporation mixtures > physical mixtures > pure artemether.

Trace determination of five triazole fungicide residues in traditional Chinese medicine samples by dispersive solid-phase extraction combined with ultrasound-assisted dispersive liquid-liquid microextraction and UHPLC-MS/MS.

PubMed

Ma, Shuping; Yuan, Xucan; Zhao, Pengfei; Sun, Hong; Ye, Xiu; Liang, Ning; Zhao, Longshan

2017-08-01

A novel and reliable method for determination of five triazole fungicide residues (triadimenol, tebuconazole, diniconazole, flutriafol, and hexaconazol) in traditional Chinese medicine samples was developed using dispersive solid-phase extraction combined with ultrasound-assisted dispersive liquid-liquid microextraction before ultra-high performance liquid chromatography with tandem mass spectrometry. The clean up of the extract was conducted using dispersive solid-phase extraction by directly adding sorbents into the extraction solution, followed by shaking and centrifugation. After that, a mixture of 400 μL trichloromethane (extraction solvent) and 0.5 mL of the above supernatant was injected rapidly into water for the dispersive liquid-liquid microextraction procedure. The factors affecting the extraction efficiency were optimized. Under the optimum conditions, the calibration curves showed good linearity in the range of 2.0-400 (tebuconazole, diniconazole, and hexaconazole) and 4.0-800 ng/g (triadimenol and flutriafol) with the regression coefficients higher than 0.9958. The limit of detection and limit of quantification for the present method were 0.5-1.1 and 1.8-4.0 ng/g, respectively. The recoveries of the target analytes ranged from 80.2 to 103.2%. The proposed method has been successfully applied to the analysis of five triazole fungicides in traditional Chinese medicine samples, and satisfactory results were obtained. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Synthesis and application of mesoporous molecular sieve for miniaturized matrix solid-phase dispersion extraction of bioactive flavonoids from toothpaste, plant, and saliva.

PubMed

Cao, Wan; Cao, Jun; Ye, Li-Hong; Xu, Jing-Jing; Hu, Shuai-Shuai; Peng, Li-Qing

2015-12-01

This article describes the use of the mesoporous molecular sieve KIT-6 as a sorbent in miniaturized matrix solid-phase dispersion (MSPD) in combination with ultra-performance LC for the determination of bioactive flavonoids in toothpaste, Scutellariae Radix, and saliva. In this study, for the first time, KIT-6 was used as a sorbent material for this mode of extraction. Compared with common silica-based sorbents (C18 and activated silica gel), the proposed KIT-6 dispersant with a three-dimensional cubic Ia3d structure and highly ordered arrays of mesoporous channels exhibits excellent adsorption capability of the tested compounds. In addition, several experimental variables, such as the mass ratio of sample to dispersant, grinding time, and elution solvent, were optimized to maximize the extraction efficiency. The proposed analytical method is simple, fast, and entails low consumption of samples, dispersants and elution solvents, thereby meeting "green chemistry" requirements. Under the optimized conditions, the recoveries of three bioactive flavonoids obtained by analyzing the spiked samples were from 89.22 to 101.17%. Also, the LODs and LOQs for determining the analytes were in the range of 0.02-0.04 μg/mL and 0.07-0.13 μg/mL, respectively. Finally, the miniaturized matrix solid-phase dispersion method was successfully applied to the analysis of target solutes in real samples, and satisfactory results were obtained. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Water-mediated solid-state transformation of a polymorphic drug during aqueous-based drug-layer coating of pellets.

PubMed

Lust, Andres; Lakio, Satu; Vintsevits, Julia; Kozlova, Jekaterina; Veski, Peep; Heinämäki, Jyrki; Kogermann, Karin

2013-11-01

During aqueous drug-layer coating, drug substance(s) are exposed to water and elevated temperatures which can lead to water-mediated process induced transformations (PITs). The effects of aqueous drug-layer coating of pellets (Cellets(®)) on the anhydrous piroxicam, PRX, were investigated in the miniaturized coating equipment and with free films. Hydroxypropyl methylcellulose (HPMC) was used as a carrier coating polymer. Free films were prepared by using an in-house small-scale rotating plate system equipped with an atomization air nozzle. Raman spectroscopy, X-ray powder diffraction (XRPD), differential scanning calorimetry (DSC), and scanning electron microscopy (SEM) were used to characterize the solid-state properties and surface morphology of the pellets and free films. The results showed that anhydrous PRX form I (AH) and monohydrate (MH) were stable during drug-layer coating, but amorphous PRX in solid dispersion (SD) crystallized as MH already after 10 min of coating. Furthermore, the increase in a dissolution rate was achieved from the drug-layer coated inert pellets compared to powder forms. In conclusion, water-mediated solid-state PITs of amorphous PRX is evident during aqueous-based drug-layer coating of pellets, and solid-state change can be verified using Raman spectroscopy. Copyright © 2013 Elsevier B.V. All rights reserved.

Structure analysis of aqueous ferrofluids at interface with silicon: neutron reflectometry data

NASA Astrophysics Data System (ADS)

Gapon, I. V.; Petrenko, V. I.; Bulavin, L. A.; Balasoiu, M.; Kubovcikova, M.; Zavisova, V.; Koneracka, M.; Kopcansky, P.; Chiriac, H.; Avdeev, M. V.

2017-05-01

Adsorption of nanoparticles from aqueous ferrofluids (FFs) on solid surface (crystalline silicon) was studied by neutron reflectometry (NR). Two kinds of FFs were considered. First kind was heavy water-based ferrofluids with magnetite nanoparticles coated by double layer of sodium oleate. Second one FF was cobalt ferrite nanoparticles stabilized by lauric acid/sodium n-dodecylsulphate layer and dispersed in water. It was obtained only a single adsorption layer for two types of ferrofluids. The impact of the magnetic nanoparticles concentration and geometry was considered in frame of the adsorption characteristic of FFs.

Graphene/activated carbon supercapacitors with sulfonated-polyetheretherketone as solid-state electrolyte and multifunctional binder

NASA Astrophysics Data System (ADS)

Chen, Y.-R.; Chiu, K.-F.; Lin, H. C.; Chen, C.-L.; Hsieh, C. Y.; Tsai, C. B.; Chu, B. T. T.

2014-11-01

Sulfonated polyetheretherketone (SPEEK) has been synthesised by sulphonation process and used as the solid-state electrolyte, binder and surfactant for supercapacitors. Reduced graphene dispersed by SPEEK is used as a high-efficiency conducting additive in solid-state supercapacitors. It is found that SPEEK can improve the stability of the reduced graphene dispersion significantly, and therefore, the solid-state supercapacitors show a large decrease in IR drop and charge-transfer resistance (Rct), resulting in a higher rate capability. The solid-state supercapacitors with the activated carbon/reduced graphene/SPEEK/electrode can be operated from 1 to 8 A/g and exhibit capacity retention of 93%. The noteworthy is more than twice higher value for capacity retention by comparison with the solid-state supercapacitors using activated carbon/reduced graphene/PVDF electrode (capacity retention is 36%). The cell of reduced graphene with SPEEK can be cycled over 5000 times at 5 A/g with no capacitance fading.

High basicity adsorbents from solid residue of cellulose and synthetic polymer co-pyrolysis for phenol removal: Kinetics and mechanism

NASA Astrophysics Data System (ADS)

Lorenc-Grabowska, Ewa; Rutkowski, Piotr

2014-10-01

The activated carbons (ACs) produced from solid residue of cellulose and synthetic polymer co-pyrolysis (CACs) and commercial activated carbon from coconut shell (GC) were used for phenol removal. The adsorption kinetics and mechanism were investigated. All studied activated carbons are predominantly microporous and are characterized by basic surface characteristics. Surface area SBET varies between 1235 and 1499 m2/g, whereas the pHPZC changes from 7.70 to 10.63. The bath adsorption of phenol (P) was carried out at ambient temperature. The equilibrium time and equilibrium sorption capacity were determined. It was found that the boundary layer effect is bigger in AC with high basic characteristics of the surface. The rate controlling step is the intraparticle diffusion in CACs only, whereas in ACs with higher amount of acidic functionalities the adsorbate-surface interaction influences the rate of kinetic as well. The equilibrium isotherms are L2 type for commercial AC and L4 for CACs. The CACs are characterized by very high adsorption capacity that vary between 312 and 417 mg/g. The main mechanism of phenol adsorption is micropore filling within pores smaller than 1.4 nm. In the absence of solvent effect further adsorption of phenol on CACs takes place. The enhanced adsorption is due to dispersive/repulsive interaction induced by oxygen functionalities.

Evaporation control research, 1959-60

USGS Publications Warehouse

,

1963-01-01

Two hundred and forty-five dispersions of long-chain alkanols were formulated by using various emulsifiers and alkanols. The dispensing and spreading ability of each of these formulations was tested. The most promising emulsifier that could be used with any of the alkanols was glyceryl monostearate (self-emulsifying). However, the concentration of the alkanol in the dispersion form varied somewhat: with the length of the carbon chain. A maximum concentration of 16 percent was obtained using the longer chain alkanols in the dispersion form without losing any of the properties of a fluid. Nine field tests were undertaken on small stock tanks. The retardant materials used in these tests were dodecanol, hexadecanol, and octadecanol. These materials were applied in either liquid or dispersion form. Four types of dispensing equipment were tested. The first type used a pressure system which sprayed a liquid onto the surface of the water. An anemometer and wind-controlled vane, operated by an electrical system, determined the length End frequency of application. The second type was similar to the first except that gravity was utilized to force the liquid onto the surface. The third type. used a drip system with rates of about 10 drops per minute. The fourth type used a gravity feed and a wind-controlled valve which allowed the dispersion material to flow onto the surface of the water when the wind was in the proper direction. In the field tests, the best reduction in evaporation was obtained using octadecanol in dispersion form and dispensed with the wind-controlled valve and gravity feed system. The maximum reduction in evaporation for a 2-week period was 27 percent. However, the economics of suppressing evaporation from stock tanks is questionable because of the short travel time across the tank by the film. There are still many problems unsolved. Some of these can be resolved in the laboratory whereas others can be resolved only in the field. Some of the more serious problems are the effect of impurities in the alkanols; the rate of cooling of the alkanol from a liquid to a solid state ; the effect of the film on the exchange of water molecules between the air and water; whether the film remains effective in suppressing evaporation for any rate of movement downwind; and the possible use of dodecanol and eicosanol as suppressants.

The effect of the London-van der Waals dispersion force on interline heat transfer

NASA Technical Reports Server (NTRS)

Wayner, P. C., Jr.

1978-01-01

A theoretical procedure to determine the heat transfer characteristics of the interline region (junction of liquid-solid-vapor) from the macroscopic optical and thermophysical properties of the system is outlined. The analysis is based on the premise that the interline transport processes are controlled by the London-van der Waals dispersion force between condensed phases (solid and liquid). Numerical values of the dispersion constant are presented. The procedure is used to compare the relative size of the interline heat sink of various systems using a constant heat flux mode. This solution demonstrates the importance of the interline heat flow number, which is evaluated for various systems.

Application of microdynamics and lattice mechanics to problems in plastic flow and fracture. Final report, 1 April 1973--31 March 1978

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bilello, J C; Liu, J M

Progress in an investigation of the application of microdynamics and lattice mechanics to the problems in plastic flow and fracture is described. The research program consisted of both theoretical formulations and experimental measurements of a number of intrinsic material parameters in bcc metals and alloys including surface energy, phonon-dispersion curves for dislocated solids, dislocation-point defect interaction energy, slip initiation and microplastic flow behavior. The study has resulted in an improved understanding in the relationship among the experimentally determined fracture surface energy, the intrinsic cohesive energy between atomic planes, and the plastic deformation associated with the initial stages of crack propagation.more » The values of intrinsic surface energy of tungsten, molybdenum, niobium and niobium-molybdenum alloys, deduced from the measurements, serve as a starting point from which fracture toughness of these materials in engineering service may be intelligently discussed.« less

Understanding the generation and maintenance of supersaturation during the dissolution of amorphous solid dispersions using modulated DSC and 1H NMR.

PubMed

Baghel, Shrawan; Cathcart, Helen; O'Reilly, Niall J

2018-01-30

In this study, the dissolution behaviour of dipyridamole (DPM) and cinnarizine (CNZ) spray-dried amorphous solid dispersions (ASDs) using polyvinyl pyrrolidone (PVP) and polyacrylic acid (PAA) as a carrier matrix were evaluated and compared. The drug concentrations achieved from the dissolution of PVP and PAA solid dispersions were significantly greater than the equilibrium solubility of crystalline DPM and CNZ in phosphate buffer pH 6.8 (PBS 6.8). The maximum drug concentration achieved by dissolution of PVP and PAA solid dispersions did not exceed the theoretically calculated apparent solubility of amorphous DPM and CNZ. However, the degree of supersaturation of DPM and CNZ increased considerably as the polymer weight fraction within the solid dispersion increased. In addition, the supersaturation profile of DPM and CNZ were studied in the presence and absence of the polymers. PAA was found to maintain a higher level of supersaturation compared to PVP. The enhanced drug solution concentration following dissolution of ASDs can be attributed to the reduced crystal growth rates of DPM and CNZ at an equivalent supersaturation. We have also shown that, for drugs having high crystallization tendency and weak drug-polymer interaction, the feasible way to increase dissolution might be increase the polymer weight fraction in the ASD. Solution 1 H NMR spectra were used to understand dissolution mechanism and to identify drug-polymer interaction. The change in electron densities of proton attached to different groups in DPM and CNZ suggested drug-polymer interaction in solution. The relative intensities of peak shift and nature of interaction between drug and polymer in different systems are different. These different effects suggest that DPM and CNZ interacts in a different way with PVP and PAA in solution which goes some way towards explaining the different polymeric effect, particularly in terms of inhibition of drug recrystallization and dissolution of DPM and CNZ ASDs. These results established that the different drug/polymer interactions in the solid state and in solution give rise to the variation in dissolution profile observed for different systems. Copyright © 2017 Elsevier B.V. All rights reserved.

High temperature regenerative H.sub.2 S sorbents

NASA Technical Reports Server (NTRS)

Flytani-Stephanopoulos, Maria (Inventor); Gavalas, George R. (Inventor); Tamhankar, Satish S. (Inventor)

1988-01-01

Efficient, regenerable sorbents for removal of H.sub.2 S from high temperature gas streams comprise porous, high surface area particles. A first class of sorbents comprise a thin film of binary oxides that form a eutectic at the temperature of the gas stream coated onto a porous, high surface area refractory support. The binary oxides are a mixture of a Group VB or VIB metal oxide with a Group IB, IIB or VIII metal oxide such as a film of V-Zn-O, V-Cu-O, Cu-Mo-O, Zn-Mo-O or Fe-Mo-O coated on an alumina support. A second class of sorbents consist of particles of unsupported mixed oxides in the form of highly dispersed solid solutions of solid compounds characterized by small crystallite size, high porosity and relatively high surface area. The mixed oxide sorbents contain one Group IB, IIB or VIIB metal oxide such as copper, zinc or manganese and one or more oxides of Groups IIIA, VIB or VII such as aluminum, iron or molybdenum. The presence of iron or aluminum maintains the Group IB, IIB or VIIB metal in its oxidized state. Presence of molybdenum results in eutectic formation at sulfidation temperature and improves the efficiency of the sorbent.

Carbon nanotubes as adsorbent of solid-phase extraction and matrix for laser desorption/ionization mass spectrometry.

PubMed

Pan, Chensong; Xu, Songyun; Zou, Hanfa; Guo, Zhong; Zhang, Yu; Guo, Baochuan

2005-02-01

A method with carbon nanotubes functioning both as the adsorbent of solid-phase extraction (SPE) and the matrix for matrix assisted laser desorption/ionization mass spectrometry (MALDI-MS) to analyze small molecules in solution has been developed. In this method, 10 microL suspensions of carbon nanotubes in 50% (vol/vol) methanol were added to the sample solution to extract analytes onto surface of carbon nanotubes because of their dramatic hydrophobicity. Carbon nanotubes in solution are deposited onto the bottom of tube with centrifugation. After removing the supernatant fluid, carbon nanotubes are suspended again with dispersant and pipetted directly onto the sample target of the MALDI-MS to perform a mass spectrometric analysis. It was demonstrated by analysis of a variety of small molecules that the resolution of peaks and the efficiency of desorption/ionization on the carbon nanotubes are better than those on the activated carbon. It is found that with the addition of glycerol and sucrose to the dispersant, the intensity, the ratio of signal to noise (S/N), and the resolution of peaks for analytes by mass spectrometry increased greatly. Compared with the previously reported method by depositing sample solution onto thin layer of carbon nanotubes, it is observed that the detection limit for analytes can be enhanced about 10 to 100 times due to solid-phase extraction of analytes in solution by carbon nanotubes. An acceptable result of simultaneously quantitative analysis of three analytes in solution has been achieved. The application in determining drugs spiked into urine has also been realized.

Nanostructured Coatings of Inner Surfaces in Microporous Matrixes

DTIC Science & Technology

2000-01-01

SURFACE ENERGY _.I", DISPERSED MATERIAL............................ ,BULK MATERIp,’ t. i02 10’ iol LM Figure 1. a) Surface arising due to process of...material dispersion . b) Surface energy per cm3 of dispersed material versus characteristic size of dispersed particles - nanostructures with different...growth and lateral microstructuring techniques have made it possible to realise low-dimensional electronic systems with quantum confined energy structure

Trace analysis of surfactants in Corexit oil dispersant formulations and seawater

NASA Astrophysics Data System (ADS)

Place, Benjamin J.; Perkins, Matt J.; Sinclair, Ewan; Barsamian, Adam L.; Blakemore, Paul R.; Field, Jennifer A.

2016-07-01

After the April 2010 explosion on the Deepwater Horizon oil rig, and subsequent release of millions of barrels of oil, two Corexit oil dispersant formulations were used in unprecedented quantities both on the surface and sub-surface of the Gulf of Mexico. Although the dispersant formulations contain four classes of surfactants, current studies to date focus on the anionic surfactant, bis-(2-ethylhexyl) sulfosuccinate (DOSS). Factors affecting the integrity of environmental and laboratory samples for Corexit analysis have not been systematically investigated. For this reason, a quantitative analytical method was developed for the detection of all four classes of surfactants, as well as the hydrolysis products of DOSS, the enantiomeric mixture of α- and β-ethylhexyl sulfosuccinate (α-/β-EHSS). The analytical method was then used to evaluate which practices for sample collection, storage, and analysis resulted in high quality data. Large volume, direct injection of seawater followed by liquid chromatography tandem mass spectrometry (LC-MS/MS) minimized analytical artifacts, analysis time, and both chemical and solid waste. Concentrations of DOSS in the seawater samples ranged from 71 to 13,000 ng/L, while the nonionic surfactants including Span 80, Tween 80, Tween 85 were detected infrequently (26% of samples) at concentrations from 840 to 9100 ng/L. The enantiomers α-/β-EHSS were detected in seawater, at concentrations from 200 to 1900 ng/L, and in both Corexit dispersant formulations, indicating α-/β-EHSS were applied to the oil spill and may be not unambiguous indicator of DOSS degradation. Best practices are provided to ensure sample integrity and data quality for environmental monitoring studies and laboratory that require the detection and quantification of Corexit-based surfactants in seawater.

Chacterization of Teleseismic Earthquakes Observed on an Ice Shelf

NASA Astrophysics Data System (ADS)

Baker, M. G.; Aster, R. C.; Anthony, R. E.; Wiens, D.; Nyblade, A.; Bromirski, P. D.; Stephen, R. A.; Gerstoft, P.

2016-12-01

Broadband seismographs deployed atop large tabular icebergs and ice shelves record a rich superposition of atmospheric, oceanic, and solid earth signals. We characterize these signals, including body and surface wave arrivals from approximately 200 global earthquakes, using a 34-station broadband array spanning the Ross Ice Shelf, Antarctica. Teleseismic earthquake arrivals are essential for constructing models of crustal and upper mantle structure, and observations on the ice shelf are key to resolving the structure of the underlying West Antarctic Rift System. To test the plausibility of passive imaging in this unique environment, we examine seasonal and spatial dependence of signal-to-noise ratios of body wave arrivals and the impact of ice shelf dynamics on surface wave dispersion. We also note unusual phase mechanics arising from the floating platform geometry.

The role of biomineralization in microbiologically influenced corrosion

NASA Technical Reports Server (NTRS)

Little, B.; Wagner, P.; Hart, K.; Ray, R.; Lavoie, D.; Nealson, K.; Aguilar, C.

1998-01-01

Synthetic iron oxides (goethite, alpha-FeO.OH; hematite, Fe2O3; and ferrihydrite, Fe(OH)3) were used as model compounds to simulate the mineralogy of surface films on carbon steel. Dissolution of these oxides exposed to pure cultures of the metal-reducing bacterium, Shewanella putrefaciens, was followed by direct atomic absorption spectroscopy measurement of ferrous iron coupled with microscopic analyses using confocal laser scanning and environmental scanning electron microscopies. During an 8-day exposure the organism colonized mineral surfaces and reduced solid ferric oxides to soluble ferrous ions. Elemental composition, as monitored by energy dispersive x-ray spectroscopy, indicated mineral replacement reactions with both ferrihydrite and goethite as iron reduction occurred. When carbon steel electrodes were exposed to S. putrefaciens, microbiologically influenced corrosion was demonstrated electrochemically and microscopically.

Interfacial Force Field Characterization in a Constrained Vapor Bubble Thermosyphon

NASA Technical Reports Server (NTRS)

DasGupta, Sunando; Plawsky, Joel L.; Wayner, Peter C., Jr.

1995-01-01

Isothermal profiles of the extended meniscus in a quartz cuvette were measured in the earth's gravitational field using an image-analyzing interferometer that is based on computer-enhanced video microscopy of the naturally occurring interference fringes. These profiles are a function of the stress field. Experimentally, the augmented Young-Laplace equation is an excellent model for the force field at the solid-liquid-vapor interfaces for heptane and pentane menisci on quartz and tetradecane on SFL6. The effects of refractive indices of the solid and liquid on the measurement techniques were demonstrated. Experimentally obtained values of the disjoining pressure and dispersion constants were compared to those predicted from the Dzyaloshinskii - Lifshitz - Pilaevskii theory for an ideal surface and reasonable agreements were obtained. A parameter introduced gives a quantitative measurement of the closeness of the system to equilibrium. The nonequilibrium behavior of this parameter is also presented

Dissolution enhancement of a drug exhibiting thermal and acidic decomposition characteristics by fusion processing: a comparative study of hot melt extrusion and KinetiSol dispersing.

PubMed

Hughey, Justin R; DiNunzio, James C; Bennett, Ryan C; Brough, Chris; Miller, Dave A; Ma, Hua; Williams, Robert O; McGinity, James W

2010-06-01

In this study, hot melt extrusion (HME) and KinetiSol Dispersing (KSD) were utilized to prepare dissolution-enhanced solid dispersions of Roche Research Compound A (ROA), a BCS class II drug. Preformulation characterization studies showed that ROA was chemically unstable at elevated temperatures and acidic pH values. Eudragit L100-55 and AQOAT LF (HPMCAS) were evaluated as carrier polymers. Dispersions were characterized for ROA recovery, crystallinity, homogeneity, and non-sink dissolution. Eudragit L100-55 dispersions prepared by HME required the use of micronized ROA and reduced residence times in order to become substantially amorphous. Compositions containing HPMCAS were also prepared by HME, but an amorphous dispersion could not be obtained. All HME compositions contained ROA-related impurities. KSD was investigated as a method to reduce the decomposition of ROA while rendering compositions amorphous. Substantially amorphous, plasticizer free compositions were processed successfully by KSD with significantly higher ROA recovery values and amorphous character than those achieved by HME. A near-infrared chemical imaging analysis was conducted on the solid dispersions as a measure of homogeneity. A statistical analysis showed similar levels of homogeneity in compositions containing Eudragit L100-55, while differences were observed in those containing HMPCAS. Non-sink dissolution analysis of all compositions showed rapid supersaturation after pH adjustment to approximately two to three times the equilibrium solubility of ROA, which was maintained for at least 24 h. The results of the study demonstrated that KSD is an effective method of forming dissolution-enhanced amorphous solid solutions in cases where HME is not a feasible technique.

Improved intestinal absorption of a poorly water-soluble oral drug using mannitol microparticles containing a nanosolid drug dispersion.

PubMed

Nishino, Yukiko; Kubota, Aya; Kanazawa, Takanori; Takashima, Yuuki; Ozeki, Tetsuya; Okada, Hiroaki

2012-11-01

A nozzle for a spray dryer that can prepare microparticles of water-soluble carriers containing various nanoparticles in a single step was previously developed in our laboratory. To enhance the solubility and intestinal absorption of poorly water-soluble drugs, we used probucol (PBL) as a poorly water-soluble drug, mannitol (MAN) as a water-soluble carrier for the microparticles, and EUDRAGIT (EUD) as a polymer vehicle for the solid dispersion. PBL-EUD-acetone-methanol and aqueous MAN solutions were simultaneously supplied through different liquid passages of the spray nozzle and dried together. PBL-EUD solid dispersion was nanoprecipitated in the MAN solution using an antisolvent mechanism and rapidly dried by surrounding it with MAN. PBL in the dispersion vehicle was amorphous and had higher physical stability according to powder X-ray diffraction and differential scanning calorimetry analysis. The bioavailability of PBL in PBL-EUD S-100-MAN microparticles after oral administration in rats was markedly higher (14- and 6.2-fold, respectively) than that of the original PBL powder and PBL-MAN microparticles. These results demonstrate that the composite microparticles containing a nanosized solid dispersion of a poorly water-soluble drug prepared using the spray nozzle developed by us should be useful to increase the solubility and bioavailability of drugs after oral administration. Copyright © 2012 Wiley Periodicals, Inc.

Ionic-liquid-based dispersive liquid-liquid microextraction combined with magnetic solid-phase extraction for the determination of aflatoxins B1 , B2 , G1 , and G2 in animal feeds by high-performance liquid chromatography with fluorescence detection.

PubMed

Zhao, Jiao; Zhu, Yan; Jiao, Yang; Ning, Jinyan; Yang, Yaling

2016-10-01

A novel two-step extraction technique combining ionic-liquid-based dispersive liquid-liquid microextraction with magnetic solid-phase extraction was developed for the preconcentration and separation of aflatoxins in animal feedstuffs before high-performance liquid chromatography coupled with fluorescence detection. In this work, ionic liquid 1-octyl-3-methylimidazolium hexafluorophosphate was used as the extractant in dispersive liquid-liquid microextraction, and hydrophobic pelargonic acid modified Fe 3 O 4 magnetic nanoparticles as an efficient adsorbent were applied to retrieve the aflatoxins-containing ionic liquid. Notably, the target of magnetic nanoparticles was the ionic liquid rather than the aflatoxins. Because of the rapid mass transfer associated with the dispersive liquid-liquid microextraction and magnetic solid phase steps, fast extraction could be achieved. The main parameters affecting the extraction recoveries of aflatoxins were investigated and optimized. Under the optimum conditions, vortexing at 2500 rpm for 1 min in the dispersive liquid-liquid microextraction and magnetic solid-phase extraction and then desorption by sonication for 2 min with acetonitrile as eluent. The recoveries were 90.3-103.7% with relative standard deviations of 3.2-6.4%. Good linearity was observed with correlation coefficients ranged from 0.9986 to 0.9995. The detection limits were 0.632, 0.087, 0.422 and 0.146 ng/mL for aflatoxins B 1 , B2, G1, and G2, respectively. The results were also compared with the pretreatment method carried out by conventional immunoaffinity columns. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Increased physical stability and improved dissolution properties of itraconazole, a class II drug, by solid dispersions that combine fast- and slow-dissolving polymers.

PubMed

Six, Karel; Verreck, Geert; Peeters, Jef; Brewster, Marcus; Van Den Mooter, Guy

2004-01-01

Solid dispersions were prepared of itraconazole-Eudragit E100, itraconazole-PVPVA64, and itraconazole-Eudragit E100/PVPVA64 using a corotating twin-screw hot-stage extruder. Modulated temperature differential scanning calorimetry (MTDSC) was used to evaluate the miscibility of the extrudates, and dissolution experiments were performed in simulated gastric fluid without pepsin (SGF(sp)). Itraconazole and Eudragit E100 are miscible up to 13% w/w drug loading. From that concentration on, phase separation is observed. Pharmaceutical performance of this dispersion was satisfactory because 80% of the drug dissolved after 30 min. Extrudates of itraconazole and PVPVA64 were completely miscible but the pharmaceutical performance was low, with 45% of drug dissolved after 3 h. Combination of both polymers in different ratios, with a fixed drug loading of 40% w/w, was evaluated. MTDSC results clearly indicated a two-phase system consisting of itraconazole-Eudragit E100 and itraconazole-PVPVA64 phases. In these extrudates, no free crystalline or glassy clusters of itraconazole were observed; all itraconazole was mixed with one of both polymers. The pharmaceutical performance was tested in SGF(sp) for different polymer ratios, and Eudragit E100/PVPVA64 ratios of 50/50 and 60/40 showed significant increases in dissolution rate and level. Polymer ratios of 70/30 and 80/20, on the other hand, had a release of 85% after 30 min. Precipitation of the drug was never observed. The combination of the two polymers provides a solid dispersion with good dissolution properties and improved physical stability compared with the binary solid dispersions of itraconazole. Copyright 2004 Wiley-Liss, Inc.

40 CFR Appendix E to Subpart E of... - Interim Method of the Determination of Asbestos in Bulk Insulation Samples

Code of Federal Regulations, 2014 CFR

2014-07-01

... characteristics of anisotropic particles. Quantitative analysis involves the use of point counting. Point counting... 0.004. • Refractive Index Liquids for Dispersion Staining: high-dispersion series, 1.550, 1.605, 1... hand. Repeat the series. Collect the dispersed solids by centrifugation at 1000 rpm for 5 minutes. Wash...

40 CFR Appendix E to Subpart E of... - Interim Method of the Determination of Asbestos in Bulk Insulation Samples

Code of Federal Regulations, 2010 CFR

2010-07-01

... characteristics of anisotropic particles. Quantitative analysis involves the use of point counting. Point counting... 0.004. • Refractive Index Liquids for Dispersion Staining: high-dispersion series, 1.550, 1.605, 1... hand. Repeat the series. Collect the dispersed solids by centrifugation at 1000 rpm for 5 minutes. Wash...

40 CFR Appendix E to Subpart E of... - Interim Method of the Determination of Asbestos in Bulk Insulation Samples

Code of Federal Regulations, 2011 CFR

2011-07-01

... characteristics of anisotropic particles. Quantitative analysis involves the use of point counting. Point counting... 0.004. • Refractive Index Liquids for Dispersion Staining: high-dispersion series, 1.550, 1.605, 1... hand. Repeat the series. Collect the dispersed solids by centrifugation at 1000 rpm for 5 minutes. Wash...

40 CFR Appendix E to Subpart E of... - Interim Method of the Determination of Asbestos in Bulk Insulation Samples

Code of Federal Regulations, 2012 CFR

2012-07-01

... characteristics of anisotropic particles. Quantitative analysis involves the use of point counting. Point counting... 0.004. • Refractive Index Liquids for Dispersion Staining: high-dispersion series, 1.550, 1.605, 1... hand. Repeat the series. Collect the dispersed solids by centrifugation at 1000 rpm for 5 minutes. Wash...

40 CFR Appendix E to Subpart E of... - Interim Method of the Determination of Asbestos in Bulk Insulation Samples

Code of Federal Regulations, 2013 CFR

2013-07-01

... characteristics of anisotropic particles. Quantitative analysis involves the use of point counting. Point counting... 0.004. • Refractive Index Liquids for Dispersion Staining: high-dispersion series, 1.550, 1.605, 1... hand. Repeat the series. Collect the dispersed solids by centrifugation at 1000 rpm for 5 minutes. Wash...

Rotary bulk solids divider

DOEpatents

Maronde, Carl P.; Killmeyer, Jr., Richard P.

1992-01-01

An apparatus for the disbursement of a bulk solid sample comprising, a gravity hopper having a top open end and a bottom discharge end, a feeder positioned beneath the gravity hopper so as to receive a bulk solid sample flowing from the bottom discharge end, and a conveyor receiving the bulk solid sample from the feeder and rotating on an axis that allows the bulk solid sample to disperse the sample to a collection station.

ROTARY BULK SOLIDS DIVIDER

DOEpatents

Maronde, Carl P.; Killmeyer JR., Richard P.

1992-03-03

An apparatus for the disbursement of a bulk solid sample comprising, a gravity hopper having a top open end and a bottom discharge end, a feeder positioned beneath the gravity hopper so as to receive a bulk solid sample flowing from the bottom discharge end, and a conveyor receiving the bulk solid sample from the feeder and rotating on an axis that allows the bulk solid sample to disperse the sample to a collection station.

Biomimetics on seed dispersal: survey and insights for space exploration.

PubMed

Pandolfi, Camilla; Izzo, Dario

2013-06-01

Seeds provide the vital genetic link and dispersal agent between successive generations of plants. Without seed dispersal as a means of reproduction, many plants would quickly die out. Because plants lack any sort of mobility and remain in the same spot for their entire lives, they rely on seed dispersal to transport their offspring throughout the environment. This can be accomplished either collectively or individually; in any case as seeds ultimately abdicate their movement, they are at the mercy of environmental factors. Thus, seed dispersal strategies are characterized by robustness, adaptability, intelligence (both behavioral and morphological), and mass and energy efficiency (including the ability to utilize environmental sources of energy available): all qualities that advanced engineering systems aim at in general, and in particular those that need to enable complex endeavors such as space exploration. Plants evolved and adapted their strategy according to their environment, and taken together, they enclose many desirable characteristics that a space mission needs to have. Understanding in detail how plants control the development of seeds, fabricate structural components for their dispersal, build molecular machineries to keep seeds dormant up to the right moment and monitor the environment to release them at the right time could provide several solutions impacting current space mission design practices. It can lead to miniaturization, higher integration and packing efficiency, energy efficiency and higher autonomy and robustness. Consequently, there would appear to be good reasons for considering biomimetic solutions from plant kingdom when designing space missions, especially to other celestial bodies, where solid and liquid surfaces, atmosphere, etc constitute and are obviously parallel with the terrestrial environment where plants evolved. In this paper, we review the current state of biomimetics on seed dispersal to improve space mission design.

Reflection and transmission of elastic waves through a couple-stress elastic slab sandwiched between two half-spaces

NASA Astrophysics Data System (ADS)

Wang, Changda; Chen, Xuejun; Wei, Peijun; Li, Yueqiu

2017-12-01

The reflection and transmission of elastic waves through a couple-stress elastic slab that is sandwiched between two couple-stress elastic half-spaces are studied in this paper. Because of the couple-stress effects, there are three types of elastic waves in the couple-stress elastic solid, two of which are dispersive. The interface conditions between two couple-stress solids involve the surface couple and rotation apart from the surface traction and displacement. The nontraditional interface conditions between the slab and two solid half-spaces are used to obtain the linear algebraic equation sets from which the amplitude ratios of reflection and transmission waves to the incident wave can be determined. Then, the energy fluxes carried by the various reflection and transmission waves are calculated numerically and the normal energy flux conservation is used to validate the numerical results. The special case, couple-stress elastic slab sandwiched by the classical elastic half-spaces, is also studied and compared with the situation that the classical elastic slab sandwiched by the classical elastic half-spaces. Incident longitudinal wave (P wave) and incident transverse wave (SV wave) are both considered. The influences of the couple-stress are mainly discussed based on the numerical results. It is found that the couple-stress mainly influences the transverse modes of elastic waves.

Extraction of acetanilides in rice using ionic liquid-based matrix solid phase dispersion-solvent flotation.

PubMed

Zhang, Liyuan; Wang, Changyuan; Li, Zuotong; Zhao, Changjiang; Zhang, Hanqi; Zhang, Dongjie

2018-04-15

Ionic liquid-based matrix solid phase dispersion-solvent flotation coupled with high performance liquid chromatography was developed for the determination of the acetanilide herbicides, including metazachlor, propanil, alachlor, propisochlor, pretilachlor, and butachlor in rice samples. Some experimental parameters, including the type of dispersant, the mass ratio of dispersant to sample, pH of sample solution, the type of extraction solvent, the type of ionic liquid, flotation time, and flow rate of N 2 were optimized. The average recoveries of the acetanilide herbicides at spiked concentrations of 50, 125, and 250 µg/kg ranged from 89.4% to 108.7%, and relative standard deviations were equal to or lower than 7.1%, the limits of quantification were in the range of 38.0 to 84.7 µg/kg. Copyright © 2017 Elsevier Ltd. All rights reserved.

Dispersed bubble reactor for enhanced gas-liquid-solids contact and mass transfer

DOE Office of Scientific and Technical Information (OSTI.GOV)

Vimalchand, Pannalal; Liu, Guohai; Peng, WanWang

An apparatus to promote gas-liquid contact and facilitate enhanced mass transfer. The dispersed bubble reactor (DBR) operates in the dispersed bubble flow regime to selectively absorb gas phase constituents into the liquid phase. The dispersion is achieved by shearing the large inlet gas bubbles into fine bubbles with circulating liquid and additional pumped liquid solvent when necessary. The DBR is capable of handling precipitates that may form during absorption or fine catalysts that may be necessary to promote liquid phase reactions. The DBR can be configured with multistage counter current flow sections by inserting concentric cylindrical sections into the risermore » to facilitate annular flow. While the DBR can absorb CO.sub.2 in liquid solvents that may lead to precipitates at high loadings, it is equally capable of handling many different types of chemical processes involving solids (precipitates/catalysts) along with gas and liquid phases.« less

Method of preparing a high solids content, low viscosity ceramic slurry

DOEpatents

Tiegs, Terry N.; Wittmer, Dale E.

1995-01-01

A method for producing a high solids content, low viscosity ceramic slurry composition comprises turbomilling a dispersion of a ceramic powder in a liquid to form a slurry having a viscosity less than 100 centipoise and a solids content equal to or greater than 48 volume percent.

Method of preparing a high solids content, low viscosity ceramic slurry

DOEpatents

Tiegs, T.N.; Wittmer, D.E.

1995-10-10

A method for producing a high solids content, low viscosity ceramic slurry composition comprises turbomilling a dispersion of a ceramic powder in a liquid to form a slurry having a viscosity less than 100 centipoise and a solids content equal to or greater than 48 volume percent.

Surface-Directed Synthesis of Erbium-Doped Yttrium Oxide Nanoparticles within Organosilane Zeptoliter Containers

PubMed Central

2015-01-01

We introduce an approach to synthesize rare earth oxide nanoparticles using high temperature without aggregation of the nanoparticles. The dispersity of the nanoparticles is controlled at the nanoscale by using small organosilane molds as reaction containers. Zeptoliter reaction vessels prepared from organosilane self-assembled monolayers (SAMs) were used for the surface-directed synthesis of rare earth oxide (REO) nanoparticles. Nanopores of octadecyltrichlorosilane were prepared on Si(111) using particle lithography with immersion steps. The nanopores were filled with a precursor solution of erbium and yttrium salts to confine the crystallization step to occur within individual zeptoliter-sized organosilane reaction vessels. Areas between the nanopores were separated by a matrix film of octadecyltrichlorosilane. With heating, the organosilane template was removed by calcination to generate a surface array of erbium-doped yttria nanoparticles. Nanoparticles synthesized by the surface-directed approach retain the periodic arrangement of the nanopores formed from mesoparticle masks. While bulk rare earth oxides can be readily prepared by solid state methods at high temperature (>900 °C), approaches for preparing REO nanoparticles are limited. Conventional wet chemistry methods are limited to low temperatures according to the boiling points of the solvents used for synthesis. To achieve crystallinity of REO nanoparticles requires steps for high-temperature processing of samples, which can cause self-aggregation and dispersity in sample diameters. The facile steps for particle lithography address the problems of aggregation and the requirement for high-temperature synthesis. PMID:25163977

A hybridization approach to efficient TiO2 photodegradation of aqueous benzalkonium chloride.

PubMed

Suchithra, Padmajan Sasikala; Carleer, Robert; Ananthakumar, Solaippan; Yperman, Jan

2015-08-15

TiO2 get positively charged upon UV-irradiation and repel the cationic pollutants away from the surface. Hybridization of AC onto TiO2 (ACT) tends catalyst surface negatively charged besides providing highly favorable adsorptions sites for cationic pollutants. The photodegradation of benzalkonium chloride (BKC), a quaternary ammonium surfactant and a pharmaceutical, is investigated with ACT. The surface charge of the catalyst in surfactant and non-surfactant aqueous dispersion under UV-irradiation is investigated and explained. The anomalous increase in COD values at the beginning of BKC-photodegradation is explained. The intermediate products formed are identified in both solution and solid phase. Trace amount of dodecane remained adsorbed on the catalyst surface after 1h UV-irradiation, but complete mineralization of BKC is achieved with 2h UV-irradiation. We propose that BKC photodegradation starts by central fission of benzyl CN bond followed by dealkylation, and demethylation steps. Copyright © 2015 Elsevier B.V. All rights reserved.

Synthesis and characterization of high surface area TiO 2/SiO 2 mesostructured nanocomposite

NASA Astrophysics Data System (ADS)

Bonne, Magali; Pronier, Stéphane; Can, Fabien; Courtois, Xavier; Valange, Sabine; Tatibouët, Jean-Michel; Royer, Sébastien; Marécot, Patrice; Duprez, Daniel

2010-06-01

Recently titania synthesis was reported using various structuration procedures, leading to the production of solid presenting high surface area but exhibiting moderate thermal stability. The study presents the synthesis of TiO 2/SiO 2 nanocomposites, a solid that can advantageously replace bulk titania samples as catalyst support. The silica host support used for the synthesis of the nanocomposite is a SBA-15 type silica, having a well-defined 2D hexagonal pore structure and a large pore size. The control of the impregnation media is important to obtain dispersed titania crystals into the porosity, the best results have been obtained using an impregnation in an excess of solvent. After calcination at low temperature (400 °C), nanocomposites having titania nanodomains (˜2-3 nm) located inside the pores and no external aggregates visible are obtained. This nanocomposite exhibits high specific surface area (close to that of the silica host support, even with a titania loading of 55 wt.%) and a narrow pore size distribution. Surprisingly, the increase in calcination temperature up to 800 °C does not allow to detect the anatase to rutile transition. Even at 800 °C, the hexagonal mesoporous structure of the silica support is maintained, and the anatase crystal domain size is evaluated at ˜10 nm, a size close to that of the silica host support porosity (8.4 nm). Comparison of their physical properties with the results presented in literature for bulk samples evidenced that these TiO 2/SiO 2 solids are promising in term of thermal stability.

Ultrasound/microwave-assisted solid-liquid-solid dispersive extraction with high-performance liquid chromatography coupled to tandem mass spectrometry for the determination of neonicotinoid insecticides in Dendrobium officinale.

PubMed

Zheng, Shuilian; Wu, Huizhen; Li, Zuguang; Wang, Jianmei; Zhang, Hu; Qian, Mingrong

2015-01-01

A one-step ultrasound/microwave-assisted solid-liquid-solid dispersive extraction procedure was used for the simultaneous determination of eight neonicotinoids (dinotefuran, nitenpyram, thiamethoxam, clothianidin, imidacloprid, acetamiprid, thiacloprid, imidaclothiz) in dried Dendrobium officinale by liquid chromatography combined with electrospray ionization triple quadrupole tandem mass spectrometry in multiple reaction monitoring mode. The samples were quickly extracted by acetonitrile and cleaned up by the mixed dispersing sorbents including primary secondary amine, C18 , and carbon-GCB. Parameters that could influence the ultrasound/microwave-assisted extraction efficiency such as microwave irradiation power, ultrasound irradiation power, temperature, and solvent were investigated. Recovery studies were performing well (70.4-113.7%) at three examined spiking levels (10, 50, and 100 μg/kg). Meanwhile, the limits of quantification for the neonicotinoids ranged from 0.87 to 1.92 μg/kg. The method showed good linearity in the concentration range of 1-100 μg/L with correlation coefficients >0.99. This quick and useful analytical method could provide a basis for monitoring neonicotinoid insecticide residues in herbs. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Determination of six pesticides in the medicinal herb Cordia salicifolia by matrix solid-phase dispersion and gas chromatography/mass spectrometry.

PubMed

de Carvalho, Pedro Henrique Viana; Prata, Vanessa de Menezes; Alves, Péricles Barreto; Navickiene, Sandro

2009-01-01

A simple and effective extraction method based on matrix solid-phase dispersion was developed for acephate, chlorpropham, pyrimicarb, bifenthrin, tetradifon, and phosalone in leaves of the medicinal plant Cordia salicifolia, whose extracts are commercialized in Brazil as diuretic, appetite suppressant, and weight loss products. The determination method was GC/MS with selected-ion monitoring. Different parameters of the method were evaluated, such as type of solid phase (C18, alumina, silica gel, and Florisil) and the amount of solid phase and eluent (dichloromethane, ethyl acetate, chloroform, and cyclohexane). The best results were obtained using 0.5 g herb sample, 0.5 g neutral alumina as the dispersant sorbent, 0.5 g C18 as the cleanup sorbent, and cyclohexane-dichloromethane (3 + 1, v/v) as the eluting solvent. The method was validated using herb samples fortified with pesticides at different concentration levels (0.3, 0.5, and 1.0 mg/kg). Average recoveries (seven replicates) ranged from 67.7 to 129.9%, with relative standard deviations between 6.3 and 26%. Detection and quantitation limits for the herb ranged from 0.10 to 0.15 and 0.15 to 0.25 mg/kg, respectively.

Dynamics of ultrathin metal films on amorphous substrates under fast thermal processing

DOE Office of Scientific and Technical Information (OSTI.GOV)

Favazza, Christopher; Kalyanaraman, Ramki; Sureshkumar, Radhakrishna

A mathematical model is developed to analyze the growth/decay rate of surface perturbations of an ultrathin metal film on an amorphous substrate (SiO{sub 2}). The formulation combines the approach of Mullins [W. W. Mullins, J. Appl. Phys. 30, 77 (1959)] for bulk surfaces, in which curvature-driven mass transport and surface deformation can occur by surface/volume diffusion and evaporation-condensation processes, with that of Spencer et al. [B. J. Spencer, P. W. Voorhees, and S. H. Davis, Phys. Rev. Lett. 67, 26 (1991)] to describe solid-state transport in thin films under epitaxial strain. Modifications of the Mullins model to account for thin-filmmore » boundary conditions result in qualitatively different dispersion relationships especially in the limit as kh{sub o}<<1, where k is the wavenumber of the perturbation and h{sub o} is the unperturbed film height. The model is applied to study the relative rate of solid-state mass transport as compared to that of liquid phase dewetting in a thin film subjected to a fast thermal pulse. Specifically, we have recently shown that multiple cycles of nanosecond (ns) pulsed laser melting and resolidification of ultrathin metal films on amorphous substrates can lead to the formation of various types of spatially ordered nanostructures [J. Trice, D. Thomas, C. Favazza, R. Sureshkumar, and R. Kalyanaraman, Phys. Rev. B 75, 235439 (2007)]. The pattern formation has been attributed to the dewetting of the thin film by a hydrodynamic instability. In such experiments the film is in the solid state during a substantial fraction of each thermal cycle. However, results of a linear stability analysis based on the aforementioned model suggest that solid-state mass transport has a negligible effect on morphological changes of the surface. Further, a qualitative analysis of the effect of thermoelastic stress, induced by the rapid temperature changes in the film-substrate bilayer, suggests that stress relaxation does not appreciably contribute to surface deformation. Hence, surface deformation caused by liquid phase instabilities is rapidly quenched-in during the cooling phase. This deformed state is further evolved by subsequent laser pulses. These results have implications to developing accurate computer simulations of thin-film dewetting by energetic beams aimed at the manufacturing of optically active nanoscale materials for applications including information processing, optical devices, and solar energy harvesting.« less

Dynamics of ultrathin metal films on amorphous substrates under fast thermal processing

NASA Astrophysics Data System (ADS)

Favazza, Christopher; Kalyanaraman, Ramki; Sureshkumar, Radhakrishna

2007-11-01

A mathematical model is developed to analyze the growth/decay rate of surface perturbations of an ultrathin metal film on an amorphous substrate (SiO2). The formulation combines the approach of Mullins [W. W. Mullins, J. Appl. Phys. 30, 77 (1959)] for bulk surfaces, in which curvature-driven mass transport and surface deformation can occur by surface/volume diffusion and evaporation-condensation processes, with that of Spencer etal . [B. J. Spencer, P. W. Voorhees, and S. H. Davis, Phys. Rev. Lett. 67, 26 (1991)] to describe solid-state transport in thin films under epitaxial strain. Modifications of the Mullins model to account for thin-film boundary conditions result in qualitatively different dispersion relationships especially in the limit as kho≪1, where k is the wavenumber of the perturbation and ho is the unperturbed film height. The model is applied to study the relative rate of solid-state mass transport as compared to that of liquid phase dewetting in a thin film subjected to a fast thermal pulse. Specifically, we have recently shown that multiple cycles of nanosecond (ns) pulsed laser melting and resolidification of ultrathin metal films on amorphous substrates can lead to the formation of various types of spatially ordered nanostructures [J. Trice, D. Thomas, C. Favazza, R. Sureshkumar, and R. Kalyanaraman, Phys. Rev. B 75, 235439 (2007)]. The pattern formation has been attributed to the dewetting of the thin film by a hydrodynamic instability. In such experiments the film is in the solid state during a substantial fraction of each thermal cycle. However, results of a linear stability analysis based on the aforementioned model suggest that solid-state mass transport has a negligible effect on morphological changes of the surface. Further, a qualitative analysis of the effect of thermoelastic stress, induced by the rapid temperature changes in the film-substrate bilayer, suggests that stress relaxation does not appreciably contribute to surface deformation. Hence, surface deformation caused by liquid phase instabilities is rapidly quenched-in during the cooling phase. This deformed state is further evolved by subsequent laser pulses. These results have implications to developing accurate computer simulations of thin-film dewetting by energetic beams aimed at the manufacturing of optically active nanoscale materials for applications including information processing, optical devices, and solar energy harvesting.

Graphene-encapsulated silica as matrix solid-phase dispersion extraction sorbents for the analysis of poly-methoxylated flavonoids in the leaves of Murraya panaculata (L.) Jack.

PubMed

Sun, Ting; Li, Xuwen; Yang, Jie; Li, Lanjie; Jin, Yongri; Shi, Xiaolei

2015-06-01

In this study, graphene-encapsulated silica was synthesized by a hydrothermal reduction strategy. The presence of silica in graphene was identified by Fourier-transform infrared spectrometry, X-ray diffraction and scanning electron microscopy. The graphene-encapsulated silica subsequently was used as adsorbent for matrix solid-phase dispersion extraction of poly-methoxylated flavonoids from the dried leaves of Murraya panaculata (L.) Jack. Compared with the other adsorbents (graphene, silica gel, C18 silica, neutral alumina, diatomaceous earth) and without any adsorbents, better results were obtained. Then a method for analysis of poly-methoxylated flavonoids was established by coupling matrix solid-phase dispersion extraction with ultra high performance liquid chromatography and UV detection. Compared with reflux extraction and ultrasonic extraction, the proposed method is quicker, more efficient and more environmental protection. Less than 10 min is needed from extraction to detection. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Enhanced chemoprophylactic and clinical efficacy of albendazole formulated as solid dispersions in experimental cystic echinococcosis.

PubMed

Pensel, Patricia E; Castro, Silvina; Allemandi, Daniel; Bruni, Sergio Sánchez; Palma, Santiago D; Elissondo, María Celina

2014-06-16

Cystic echinococcosis is a chronic, complex, and still neglected disease. Although albendazole has demonstrated efficacy, only about one-third of patients experience complete remission or cure and 30-50% of treated patients develop some evidence of a therapeutic response. Different strategies have been developed in order to improve the albendazole water solubility and dissolution rate. The aim of the current work was to investigate the chemoprophylactic and clinical efficacy of an albendazole:poloxamer 188 solid dispersion formulation on mice infected with Echinococcus granulosus metacestodes. Albendazole formulated as solid dispersion had greater chemoprophylactic and clinical efficacy than albendazole alone. The improved in therapeutic efficacy could be a consequence of the increase in the systemic availability of albendazole sulfoxide. The work reported here demonstrates that in vivo treatment with albendazole:poloxamer 188 impairs the development of the hydatid cysts. This new pharmacotechnically based strategy could be a suitable alternative for treating cystic echinococcosis in humans. Copyright © 2014 Elsevier B.V. All rights reserved.

Characterization of proton exchange membrane materials for fuel cells by solid state nuclear magnetic resonance

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kong, Zueqian

2010-01-01

Solid-state nuclear magnetic resonance (NMR) has been used to explore the nanometer-scale structure of Nafion, the widely used fuel cell membrane, and its composites. We have shown that solid-state NMR can characterize chemical structure and composition, domain size and morphology, internuclear distances, molecular dynamics, etc. The newly-developed water channel model of Nafion has been confirmed, and important characteristic length-scales established. Nafion-based organic and inorganic composites with special properties have also been characterized and their structures elucidated. The morphology of Nafion varies with hydration level, and is reflected in the changes in surface-to-volume (S/V) ratio of the polymer obtained by small-anglemore » X-ray scattering (SAXS). The S/V ratios of different Nafion models have been evaluated numerically. It has been found that only the water channel model gives the measured S/V ratios in the normal hydration range of a working fuel cell, while dispersed water molecules and polymer ribbons account for the structures at low and high hydration levels, respectively.« less

Morphological Control of In x Ga 1–x P Nanocrystals Synthesized in a Nonthermal Plasma

DOE PAGES

Bronstein, Noah D.; Wheeler, Lance M.; Anderson, Nicholas C.; ...

2018-04-09

We explore the growth of InxGa1-xP nanocrystals (x = 1, InP; x = 0, GaP; and 1 > x > 0, alloys) in a nonthermal plasma. By tuning the reactor conditions, we gain control over the morphology of the final product, producing either 10 nm diameter hollow nanocrystals or smaller 3 nm solid nanocrystals. We observe the gas-phase chemistry in the plasma reactor using plasma emission spectroscopy to understand the growth mechanism of the hollow versus solid morphology. We also connect this plasma chemistry to the subsequent native surface chemistry of the nanocrystals, which is dominated by the presence ofmore » both dative- and lattice-bound phosphine species. The dative phosphines react readily with oleylamine in an L-type ligand exchange reaction, evolving phosphines and allowing the particles to be dispersed in nonpolar solvents. Subsequent treatment by HF causes the solid InP1.5 and In0.5Ga0.5P1.3 to become photoluminescent, whereas the hollow particles remain nonemissive.« less

Morphological Control of In xGa 1–xP Nanocrystals Synthesized in a Nonthermal Plasma

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bronstein, Noah D.; Wheeler, Lance M.; Anderson, Nicholas C.

Here, we explore the growth of In xGa 1–xP nanocrystals (x = 1, InP; x = 0, GaP; and 1 > x > 0, alloys) in a nonthermal plasma. By tuning the reactor conditions, we gain control over the morphology of the final product, producing either 10 nm diameter hollow nanocrystals or smaller 3 nm solid nanocrystals. We observe the gas-phase chemistry in the plasma reactor using plasma emission spectroscopy to understand the growth mechanism of the hollow versus solid morphology. We also connect this plasma chemistry to the subsequent native surface chemistry of the nanocrystals, which is dominated bymore » the presence of both dative- and lattice-bound phosphine species. The dative phosphines react readily with oleylamine in an L-type ligand exchange reaction, evolving phosphines and allowing the particles to be dispersed in nonpolar solvents. Subsequent treatment by HF causes the solid InP 1.5 and In 0.5Ga 0.5P 1.3 to become photoluminescent, whereas the hollow particles remain nonemissive.« less

Morphological Control of In xGa 1–xP Nanocrystals Synthesized in a Nonthermal Plasma

DOE PAGES

Bronstein, Noah D.; Wheeler, Lance M.; Anderson, Nicholas C.; ...

2018-04-09

Here, we explore the growth of In xGa 1–xP nanocrystals (x = 1, InP; x = 0, GaP; and 1 > x > 0, alloys) in a nonthermal plasma. By tuning the reactor conditions, we gain control over the morphology of the final product, producing either 10 nm diameter hollow nanocrystals or smaller 3 nm solid nanocrystals. We observe the gas-phase chemistry in the plasma reactor using plasma emission spectroscopy to understand the growth mechanism of the hollow versus solid morphology. We also connect this plasma chemistry to the subsequent native surface chemistry of the nanocrystals, which is dominated bymore » the presence of both dative- and lattice-bound phosphine species. The dative phosphines react readily with oleylamine in an L-type ligand exchange reaction, evolving phosphines and allowing the particles to be dispersed in nonpolar solvents. Subsequent treatment by HF causes the solid InP 1.5 and In 0.5Ga 0.5P 1.3 to become photoluminescent, whereas the hollow particles remain nonemissive.« less

Planetesimal formation in self-gravitating discs

NASA Astrophysics Data System (ADS)

Gibbons, P. G.; Rice, W. K. M.; Mamatsashvili, G. R.

2012-10-01

We study particle dynamics in local two-dimensional simulations of self-gravitating accretion discs with a simple cooling law. It is well known that the structure which arises in the gaseous component of the disc due to a gravitational instability can have a significant effect on the evolution of dust particles. Previous results using global simulations indicate that spiral density waves are highly efficient at collecting dust particles, creating significant local overdensities which may be able to undergo gravitational collapse. We expand on these findings using a range of cooling times to mimic the conditions at a large range of radii within the disc. Here we use the PENCIL code to solve the 2D local shearing sheet equations for gas on a fixed grid together with the equations of motion for solids coupled to the gas solely through aerodynamic drag force. We find that spiral density waves can create significant enhancements in the surface density of solids, equivalent to 1-10 cm sized particles in a disc following the profiles of Clarke around an ˜1 M⊙ star, causing it to reach concentrations several orders of magnitude larger than the particles mean surface density. We also study the velocity dispersion of the particles, finding that the spiral structure can result in the particle velocities becoming highly ordered, having a narrow velocity dispersion. This implies low relative velocities between particles, which in turn suggest that collisions are typically low energy, lessening the likelihood of grain destruction. Both these findings suggest that the density waves that arise due to gravitational instabilities in the early stages of star formation provide excellent sites for the formation of large, planetesimal-sized objects.

Sodium alginate as a potential carrier in solid dispersion formulations to enhance dissolution rate and apparent water solubility of BCS II drugs.

PubMed

Borba, Paola Aline Amarante; Pinotti, Marihá; de Campos, Carlos Eduardo Maduro; Pezzini, Bianca Ramos; Stulzer, Hellen Karine

2016-02-10

The solid dispersion technique is the most effective method for improving the dissolution rate of poorly water-soluble drugs, however it depends on a suitable carrier selection. The work explored the use of the biopolymer sodium alginate (SA) as a potential carrier in solid dispersions (SD). The data demonstrated that SA was able to improve the biopharmaceutical properties of the BCS II drug telmisartan (TEL) of low solubility even using relative small drug:polymer ratio. A solid state grinding process was used to prepare the solid dispersions (SD) during 45 min. The SD were prepared in different proportions of drug and carrier of 1:1, 1:3, 1:5, 1:7 and 1:9 (mass/mass). DSC, XRPD, FTIR and Raman confirmed the presence of molecular interactions between TEL and the carrier. FTIR supports the presence of hydrogen bonds between TEL and the carrier. SD_1:5, SD_1:7 and SD_1:9 enhanced the dissolution rate of the drug releasing more than 80% of the drug in just 30 min (83%, 84% and 87%). The the t-test results demonstrated equal dissolution efficiency values for SD_1:7 and Micardis(®), however the similarity (f2) and difference (f1) fit factors showed that the SD and Micardis(®) are statistically different. The physical stability studies demonstrated that SD using sodium alginate as a carrier remained unchanged during the period of 90 days at room temperature, showing that the sodium alginate acts as a good anti plasticizer agent, preventing the drug recrystallization. Copyright © 2015 Elsevier Ltd. All rights reserved.

Dual Activity of Hydroxypropyl-β-Cyclodextrin and Water-Soluble Carriers on the Solubility of Carvedilol.

PubMed

Zoghbi, Abdelmoumin; Geng, Tianjiao; Wang, Bo

2017-11-01

Carvedilol (CAR) is a non-selective α and β blocker categorized as class II drug with low water solubility. Several recent studies have investigated ways to overcome this problem. The aim of the present study was to combine two of these methods: the inclusion complex using hydroxypropyl-β-cyclodextrin (HPβCD) with solid dispersion using two carriers: Poloxamer 188 (PLX) and Polyvinylpyrrolidone K-30 (PVP) to enhance the solubility, bioavailability, and the stability of CAR. Kneading method was used to prepare CAR-HPβCD inclusion complex (KD). The action of different carriers separately and in combination on Carvedilol solubility was investigated in three series. CAR-carrier and KD-carrier solid dispersions were prepared by solvent evaporation method. In vitro dissolution test was conducted in three different media: double-distilled water (DDW), simulative gastric fluid (SGF), and PBS pH 6.8 (PBS). The interactions between CAR, HPβCD, and different carriers were explored by Fourier transform infrared spectroscopy (FTIR), powder X-ray diffractometry (XRD), and differential scanning colorimetry (DSC). The results showed higher solubility of CAR in KD-PVP solid dispersions up to 70, 25, and 22 fold compared to pure CAR in DDW, SGF, and PBS, respectively. DSC and XRD analyses indicated an improved degree of transformation of CAR in KD-PVP solid dispersion from crystalline to amorphous state. This study provides a new successful combination of two polymers with the dual action of HPβCD and PLX/PVP on water solubility and bioavailability of CAR.

Investigation of Phase Mixing in Amorphous Solid Dispersions of AMG 517 in HPMC-AS Using DSC, Solid-State NMR, and Solution Calorimetry.

PubMed

Calahan, Julie L; Azali, Stephanie C; Munson, Eric J; Nagapudi, Karthik

2015-11-02

Intimate phase mixing between the drug and the polymer is considered a prerequisite to achieve good physical stability for amorphous solid dispersions. In this article, spray dried amorphous dispersions (ASDs) of AMG 517 and HPMC-as were studied by differential scanning calorimetry (DSC), solid-state NMR (SSNMR), and solution calorimetry. DSC analysis showed a weakly asymmetric (ΔTg ≈ 13.5) system with a single glass transition for blends of different compositions indicating phase mixing. The Tg-composition data was modeled using the BKCV equation to accommodate the observed negative deviation from ideality. Proton spin-lattice relaxation times in the laboratory and rotating frames ((1)H T1 and T1ρ), as measured by SSNMR, were consistent with the observation that the components of the dispersion were in intimate contact over a 10-20 nm length scale. Based on the heat of mixing calculated from solution calorimetry and the entropy of mixing calculated from the Flory-Huggins theory, the free energy of mixing was calculated. The free energy of mixing was found to be positive for all ASDs, indicating that the drug and polymer are thermodynamically predisposed to phase separation at 25 °C. This suggests that miscibility measured by DSC and SSNMR is achieved kinetically as the result of intimate mixing between drug and polymer during the spray drying process. This kinetic phase mixing is responsible for the physical stability of the ASD.

Simultaneous determination and qualitative analysis of six types of components in Naoxintong capsule by miniaturized matrix solid-phase dispersion extraction coupled with ultra high-performance liquid chromatography with photodiode array detection and quadrupole time-of-flight mass spectrometry.

PubMed

Wang, Huilin; Jiang, Yan; Ding, Mingya; Li, Jin; Hao, Jia; He, Jun; Wang, Hui; Gao, Xiu-Mei; Chang, Yan-Xu

2018-02-03

A simple and effective sample preparation process based on miniaturized matrix solid-phase dispersion was developed for simultaneous determination of phenolic acids (gallic acid, chlorogenic acid, ferulic acid, 3,5-dicaffeoylqunic acid, 1,5-dicaffeoylqunic acid, rosmarinic acid, lithospermic acid, and salvianolic acid B), flavonoids (kaempferol-3-O-rutinoside, calycosin, and formononetin), lactones (ligustilide and butyllidephthalide), monoterpenoids (paeoniflorin), phenanthraquinones (cryptotanshinone), and furans (5-hydroxymethylfurfural) in Naoxintong capsule by ultra high-performance liquid chromatography. The optimized condition was that 25 mg Naoxintong powder was blended homogeneously with 100 mg Florisil PR for 4 min. One milliliter of methanol/water (75:25, v/v) acidified by 0.05% formic acid was selected to elute all components. It was found that the recoveries of the six types of components ranged from 61.36 to 96.94%. The proposed miniaturized matrix solid-phase dispersion coupled with ultra high-performance liquid chromatography was successfully applied to simultaneous determination of the six types of components in Naoxintong capsules. The results demonstrated that the proposed miniaturized matrix solid-phase dispersion coupled with ultra high-performance liquid chromatography could be used as an environmentally friendly tool for the extraction and determination of multiple bioactive components in natural products. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Preparation and characterization of fusion processed solid dispersions containing a viscous thermally labile polymeric carrier.

PubMed

Hughey, Justin R; Keen, Justin M; Miller, Dave A; Brough, Chris; McGinity, James W

2012-11-15

The primary aim of the present study was to investigate the ability of hydroxypropyl and methoxyl substituted cellulose ethers to stabilize supersaturated concentrations of itraconazole (ITZ), a poorly water-soluble weak base, after an acid-to-neutral pH transition. A secondary aim of the study was to evaluate the effect of fusion processes on polymer stability and molecular weight. Polymer screening studies showed that stabilization of ITZ supersaturation was related to the molecular weight of the polymer and levels of hydroxypropyl and methoxyl substitution. METHOCEL E50LV (E50LV), which is characterized as having a high melt viscosity, was selected for solid dispersion formulation studies. Hot-melt extrusion processing of E50LV based compositions resulted in high torque loads, low material throughput and polymer degradation. KinetiSol Dispersing, a novel fusion based processing technique, was evaluated as a method to prepare the solid dispersions with reduced levels of polymer degradation. An experimental design revealed that polymer molecular weight was sensitive to shearing forces and high temperatures. However, optimal processing conditions resulted in significantly reduced E50LV degradation relative to HME processing. The technique was effectively utilized to prepare homogenous solid solutions of E50LV and ITZ, characterized as having a single glass transition temperature over a wide range of drug loadings. All prepared compositions provided for a high degree of ITZ supersaturation stabilization. Copyright © 2012 Elsevier B.V. All rights reserved.

Comparison between hot-melt extrusion and spray-drying for manufacturing solid dispersions of the graft copolymer of ethylene glycol and vinylalcohol.

PubMed

Guns, Sandra; Dereymaker, Aswin; Kayaert, Pieterjan; Mathot, Vincent; Martens, Johan A; Van den Mooter, Guy

2011-03-01

To investigate the effect of the manufacturing method (spray-drying or hot-melt extrusion) on the kinetic miscibility of miconazole and the graft copolymer poly(ethyleneglycol-g-vinylalcohol). The effect of heat pre-treatment of solutions used for spray-drying and the use of spray-dried copolymer as excipient for hot-melt extrusion was investigated. The solid dispersions were prepared at different drug-polymer ratios and analyzed with modulated differential scanning calorimetry and X-ray powder diffraction. Miconazole either mixed with the PEG-fraction of the copolymer or crystallized in the same or a different polymorph as the starting material. The kinetic miscibility was higher for the solid dispersions obtained from solutions which were pre-heated compared to those spray-dried from solutions at ambient temperature. Hot-melt extrusion resulted in an even higher mixing capability. Here the use of the spray-dried copolymer did not show any benefit concerning the kinetic miscibility of the drug and copolymer, but it resulted in a remarkable decrease in the torque experienced by the extruder allowing extrusion at lower temperature and torque. The manufacturing method has an influence on the mixing capacity and phase behavior of solid dispersions. Heat pre-treatment of the solutions before spray-drying can result in a higher kinetic miscibility. Amorphization of the copolymer by spray-drying before using it as an excipient for hot-melt extrusion can be a manufacturing benefit.

Application of melt extrusion in the development of a physically and chemically stable high-energy amorphous solid dispersion of a poorly water-soluble drug.

PubMed

Lakshman, Jay P; Cao, Yu; Kowalski, James; Serajuddin, Abu T M

2008-01-01

Formulation of active pharmaceutical ingredients (API) in high-energy amorphous forms is a common strategy to enhance solubility, dissolution rate and, consequently, oral bioavailability of poorly water-soluble drugs. Amorphous APIs are, however, susceptible to recrystallization and, therefore, there is a need to physically stabilize them as solid dispersions in polymeric carriers. Hot melt extrusion has in recent years gained wide acceptance as a method of choice for the preparation of solid dispersions. There is a potential that the API, the polymer or both may degrade if excessively high temperature is needed in the melt extrusion process, especially when the melting point of the API is high. This report details a novel method where the API was first converted to an amorphous form by solvent evaporation and then melt-extruded with a suitable polymer at a drug load of at least 20% w/w. By this means, melt extrusion could be performed much below the melting temperature of the drug substance. Since the glass transition temperature of the amorphous drug was lower than that of the polymer used, the drug substance itself served as the plasticizer for the polymer. The addition of surfactants in the matrix enhanced dispersion and subsequent dissolution of the drug in aqueous media. The amorphous melt extrusion formulations showed higher bioavailability than formulations containing the crystalline API. There was no conversion of amorphous solid to its crystalline form during accelerated stability testing of dosage forms.

Synthesis of oxocarbon-encapsulated gold nanoparticles with blue-shifted localized surface plasmon resonance by pulsed laser ablation in water with CO2 absorbers

NASA Astrophysics Data System (ADS)

Del Rosso, T.; Rey, N. A.; Rosado, T.; Landi, S.; Larrude, D. G.; Romani, E. C.; Freire Junior, F. L.; Quinteiro, S. M.; Cremona, M.; Aucelio, R. Q.; Margheri, G.; Pandoli, O.

2016-06-01

Colloidal suspensions of oxocarbon-encapsulated gold nanoparticles have been synthesized in a one-step procedure by pulsed-laser ablation (PLA) at 532 nm of a solid gold target placed in aqueous solution containing CO2 absorbers, but without any stabilizing agent. Multi-wavelength surface enhanced Raman spectroscopy allows the identification of adsorbed amorphous carbon and graphite, Au-carbonyl, Au coordinated CO2-derived bicarbonates/carbonates and hydroxyl groups around the AuNPs core. Scanning electron microscopy, energy dispersive x-ray analysis and high resolution transmission electron microscopy highlight the organic shell structure around the crystalline metal core. The stability of the colloidal solution of nanocomposites (NCs) seems to be driven by solvation forces and is achieved only in neutral or basic pH using monovalent hydroxide counter-ions (NaOH, KOH). The NCs are characterized by a blue shift of the localized surface plasmon resonance (LSPR) band typical of metal-ligand stabilization by terminal π-back bonding, attributed to a core charging effect caused by Au-carbonyls. Total organic carbon measurements detect the final content of organic carbon in the colloidal solution of NCs that is about six times higher than the value of the water solution used to perform PLA. The colloidal dispersions of NCs are stable for months and are applied as analytical probes in amino glycoside antibiotic LSPR based sensing.

Synthesis of oxocarbon-encapsulated gold nanoparticles with blue-shifted localized surface plasmon resonance by pulsed laser ablation in water with CO2 absorbers.

PubMed

Del Rosso, T; Rey, N A; Rosado, T; Landi, S; Larrude, D G; Romani, E C; Junior, F L Freire; Quinteiro, S M; Cremona, M; Aucelio, R Q; Margheri, G; Pandoli, O

2016-06-24

Colloidal suspensions of oxocarbon-encapsulated gold nanoparticles have been synthesized in a one-step procedure by pulsed-laser ablation (PLA) at 532 nm of a solid gold target placed in aqueous solution containing CO2 absorbers, but without any stabilizing agent. Multi-wavelength surface enhanced Raman spectroscopy allows the identification of adsorbed amorphous carbon and graphite, Au-carbonyl, Au coordinated CO2-derived bicarbonates/carbonates and hydroxyl groups around the AuNPs core. Scanning electron microscopy, energy dispersive x-ray analysis and high resolution transmission electron microscopy highlight the organic shell structure around the crystalline metal core. The stability of the colloidal solution of nanocomposites (NCs) seems to be driven by solvation forces and is achieved only in neutral or basic pH using monovalent hydroxide counter-ions (NaOH, KOH). The NCs are characterized by a blue shift of the localized surface plasmon resonance (LSPR) band typical of metal-ligand stabilization by terminal π-back bonding, attributed to a core charging effect caused by Au-carbonyls. Total organic carbon measurements detect the final content of organic carbon in the colloidal solution of NCs that is about six times higher than the value of the water solution used to perform PLA. The colloidal dispersions of NCs are stable for months and are applied as analytical probes in amino glycoside antibiotic LSPR based sensing.

A method for grindability testing using the Scirocco disperser.

PubMed

Bonakdar, Tina; Ali, Muzammil; Dogbe, Selasi; Ghadiri, Mojtaba; Tinke, Arjen

2016-03-30

In the early stages of development of a new Active Pharmaceutical Ingredient (API), insufficient material quantity is available for addressing processing issues, and it is highly desirable to be able to assess processability issues using the smallest possible powder sample quantity. A good example is milling of new active pharmaceutical ingredients. For particle breakage that is sensitive to strain rate, impact testing is the most appropriate method. However, there is no commercially available single particle impact tester for fine particulate solids. In contrast, dry powder dispersers, such as the Scirocco disperser of the Malvern Mastersizer 2000, are widely available, and can be used for this purpose, provided particle impact velocity is known. However, the distance within which the particles can accelerate before impacting on the bend is very short and different particle sizes accelerate to different velocities before impact. As the breakage is proportional to the square of impact velocity, the interpretation of breakage data is not straightforward and requires an analysis of particle velocity as a function of size, density and shape. We report our work using an integrated experimental and CFD modelling approach to evaluate the suitability of this device as a grindability testing device, with the particle sizing being done immediately following dispersion by laser diffraction. Aspirin, sucrose and α-lactose monohydrate are tested using narrow sieve cuts in order to minimise variations in impact velocity. The tests are carried out at eight different air nozzle pressures. As intuitively expected, smaller particles accelerate faster and impact the wall at a higher velocity compared to the larger particles. However, for a given velocity the extent of breakage of larger particles is larger. Using a numerical simulation based on CFD, the relationship between impact velocity and particle size and density has been established assuming a spherical shape, and using one-way coupling, as the particle concentration is very low. Taking account of these dependencies, a clear unification of the change in the specific surface area as a function of particle size, density and impact velocity is observed, and the slope of the fitted line gives a measure of grindability for each material. The trend of data obtained here matches the one obtained by single particle impact testing. Hence aerodynamic dispersion of solids by the Scirocco disperser can be used to evaluate the ease of grindability of different materials. Copyright © 2016 Elsevier B.V. All rights reserved.

Ignition kinetics of boron in primary combustion products of propellant based on its unique characteristics

NASA Astrophysics Data System (ADS)

Ao, Wen; Wang, Yang; Wu, Shixi

2017-07-01

Study on the boron-based primary combustion products can bridge the gap between primary combustion and secondary combustion in solid rocket ramjets. To clarify the initial state and ignition characteristics of boron particles in the after-burning chamber of solid rocket ramjets, the elemental, composition and morphology of the primary combustion products collected under gas generator chamber pressure of 0.2 MPa and 6 MPa were investigated by energy dispersive (EDS), X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy with energy dispersive (SEM-EDS) individually. The ignition times of boron particles among the primary combustion products were determined using a high temperature tube furnace system. The BD model was adopted for numerical verification. The numerical solution procedure of boron ignition model in a real afterburner chamber was modified. The results show that the sum of B, C, O elements in the primary combustion products reaches approximately 90%. The primary combustion products are mainly consisted of B, C, and B2O3. Images of the primary combustion products present highly agglomeration, indicating an oxidation of boron surface. Numerous spherical carbon particles with a diameter around 100 nm are observed in the products. Three features of the boron in the primary combustion products are obtained, compared to virgin boron. First most of the boron lumps are covered by carbon particles on the surface. Second the mean particle size is five times larger than that of virgin boron. Third the overall initial oxide layer covered on boron surface increases its thickness by above 0.1 μm. The ignition time of boron in the primary combustion products reaches 20-30 ms under 1673-1873 K, which is quite different from virgin boron of 4 ms. Numerical calculation results show the key reason leading to such a long ignition time is the variation of the initial oxide layer thickness. In conclusion, the physicochemical properties of boron particles are found to differ with virgin boron after primary combustion process. The accurate evaluation of the initial oxide layer thickness and initial particle radius is a crucial procedure before the numerical calculation of boron ignition kinetics. Results of our study are expected to provide better insight in the simulation of solid rocket ramjets working process.

Modelling low-frequency volcanic earthquakes in a viscoelastic medium with topography

NASA Astrophysics Data System (ADS)

Jousset, Philippe; Neuberg, Jürgen; Jolly, Arthur

2004-11-01

Magma properties are fundamental to explain the volcanic eruption style as well as the generation and propagation of seismic waves. This study focusses on magma properties and rheology and their impact on low-frequency volcanic earthquakes. We investigate the effects of anelasticity and topography on the amplitudes and spectra of synthetic low-frequency earthquakes. Using a 2-D finite-difference scheme, we model the propagation of seismic energy initiated in a fluid-filled conduit embedded in a homogeneous viscoelastic medium with topography. We model intrinsic attenuation by linear viscoelastic theory and we show that volcanic media can be approximated by a standard linear solid (SLS) for seismic frequencies above 2 Hz. Results demonstrate that attenuation modifies both amplitudes and dispersive characteristics of low-frequency earthquakes. Low frequency volcanic earthquakes are dispersive by nature; however, if attenuation is introduced, their dispersion characteristics will be altered. The topography modifies the amplitudes, depending on the position of the seismographs at the surface. This study shows that we need to take into account attenuation and topography to interpret correctly observed low-frequency volcanic earthquakes. It also suggests that the rheological properties of magmas may be constrained by the analysis of low-frequency seismograms.

The ionic versus metallic nature of 2D electrides: a density-functional description.

PubMed

Dale, Stephen G; Johnson, Erin R

2017-10-18

The two-dimensional (2D) electrides are a highly unusual class of materials, possessing interstitial electron layers sandwiched between cationic atomic layers of the solid. In this work, density-functional theory, with the exchange-hole dipole moment dispersion correction, is used to investigate exfoliation and interlayer sliding of the only two experimentally known 2D electrides: [Ca 2 N] + e - and [Y 2 C] 2+ (2e - ). Examination of the valence states during exfoliation identifies intercalated electrons in the bulk and weakly-bound surface-states in the fully-expanded case. The calculated exfoliation energies for the 2D electrides are found to be much higher than for typical 2D materials, which is attributed to the ionic nature of the electrides and the strong Coulomb forces governing the interlayer interactions. Conversely, the calculated sliding barriers are found to be quite low, comparable to those for typical 2D materials, and are effectively unchanged by exclusion of dispersion. We conjecture that the metallic nature of the interstitial electrons allows the atomic layers to move relative to each other without significantly altering the interlayer binding. Finally, comparison with previous works reveals the importance of a system-dependent dispersion correction in the density-functional treatment.

Engineering New Layered Solids from Exfoliated Inorganics: a Periodically Alternating Hydrotalcite – Montmorillonite Layered Hybrid

PubMed Central

Chalasani, Rajesh; Gupta, Amit; Vasudevan, Sukumaran

2013-01-01

Two-dimensional (2D) nanosheets obtained by exfoliating inorganic layered crystals have emerged as a new class of materials with unique attributes. One of the critical challenges is to develop robust and versatile methods for creating new nanostructures from these 2D-nanosheets. Here we report the delamination of layered materials that belonging to two different classes - the cationic clay, montmorillonite, and the anionic clay, hydrotalcite - by intercalation of appropriate ionic surfactants followed by dispersion in a non-polar solvent. The solids are delaminated to single layers of atomic thickness with the ionic surfactants remaining tethered to the inorganic and consequently the nanosheets are electrically neutral. We then show that when dispersions of the two solids are mixed the exfoliated sheets self-assemble as a new layered solid with periodically alternating hydrotalcite and montmorillonite layers. The procedure outlined here is easily extended to other layered solids for creating new superstructures from 2D-nanosheets by self-assembly. PMID:24336682

Solid-state rechargeable magnesium battery

DOEpatents

Shao, Yuyan; Liu, Jun; Liu, Tianbiao; Li, Guosheng

2016-09-06

Embodiments of a solid-state electrolyte comprising magnesium borohydride, polyethylene oxide, and optionally a Group IIA or transition metal oxide are disclosed. The solid-state electrolyte may be a thin film comprising a dispersion of magnesium borohydride and magnesium oxide nanoparticles in polyethylene oxide. Rechargeable magnesium batteries including the disclosed solid-state electrolyte may have a coulombic efficiency .gtoreq.95% and exhibit cycling stability for at least 50 cycles.

Fabrication of biomimetic superhydrophobic surface using hierarchical polyaniline spheres.

PubMed

Dong, Xiaofei; Wang, Jixiao; Zhao, Yanchai; Wang, Zhi; Wang, Shichang

2011-06-01

Wettability and water-adhesion behavior are the most important properties of solid surfaces from both fundamental and practical aspects. Here, the biomimetic superhydrophobic surface was fabricated via a simple coating process using polyaniline (PANI) microspheres which is covered with PANI nanowires as functional component, and poly-vinyl butyral (PVB, poly-vinyl alcohol crosslinked with n-butylaldehyde) as PANI microsphere adhering improvement agent to the substrate. The obtained surface displays superhydrophobic behavior without any modification with low-surface-energy materials such as thiol- or fluoroalkylsilane. The effects of coating process and the content of PANI microspheres on superhydropbobic behavior were discussed. Combine contact angle, water-adhesion measurements, scanning electronic microscopy (SEM) observations with selected areas energy dispersion spectrometer (EDS), the hydrophobic mechanism was proposed. The superhydrophobicity is attributed to a hierarchical morphology of PANI microspheres and the nature of the material itself. In addition, induced by van der Waals forces, the created superhydrophobic surface here shows the strong water-adhesion behavior. The surface has the combination performance of Lotus leaf and gecko's pad. The special wettability would be of great significance to the liquid microtransport in microfluid devices. The experimental results show that the ordinary coating process is a facile approach for fabrication of superhydrophobic surfaces.

Propagation of Love waves with surface effects in an electrically-shorted piezoelectric nanofilm on a half-space elastic substrate.

PubMed

Zhang, Sijia; Gu, Bin; Zhang, Hongbin; Feng, Xi-Qiao; Pan, Rongying; Alamusi; Hu, Ning

2016-03-01

The propagation of Love waves in the structure consisting of a nanosized piezoelectric film and a semi-infinite elastic substrate is investigated in the present paper with the consideration of surface effects. In our analysis, surface effects are taken into account in terms of the surface elasticity theory and the electrically-shorted conditions are adopted on the free surface of the piezoelectric film and the interface between the film and the substrate. This work focuses on the new features in the dispersion relations of different modes due to surface effects. It is found that with the existence of surface effects, the frequency dispersion of Love waves shows the distinct dependence on the thickness and the surface constants when the film thickness reduces to nanometers. In general, phase velocities of all dispersion modes increase with the decrease of the film thickness and the increase of the surface constants. However, surface effects play different functions in the frequency dispersions of different modes, especially for the first mode dispersion. Moreover, different forms of Love waves are observed in the first mode dispersion, depending on the presence of the surface effects on the surface and the interface. Copyright © 2015 Elsevier B.V. All rights reserved.

Surface nucleation and independent growth of Ce(OH)4 within confinement space on modified carbon black surface to prepare nano-CeO2 without agglomeration

NASA Astrophysics Data System (ADS)

Zhang, Xinyue; Xia, Chunhui; Li, Kaitao; Lin, Yanjun

2018-06-01

Highly dispersed negative carboxyl groups can be formed on carbon black (CB) surface modified with strong nitric acid. Therefore positive cations can be uniformly absorbed by carboxyl groups and precipitated within a confinement space on modified CB surface to prepare highly dispersed nanomaterials. In this paper, the formation and dispersion status of surface negative carboxyl groups, adsorption status of Ce3+, surface confinement nucleation, crystallization and calcination process were studied by EDS, SEM, and laser particle size analysis. The results show that the carboxyl groups formed on modified CB surface are highly dispersed, and Ce3+ cations can be uniformly anchored by carboxyl groups. Therefore, highly dispersed Ce3+ can react with OH- within a confinement surface region to form positive nano-Ce(OH)4 nuclei which also can be adsorbed by electrostatic attraction. After independent growth of Ce(OH)4 without agglomeration, highly dispersed CeO2 nanoparticles without agglomeration can be prepared together with the help of effectively isolates by CO2 released in the combustion of CB.

Surface nucleation and independent growth of Ce(OH)4 within confinement space on modified carbon black surface to prepare nano-CeO2 without agglomeration

NASA Astrophysics Data System (ADS)

Zhang, Xinyue; Xia, Chunhui; Li, Kaitao; Lin, Yanjun

2018-04-01

Highly dispersed negative carboxyl groups can be formed on carbon black (CB) surface modified with strong nitric acid. Therefore positive cations can be uniformly absorbed by carboxyl groups and precipitated within a confinement space on modified CB surface to prepare highly dispersed nanomaterials. In this paper, the formation and dispersion status of surface negative carboxyl groups, adsorption status of Ce3+, surface confinement nucleation, crystallization and calcination process were studied by EDS, SEM, and laser particle size analysis. The results show that the carboxyl groups formed on modified CB surface are highly dispersed, and Ce3+ cations can be uniformly anchored by carboxyl groups. Therefore, highly dispersed Ce3+ can react with OH- within a confinement surface region to form positive nano-Ce(OH)4 nuclei which also can be adsorbed by electrostatic attraction. After independent growth of Ce(OH)4 without agglomeration, highly dispersed CeO2 nanoparticles without agglomeration can be prepared together with the help of effectively isolates by CO2 released in the combustion of CB.

A Preliminary Experimental Investigation of Wet Fine Erosion in Two-Phase Flow

NASA Astrophysics Data System (ADS)

Ya, H. H.; Luthfi, Haziq; Ngo, Nguyet-Tran; Hassan, Suhaimi; Pao, William

2018-03-01

Solid particles below 62 μm is classified as fine. In oil producing operation, the most commonly used downhole sand screen can only capture solid particles of 140 μm and above. Most predictive erosion model is limited to particle size of 100 μm with single phase flow assumption because it is commonly believed that erosion due to particles below 100 μm is insignificant and typically ignored by oil and gas consultants when proposing facilities design. The objective of this paper is to investigate the impact of fines particle on mild steel plate in two-phase flow at different collision angles. A two phase flow loop was set up. The average size of fine particle was 60 μm, mixed with water with sand to water ratio at 1:65 wt/wt. The mild steel plates were oriented at three different impact angles which are -30°, 30° and 90°, with respect to the horizon. Scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX), surface roughness and Vickers micro hardness techniques were used to quantify the effects of fine particle on the exposed surface.

Laser-based standoff detection of surface-bound explosive chemicals

NASA Astrophysics Data System (ADS)

Huestis, David L.; Smith, Gregory P.; Oser, Harald

2010-04-01

Avoiding or minimizing potential damage from improvised explosive devices (IEDs) such as suicide, roadside, or vehicle bombs requires that the explosive device be detected and neutralized outside its effective blast radius. Only a few seconds may be available to both identify the device as hazardous and implement a response. As discussed in a study by the National Research Council, current technology is still far from capable of meeting these objectives. Conventional nitrocarbon explosive chemicals have very low vapor pressures, and any vapors are easily dispersed in air. Many pointdetection approaches rely on collecting trace solid residues from dust particles or surfaces. Practical approaches for standoff detection are yet to be developed. For the past 5 years, SRI International has been working toward development of a novel scheme for standoff detection of explosive chemicals that uses infrared (IR) laser evaporation of surfacebound explosive followed by ultraviolet (UV) laser photofragmentation of the explosive chemical vapor, and then UV laser-induced fluorescence (LIF) of nitric oxide. This method offers the potential of long standoff range (up to 100 m or more), high sensitivity (vaporized solid), simplicity (no spectrometer or library of reference spectra), and selectivity (only nitrocompounds).

On the nanostructuring and catalytic promotion of intermediate temperature solid oxide fuel cell (IT-SOFC) cathodes

NASA Astrophysics Data System (ADS)

Serra, José M.; Buchkremer, Hans-Peter

Solid oxide fuel cells (SOFCs) are highly efficient energy converters for both stationary and mobile purposes. However, their market introduction still demands the reduction of manufacture costs and one possible way to reach this goal is the decrease of the operating temperatures, which entails the improvement of the cathode electrocatalytic properties. An ideal cathode material may have mixed ionic and electronic conductivity as well as proper catalytic properties. Nanostructuring and catalytic promotion of mixed conducting perovskites (e.g. La 0.58Sr 0.4Fe 0.8Co 0.2O 3- δ) seem to be promising approaches to overcoming cathode polarization problems and are briefly illustrated here. The preparation of nanostructured cathodes with relatively high surface area and enough thermal stability enables to improve the oxygen exchange rate and therefore the overall SOFC performance. A similar effect was obtained by catalytic promoting the perovskite surface, allowing decoupling the catalytic and ionic-transport properties in the cathode design. Noble metal incorporation may improve the reversibility of the reduction cycles involved in the oxygen reduction. Under the cathode oxidizing conditions, Pd seems to be partially dissolved in the perovskite structure and as a result very well dispersed.

Investigation of aluminosilicate as a solid oxide fuel cell refractory

NASA Astrophysics Data System (ADS)

Gentile, Paul S.; Sofie, Stephen W.

2011-05-01

Aluminosilicate represents a potential low cost alternative to alumina for solid oxide fuel cell (SOFC) refractory applications. The objectives of this investigation are to study: (1) changes of aluminosilicate chemistry and morphology under SOFC conditions, (2) deposition of aluminosilicate vapors on yttria stabilized zirconia (YSZ) and nickel, and (3) effects of aluminosilicate vapors on SOFC electrochemical performance. Thermal treatment of aluminosilicate under high temperature SOFC conditions is shown to result in increased mullite concentrations at the surface due to diffusion of silicon from the bulk. Water vapor accelerates the rate of surface diffusion resulting in a more uniform distribution of silicon. The high temperature condensation of volatile gases released from aluminosilicate preferentially deposit on YSZ rather than nickel. Silicon vapor deposited on YSZ consists primarily of aluminum rich clusters enclosed in an amorphous siliceous layer. Increased concentrations of silicon are observed in enlarged grain boundaries indicating separation of YSZ grains by insulating glassy phase. The presence of aluminosilicate powder in the hot zone of a fuel line supplying humidified hydrogen to an SOFC anode impeded peak performance and accelerated degradation. Energy dispersive X-ray spectroscopy detected concentrations of silicon at the interface between the electrolyte and anode interlayer above impurity levels.

Carbon fiber brush electrode as a novel substrate for atmospheric solids analysis probe (ASAP) mass spectrometry: Electrochemical oxidation of brominated phenols.

PubMed

Skopalová, Jana; Barták, Petr; Bednář, Petr; Tomková, Hana; Ingr, Tomáš; Lorencová, Iveta; Kučerová, Pavla; Papoušek, Roman; Borovcová, Lucie; Lemr, Karel

2018-01-25

A carbon fiber brush electrode (CFBE) was newly designed and used as a substrate for both controlled potential electrolysis and atmospheric solids analysis probe (ASAP) mass spectrometry. Electropolymerized and strongly adsorbed products of electrolysis were directly desorbed and ionized from the electrode surface. Electrochemical properties of the electrode investigated by cyclic voltammetry revealed large electroactive surface area (23 ± 3 cm 2 ) at 1.3 cm long array of carbon fibers with diameter 6-9 μm. Some products of electrochemical oxidation of pentabromophenol and 2,4,6-tribromophenol formed a compact layer on the carbon fibers and were analyzed using ASAP. Eleven new oligomeric products were identified including quinones and biphenoquinones. These compounds were not observed previously in electrolyzed solutions by liquid or gas chromatography/mass spectrometry. The thickness around 58 nm and 45 nm of the oxidation products layers deposited on carbon fibers during electrolysis of pentabromophenol and 2,4,6-tribromophenol, respectively, was estimated from atomic force microscopy analysis and confirmed by scanning electron microscopy with energy-dispersive X-ray spectroscopy measurements. Copyright © 2017 Elsevier B.V. All rights reserved.