Transformation of eutectic emulsion to nanosuspension fabricating with solvent evaporation and ultrasonication technique

PubMed Central

Phaechamud, Thawatchai; Tuntarawongsa, Sarun

2016-01-01

Eutectic solvent can solubilize high amount of some therapeutic compounds. Volatile eutectic solvent is interesting to be used as solvent in the preparation of nanosuspension with emulsion solvent evaporation technique. The mechanism of transformation from the eutectic emulsion to nanosuspension was investigated in this study. The 30% w/w ibuprofen eutectic solution was used as the internal phase, and the external phase is composed of Tween 80 as emulsifier. Ibuprofen nanosuspension was prepared by eutectic emulsion solvent evaporating method followed with ultrasonication. During evaporation process, the ibuprofen concentration in emulsion droplets was increased leading to a drug supersaturation but did not immediately recrystallize because of low glass transition temperature (Tg) of ibuprofen. The contact angle of the internal phase on ibuprofen was apparently lower than that of the external phase at all times of evaporation, indicating that the ibuprofen crystals were preferentially wetted by the internal phase than the external phase. From calculated dewetting value ibuprofen crystallization occurred in the droplet. Crystallization of the drug was initiated with external mechanical force, and the particle size of the drug was larger due to Ostwald ripening. Cavitation force from ultrasonication minimized the ibuprofen crystals to the nanoscale. Particle size and zeta potential of formulated ibuprofen nanosuspension were 330.87±51.49 nm and −31.1±1.6 mV, respectively, and exhibited a fast dissolution. Therefore, the combination of eutectic emulsion solvent evaporation method with ultrasonication was favorable for fabricating an ibuprofen nanosuspension, and the transformation mechanism was attained successfully. PMID:27366064

Transformation of eutectic emulsion to nanosuspension fabricating with solvent evaporation and ultrasonication technique.

PubMed

Phaechamud, Thawatchai; Tuntarawongsa, Sarun

2016-01-01

Eutectic solvent can solubilize high amount of some therapeutic compounds. Volatile eutectic solvent is interesting to be used as solvent in the preparation of nanosuspension with emulsion solvent evaporation technique. The mechanism of transformation from the eutectic emulsion to nanosuspension was investigated in this study. The 30% w/w ibuprofen eutectic solution was used as the internal phase, and the external phase is composed of Tween 80 as emulsifier. Ibuprofen nanosuspension was prepared by eutectic emulsion solvent evaporating method followed with ultrasonication. During evaporation process, the ibuprofen concentration in emulsion droplets was increased leading to a drug supersaturation but did not immediately recrystallize because of low glass transition temperature (T g) of ibuprofen. The contact angle of the internal phase on ibuprofen was apparently lower than that of the external phase at all times of evaporation, indicating that the ibuprofen crystals were preferentially wetted by the internal phase than the external phase. From calculated dewetting value ibuprofen crystallization occurred in the droplet. Crystallization of the drug was initiated with external mechanical force, and the particle size of the drug was larger due to Ostwald ripening. Cavitation force from ultrasonication minimized the ibuprofen crystals to the nanoscale. Particle size and zeta potential of formulated ibuprofen nanosuspension were 330.87±51.49 nm and -31.1±1.6 mV, respectively, and exhibited a fast dissolution. Therefore, the combination of eutectic emulsion solvent evaporation method with ultrasonication was favorable for fabricating an ibuprofen nanosuspension, and the transformation mechanism was attained successfully.

Laboratory comparison of solvent-loaded and solvent-free emulsions

DOT National Transportation Integrated Search

2000-09-01

Asphalt emulsions have been widely used in highway construction and maintenance since the 1920s, initially as dust palliatives and spray applications. More recently, they have been used in more diverse paving applications such as base and surface cou...

Controlled assembly of nanoparticle structures: spherical and toroidal superlattices and nanoparticle-coated polymeric beads.

PubMed

Isojima, Tatsushi; Suh, Su Kyung; Vander Sande, John B; Hatton, T Alan

2009-07-21

The emulsion droplet solvent evaporation method has been used to prepare nanoclusters of monodisperse magnetite nanoparticles of varying morphologies depending on the temperature and rate of solvent evaporation and on the composition (solvent, presence of polymer, nanoparticle concentration, etc.) of the emulsion droplets. In the absence of a polymer, and with increasing solvent evaporation temperatures, the nanoparticles formed single- or multidomain crystalline superlattices, amorphous spherical aggregates, or toroidal clusters, as determined by the energetics and dynamics of the solvent evaporation process. When polymers that are incompatible with the nanoparticle coatings were included in the emulsion formulation, monolayer- and multilayer-coated polymer beads and partially coated Janus beads were prepared; the nanoparticles were expelled by the polymer as its concentration increased on evaporation of the solvent and accumulated on the surfaces of the beads in a well-ordered structure. The precise number of nanoparticle layers depended on the polymer/magnetic nanoparticle ratio in the oil droplet phase parent emulsion. The magnetic nanoparticle superstructures responded to the application of a modest magnetic field by forming regular chains with alignment of nonuniform structures (e.g., toroids and Janus beads) that are in accord with theoretical predictions and with observations in other systems.

Studies on the formation of polymeric nano-emulsions obtained via low-energy emulsification and their use as templates for drug delivery nanoparticle dispersions.

PubMed

Calderó, G; Montes, R; Llinàs, M; García-Celma, M J; Porras, M; Solans, C

2016-09-01

Ethylcellulose nanoparticles have been obtained from O/W nano-emulsions of the water/polyoxyethylene 10 oleyl ether/[ethyl acetate+4wt% ethylcellulose] system by low energy-energy emulsification at 25°C. Nano-emulsions with droplet sizes below 200nm and high kinetic stability were chosen for solubilising dexamethasone (DXM). Phase behaviour, conductivity and optical analysis studies of the system have evidenced for the first time that both, the polymer and the drug play a role on the structure of the aggregates formed along the emulsification path. Nano-emulsion formation may take place by both, phase inversion and self-emulsification. Spherical polymeric nanoparticles containing surfactant, showing sizes below 160nm have been obtained from the nano-emulsions by organic solvent evaporation. DXM loading in the nanoparticles was high (>90%). The release kinetics of nanoparticle dispersions with similar particle size and encapsulated DXM but different polymer to surfactant ratio were studied and compared to an aqueous DXM solution. Drug release from the nanoparticle dispersions was slower than from the aqueous solution. While the DXM solution showed a Fickian release pattern, the release behaviour from the nanoparticle dispersions was faster than that expected from a pure Fickian release. A coupled diffusion/relaxation model fitted the results very well, suggesting that polymer chains undergo conformational changes enhancing drug release. The contribution of diffusion and relaxation to drug transport in the nanoparticle dispersions depended on their composition and release time. Surfactant micelles present in the nanoparticle dispersion may exert a mild reservoir effect. The small particle size and the prolonged DXM release provided by the ethylcellulose nanoparticle dispersions make them suitable vehicles for controlled drug delivery applications. Copyright © 2016 Elsevier B.V. All rights reserved.

Polymeric nanoparticles of siRNA prepared by a double-emulsion solvent-diffusion technique: Physicochemical properties, toxicity, biodistribution and efficacy in a mammary carcinoma mice model.

PubMed

Ben David-Naim, Meital; Grad, Etty; Aizik, Gil; Nordling-David, Mirjam M; Moshel, Ofra; Granot, Zvi; Golomb, Gershon

2017-11-01

siRNA-loaded nanoparticles (NPs) administered systemically can overcome the poor stability and rapid elimination of free double-stranded RNA in circulation, resulting in increased tumor accumulation and efficacy. siRNA against osteopontin (siOPN), a protein involved in breast cancer development, was encapsulated in poly(D,L-lactic-co-glycolic acid) NPs by a double emulsion solvent diffusion (DESD) technique. We also compared the effect of polyethylenimine (PEI) molecular weight (800 Da and 25 kDa), used as the counter-ion for siRNA complexation, on the physicochemical properties of the NPs, cytotoxicity, and cellular uptake. NPs prepared by the DESD technique were obtained at the desired size (∼170 nm) using both types of PEIs, and were characterized with a neutral surface charge, high encapsulation yield (up to ∼60%), siOPN concentration of 5.6-8.4 μg/mg, stability in physiologic conditions in vitro and in vivo, and long-term shelf-life stability (> 3 years). The NPs prepared using both PEIs exhibited no cytotoxicity in primary smooth muscle culture, and no detrimental effect on mice liver enzymes following their IV administration. Following cellular uptake and biodistribution studies, the therapeutic potential of the NPs was demonstrated by a significant decrease of tumor progression and size in an ectopic xenograft model of mammary carcinoma in mice. Copyright © 2017 Elsevier Ltd. All rights reserved.

Emulsion-Based RIR-MAPLE Deposition of Conjugated Polymers: Primary Solvent Effect and Its Implications on Organic Solar Cell Performance.

PubMed

Ge, Wangyao; Li, Nan K; McCormick, Ryan D; Lichtenberg, Eli; Yingling, Yaroslava G; Stiff-Roberts, Adrienne D

2016-08-03

Emulsion-based, resonant infrared matrix-assisted pulsed laser evaporation (RIR-MAPLE) has been demonstrated as an alternative technique to deposit conjugated polymer films for photovoltaic applications; yet, a fundamental understanding of how the emulsion target characteristics translate into film properties and solar cell performance is unclear. Such understanding is crucial to enable the rational improvement of organic solar cell (OSC) efficiency and to realize the expected advantages of emulsion-based RIR-MAPLE for OSC fabrication. In this paper, the effect of the primary solvent used in the emulsion target is studied, both experimentally and theoretically, and it is found to determine the conjugated polymer cluster size in the emulsion as well as surface roughness and internal morphology of resulting polymer films. By using a primary solvent with low solubility-in-water and low vapor pressure, the surface roughness of deposited P3HT and PCPDTBT polymer films was reduced to 10 nm, and the efficiency of P3HT:PC61BM OSCs was increased to 3.2% (∼100 times higher compared to the first MAPLE OSC demonstration [ Caricato , A. P. ; Appl. Phys. Lett. 2012 , 100 , 073306 ]). This work unveils the mechanism of polymer film formation using emulsion-based RIR-MAPLE and provides insight and direction to determine the best ways to take advantage of the emulsion target approach to control film properties for different applications.

Double emulsion solvent evaporation techniques used for drug encapsulation.

PubMed

Iqbal, Muhammad; Zafar, Nadiah; Fessi, Hatem; Elaissari, Abdelhamid

2015-12-30

Double emulsions are complex systems, also called "emulsions of emulsions", in which the droplets of the dispersed phase contain one or more types of smaller dispersed droplets themselves. Double emulsions have the potential for encapsulation of both hydrophobic as well as hydrophilic drugs, cosmetics, foods and other high value products. Techniques based on double emulsions are commonly used for the encapsulation of hydrophilic molecules, which suffer from low encapsulation efficiency because of rapid drug partitioning into the external aqueous phase when using single emulsions. The main issue when using double emulsions is their production in a well-controlled manner, with homogeneous droplet size by optimizing different process variables. In this review special attention has been paid to the application of double emulsion techniques for the encapsulation of various hydrophilic and hydrophobic anticancer drugs, anti-inflammatory drugs, antibiotic drugs, proteins and amino acids and their applications in theranostics. Moreover, the optimized ratio of the different phases and other process parameters of double emulsions are discussed. Finally, the results published regarding various types of solvents, stabilizers and polymers used for the encapsulation of several active substances via double emulsion processes are reported. Copyright © 2015 Elsevier B.V. All rights reserved.

Annatto Polymeric Microparticles: Natural Product Encapsulation by the Emulsion-Solvent Evaporation Method

ERIC Educational Resources Information Center

Teixeira, Zaine; Duran, Nelson; Guterres, Silvia S.

2008-01-01

In this experiment, the extract from annatto seeds was encapsulated in poly(3-hydroxybutyrate-co-3-hydroxyvalerate) (PHBV) particles by the emulsion-solvent evaporation method. The particles were washed and centrifuged to remove excess stabilizer and then freeze-dried. The main compound of annatto seeds, bixin, has antioxidant properties as well…

[Influence of wall polymer and preparation process on the particle size and encapsulation of hemoglobin microcapsules].

PubMed

Qiu, Wei; Ma, Guang-Hui; Meng, Fan-Tao; Su, Zhi-Guo

2004-03-01

Methoxypoly (ethylene glycol)- block-poly (DL-lactide) (PELA) microcapsules containing bovine hemoglobin (BHb) were prepared by a W/O/W double emulsion-solvent diffusion process. The P50 and Hill coeffcient were 3466 Pa and 2.4 respectively, which were near to the natural bioactivity of bovine hemoglobin. The results suggested that polymer composition had significant influence on encapsulation efficiency and particle size of microcapsules. The encapsulation efficiency could reach 90% and the particle size 3 - 5 microm when the PELA copolymer containing MPEG 2000 block was used. The encapsulation efficiency and particle size increased with the concentration of PELA. Increasing the concentrations of NaCl in outer aqueous solution resulted in the increase of encapsulation efficiency and the decrease of particle size. As the concentration of stabilizer in outer aqueous solution increased in the range of 10 g/L to 20 g/L, the particle size reduced while encapsulation efficiency was increased, further increase of the stabilizer concentration would decrease encapsulation efficiency. Increasing of primary emulsion stirring rate was advantageous to the improvement of encapsulation efficiency though it had little influence on the particle size. The influence of re-emulsion stirring rate was complicated, which was not apparent in the case of large volume of re-emulsion solution. When the wall polymer and primary emulsion stirring rate were fixed, the encapsulation efficiency decreased as the particle size reduced.

Preparation of hemoglobin-loaded nano-sized particles with porous structure as oxygen carriers.

PubMed

Zhao, Jian; Liu, Chang-Sheng; Yuan, Yuan; Tao, Xin-Yi; Shan, Xiao-Qian; Sheng, Yan; Wu, Fan

2007-03-01

Hb (hemoglobin)-loaded particles (HbP) encapsulated by a biodegradable polymer used as oxygen carrier were prepared. A modified double emulsion and solvent diffusion/evaporation method was adopted. All experiments were performed based on two types of biodegradable polymers, poly(epsilon-caprolactone) (PCL) and poly(epsilon-caprolactone-ethylene glycol) (PCL-PEG). The biodistribution and the survival time in blood of the particles were investigated in a mouse model. Encapsulation efficiency and pore-connecting efficiency were evaluated by a novel sulfocyanate potassium method. The influence of process parameters on the particle size and pore-connecting efficiency (PCE%) of nanoparticles have been discussed. The prepared conditions: solvent, external aqueous phase, pressure were discussed. The system utilizing dichloromethane (DCM)/ethyl acetate (EA) as a solvent with an unsaturated external aqueous phase yielded the highest encapsulation efficiency (87.35%) with a small mean particle size (153 nm). The formation of porous channels was attributed to the diffusion of solvent. The PCE% was more sensitive to the rate of solvent diffusion that was obviously affected by the preparation temperature. The PCE% reached 87.47% when PCL-PEG was employed at 25 degrees C. P(50) of HbP was 27 mmHg, which does not seem to be greatly affected by the encapsulation procedure. In vivo, following intravenous injection of 6-coumarin labeled HbP, the major organ accumulating Hb-loaded particles was the liver. The half-life of nano-sized PCL HbP was 3.1 times as long as the micro-sized PCL HbP. Also, Nano-sized as well as a PEGylated surface on HbP is beneficial for prolonged blood residence (7.2 fold increase).

Development of eco-friendly submicron emulsions stabilized by a bio-derived gum.

PubMed

Pérez-Mosqueda, Luis María; Ramírez, Pablo; Trujillo-Cayado, Luis Alfonso; Santos, Jenifer; Muñoz, José

2014-11-01

Many traditional organic solvents are being gradually replaced by ecofriendly alternatives. D-Limonene is a terpenic (bio)-solvent that fulfils the requirements to be considered a green solvent. D-Limonene sub-micron emulsions suffer from Ostwald ripening destabilization. In this study, we examined the influence of the addition of a natural gum (rosin gum) to D-limonene in order to prevent Ostwald ripening. This contribution deals with the study of emulsions formulated with a mixture of D-limonene and rosin gum as dispersed phase and Pluronic PE9400 as emulsifier. The procedure followed for the development of these formulations was based on the application of product design principles. This led to the optimum ratio rosin gum/D-limonene and subsequently to the optimum surfactant concentration. The combination of different techniques (rheology, laser diffraction and multiple light scattering) was demonstrated to be a powerful tool to assist in the prediction of the emulsions destabilization process. Not only did the addition of rosin gum highly increase the stability of these emulsions by inhibiting the Ostwald ripening, but it also reduced the emulsions droplet size. Thus, we found that stable sub-micron D-limonene-in-water emulsions have been obtained in the range 3-6 wt% Pluronic PE-9400 by means of a single-step rotor/stator homogenizing process. Copyright © 2014 Elsevier B.V. All rights reserved.

Development of a Supported Emulsion Liquid Membrane System for Propionic Acid Separation in a Microgravity Environment

NASA Technical Reports Server (NTRS)

Li, Jin; Hu, Shih-Yao B.; Wiencek, John M.

2001-01-01

Perstractive fermentation is a good way to increase the productivity of bioreactors. Using Propionibacteria as the model system, the feasibility of using supported emulsion liquid membrane (SELM) for perstractive fermentation is assessed in this study. Five industrial solvents were considered as the solvent for preparing the SELM. The more polar a solvent is, the higher the partition coefficient. However, toxicity of a solvent also increases with its polarity. CO-1055 (industrial decanol/octanol blend) has the highest partition coefficient toward propionic acid among the solvents that has no molecular toxicity toward Propionibacteria. A preliminary extraction study was conducted using tetradecane as solvent in a hydrophobic hollow fiber contactor. The result confirmed that SELM eliminates the equilibrium limitation of conventional liquid-liquid extraction, and allows the use of a non-toxic solvent with low partition coefficient.

Preparation of non-porous microspheres with high entrapment efficiency of proteins by a (water-in-oil)-in-oil emulsion technique.

PubMed

Viswanathan, N B; Thomas, P A; Pandit, J K; Kulkarni, M G; Mashelkar, R A

1999-03-08

Emulsification-solvent removal methods have been widely used for encapsulating bioactive macromolecules like proteins and polypeptides in biodegradable polymers. We report, a (water-in-oil)-in-oil emulsion technique wherein proteins and polypeptides differing in molecular weight and shape were encapsulated in polymers of current biomedical interest. When an oil was used as the processing medium in combination with a carefully selected mixed solvent system such that a stable (w/o1/o2 emulsion is formed and solvents are removed by a combination of extraction and evaporation, the entrapment efficiency was high and the product nonporous. The entrapment efficiency of globular proteins exceeded 90% while that of fibrous proteins was around 70%. Fracture studies revealed that the polymer matrix was dense. The mechanism of entrapment involved solvent-induced precipitation of the protein as the microspheres were being formed. The principle of the method will find use in preparation of non-porous polymer microparticles with reduced burst effect.

Feasibility of Surfactant-Free Supported Emulsion Liquid Membrane Extraction

NASA Technical Reports Server (NTRS)

Hu, Shih-Yao B.; Li, Jin; Wiencek, John M.

2001-01-01

Supported emulsion liquid membrane (SELM) is an effective means to conduct liquid-liquid extraction. SELM extraction is particularly attractive for separation tasks in the microgravity environment where density difference between the solvent and the internal phase of the emulsion is inconsequential and a stable dispersion can be maintained without surfactant. In this research, dispersed two-phase flow in SELM extraction is modeled using the Lagrangian method. The results show that SELM extraction process in the microgravity environment can be simulated on earth by matching the density of the solvent and the stripping phase. Feasibility of surfactant-free SELM (SFSELM) extraction is assessed by studying the coalescence behavior of the internal phase in the absence of the surfactant. Although the contacting area between the solvent and the internal phase in SFSELM extraction is significantly less than the area provided by regular emulsion due to drop coalescence, it is comparable to the area provided by a typical hollow-fiber membrane. Thus, the stripping process is highly unlikely to become the rate-limiting step in SFSELM extraction. SFSELM remains an effective way to achieve simultaneous extraction and stripping and is able to eliminate the equilibrium limitation in the typical solvent extraction processes. The SFSELM design is similar to the supported liquid membrane design in some aspects.

Microfluidic preparation and self diffusion PFG-NMR analysis of monodisperse water-in-oil-in-water double emulsions.

PubMed

Hughes, Eric; Maan, Abid Aslam; Acquistapace, Simone; Burbidge, Adam; Johns, Michael L; Gunes, Deniz Z; Clausen, Pascal; Syrbe, Axel; Hugo, Julien; Schroen, Karin; Miralles, Vincent; Atkins, Tim; Gray, Richard; Homewood, Philip; Zick, Klaus

2013-01-01

Monodisperse water-in-oil-in-water (WOW) double emulsions have been prepared using microfluidic glass devices designed and built primarily from off the shelf components. The systems were easy to assemble and use. They were capable of producing double emulsions with an outer droplet size from 100 to 40 μm. Depending on how the devices were operated, double emulsions containing either single or multiple water droplets could be produced. Pulsed-field gradient self-diffusion NMR experiments have been performed on the monodisperse water-in-oil-in-water double emulsions to obtain information on the inner water droplet diameter and the distribution of the water in the different phases of the double emulsion. This has been achieved by applying regularization methods to the self-diffusion data. Using these methods the stability of the double emulsions to osmotic pressure imbalance has been followed by observing the change in the size of the inner water droplets over time. Copyright © 2012 Elsevier Inc. All rights reserved.

Zero-Valent Metal Emulsion for Reductive Dehalogenation of DNAPLs

NASA Technical Reports Server (NTRS)

Reinhart, Debra R. (Inventor); Clausen, Christian (Inventor); Gelger, Cherie L. (Inventor); Quinn, Jacqueline (Inventor); Brooks, Kathleen (Inventor)

2006-01-01

A zero-valent metal emulsion is used to dehalogenate solvents, such as pooled dense non-aqueous phase liquids (DNAPLs), including trichloroethylene (TCE). The zero-valent metal emulsion contains zero-valent metal particles, a surfactant, oil and water, The preferred zero-valent metal particles are nanoscale and microscale zero-valent iron particles.

Zero-Valent Metal Emulsion for Reductive Dehalogenation of DNAPLS

NASA Technical Reports Server (NTRS)

Reinhart, Debra R. (Inventor); Clausen, Christian (Inventor); Geiger, Cherie L. (Inventor); Quinn, Jacqueline (Inventor); Brooks, Kathleen (Inventor)

2003-01-01

A zero-valent metal emulsion is used to dehalogenate solvents, such as pooled dense non-aqueous phase liquids (DNAPLs), including trichloroethylene (TCE). The zero-valent metal emulsion contains zero-valent metal particles, a surfactant, oil and water. The preferred zero-valent metal particles are nanoscale and microscale zero-valent iron particles

Development of Poly(lactide-co-glicolide) Nanoparticles Incorporating Morphine Hydrochloride to Prolong its Circulation in Blood.

PubMed

Gomez-Murcia, Victoria; Montalban, Mercedes Garcia; Gomez-Fernandez, Juan C; Almela, Pilar

2017-01-01

Formulations incorporating nanoparticles (NPs) are widely used to prolong drug release. In this regard, poly(lactide-co-glicolide) (PLGA) is often used in their preparation due to its high degree of biocompatibility and biodegradability. In the present study, morphine HCl is incorporated in PLGA-NPs and different preparation alternatives are evaluated for their effects on the properties, stability and capacity of encapsulation. NPs were prepared by a double emulsion solvent diffusion-ammonium loading (DESD-AL) or double emulsion solvent diffusion-traditional (DESD-T) technique. NP morphology, size, zeta potential and encapsulation efficiency were investigated. In vitro studies were performed in phosphate buffer pH 7.4 at 37 ºC and deionized water at 4ºC. Adult male Swiss mice were used to study the pharmacokinetic behavior in vivo. Our results show that DESD-AL provides a higher level of morphine entrapment and that increasing the sonication time reduces the size but does not appreciably reduce the entrapment percentage. It was also observed that NP stability was greater when Pluronic F68 was used rather than PVA, and that in vitro assays provided better results with low concentrations of both stabilizers. Lyophilized NPs, after rehydration showed properties that were only slightly different from those of the untreated ones, with no sign of precipitation or aggregation. Finally, the obtained NPs enhanced morphine bioavailability. In conclusion, a useful method for encapsulating morphine in order to obtain an extended delivery period is described and its effects are compared with those of the free drug. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

Morphological Evolution of Block Copolymer Particles: Effect of Solvent Evaporation Rate on Particle Shape and Morphology.

PubMed

Shin, Jae Man; Kim, YongJoo; Yun, Hongseok; Yi, Gi-Ra; Kim, Bumjoon J

2017-02-28

Shape and morphology of polymeric particles are of great importance in controlling their optical properties or self-assembly into unusual superstructures. Confinement of block copolymers (BCPs) in evaporative emulsions affords particles with diverse structures, including prolate ellipsoids, onion-like spheres, oblate ellipsoids, and others. Herein, we report that the evaporation rate of solvent from emulsions encapsulating symmetric polystyrene-b-polybutadiene (PS-b-PB) determines the shape and internal nanostructure of micron-sized BCP particles. A distinct morphological transition from the ellipsoids with striped lamellae to the onion-like spheres was observed with decreasing evaporation rate. Experiments and dissipative particle dynamics (DPD) simulations showed that the evaporation rate affected the organization of BCPs at the particle surface, which determined the final shape and internal nanostructure of the particles. Differences in the solvent diffusion rates in PS and PB at rapid evaporation rates induced alignment of both domains perpendicular to the particle surface, resulting in ellipsoids with axial lamellar stripes. Slower evaporation rates provided sufficient time for BCP organization into onion-like structures with PB as the outermost layer, owing to the preferential interaction of PB with the surroundings. BCP molecular weight was found to influence the critical evaporation rate corresponding to the morphological transition from ellipsoid to onion-like particles, as well as the ellipsoid aspect ratio. DPD simulations produced morphologies similar to those obtained from experiments and thus elucidated the mechanism and driving forces responsible for the evaporation-induced assembly of BCPs into particles with well-defined shapes and morphologies.

Penetration studies of an extremely lipophilic active model substance from an oil-in-water emulsion: influence of the lipophilicity of the formulation in human skin - part 2.

PubMed

Naumann, S; Lange, S; Polak, G; Kalhoelfer, V; Motlagh, L; Goebel, A; Wohlrab, J; Neubert, R H H

2014-01-01

The effect of the lipophilicity of a carrier on human skin penetration of an extremely lipophilic active model substance was evaluated by using Franz type diffusion cells. Oil-in-water model emulsions containing different amounts of the oily phase were prepared, and Myritol® PC (M-PC) was selected as lipophilic marker component of the oily phase. The penetrated amounts of the lipophilic model substance salicyloyl phytosphingosine (SP) were determined by high-performance liquid chromatography with ultraviolet detection, while M-PC was detected using gas chromatography coupled with mass spectrometry. It has been ascertained that the amount of the lipid phase within the emulsion influenced the penetration profile of the active ingredient SP. The emulsion containing the lowest proportion of the lipid phase provides the best conditions for SP penetration. Surprisingly, the penetration behavior of M-PC was influenced by the oily phase in the same way. Regarding the M-PC and the SP penetration profiles from each emulsion, a solvent drag mechanism can be assumed whereby M-PC acts as penetration enhancer. In conclusion, the penetration rate of the active ingredient SP and the marker component M-PC are in reverse proportion to the oil content of the formulations. The lipophilicity of SP and M-PC, their solubility and their thermodynamic activity within the vehicle could have an effect on their penetration behavior. Additionally, M-PC has the property to enhance the penetration rates of extremely lipophilic substances even at low concentrations.

Preparation of Starch/Gelatin Blend Microparticles by a Water-in-Oil Emulsion Method for Controlled Release Drug Delivery.

PubMed

Phromsopha, Theeraphol; Baimark, Yodthong

2014-01-01

Information on the preparation and properties of starch/gelatin blend microparticles with and without crosslinking for drug delivery is presented. The blend microparticles were prepared by the water-in-oil emulsion solvent diffusion method. Glutaraldehyde and methylene blue were used as the crosslinker and the water-soluble drug model, respectively. The blend microparticles were characterized by scanning electron microscopy (SEM), Fourier transform infrared (FTIR) spectroscopy, and UV-Vis spectroscopy. The functional groups of the starch and gelatin blend matrices were determined from the FTIR spectra. Blend microparticles with a nearly spherical shape and internal porous structure were observed from SEM images. The average particle size of the gelatin microparticles depended on the crosslinker ratio but not on the starch/gelatin blend ratio. The in vitro drug release content significantly decreased as the crosslinker ratio increased and the starch blend ratio decreased. The results demonstrated that the starch/gelatin blend microparticles should be a useful controlled release delivery carrier for water-soluble drugs.

Preparation of Starch/Gelatin Blend Microparticles by a Water-in-Oil Emulsion Method for Controlled Release Drug Delivery

PubMed Central

Phromsopha, Theeraphol; Baimark, Yodthong

2014-01-01

Information on the preparation and properties of starch/gelatin blend microparticles with and without crosslinking for drug delivery is presented. The blend microparticles were prepared by the water-in-oil emulsion solvent diffusion method. Glutaraldehyde and methylene blue were used as the crosslinker and the water-soluble drug model, respectively. The blend microparticles were characterized by scanning electron microscopy (SEM), Fourier transform infrared (FTIR) spectroscopy, and UV-Vis spectroscopy. The functional groups of the starch and gelatin blend matrices were determined from the FTIR spectra. Blend microparticles with a nearly spherical shape and internal porous structure were observed from SEM images. The average particle size of the gelatin microparticles depended on the crosslinker ratio but not on the starch/gelatin blend ratio. The in vitro drug release content significantly decreased as the crosslinker ratio increased and the starch blend ratio decreased. The results demonstrated that the starch/gelatin blend microparticles should be a useful controlled release delivery carrier for water-soluble drugs. PMID:24868207

A New Technique for Measuring Concentration Dependence of Self and Collective Diffusivity by using a Single Sample

NASA Astrophysics Data System (ADS)

Sirorattanakul, Krittanon; Shen, Chong; Ou-Yang, Daniel

Diffusivity governs the dynamics of interacting particles suspended in a solvent. At high particle concentration, the interactions between particles become non-negligible, making the values of self and collective diffusivity diverge and concentration-dependent. Conventional methods for measuring this dependency, such as forced Rayleigh scattering, fluorescence correlation spectroscopy (FCS), and dynamic light scattering (DLS) require preparation of multiple samples. We present a new technique to measure this dependency by using only a single sample. Dielectrophoresis (DEP) is used to create concentration gradient in the solution. Across this concentration distribution, we use FCS to measure the concentration-dependent self diffusivity. Then, we switch off DEP to allow the particles to diffuse back to equilibrium. We obtain the time series of concentration distribution from fluorescence microscopy and use them to determine the concentration-dependent collective diffusivity. We compare the experimental results with computer simulations to verify the validity of this technique. Time and spatial resolution limits of FCS and imaging are also analyzed to estimate the limitation of the proposed technique. NSF DMR-0923299, Lehigh College of Arts and Sciences Undergraduate Research Grant, Lehigh Department of Physics, Emulsion Polymers Institute.

Implementation of quality by design principles in the development of microsponges as drug delivery carriers: Identification and optimization of critical factors using multivariate statistical analyses and design of experiments studies.

PubMed

Simonoska Crcarevska, Maja; Dimitrovska, Aneta; Sibinovska, Nadica; Mladenovska, Kristina; Slavevska Raicki, Renata; Glavas Dodov, Marija

2015-07-15

Microsponges drug delivery system (MDDC) was prepared by double emulsion-solvent-diffusion technique using rotor-stator homogenization. Quality by design (QbD) concept was implemented for the development of MDDC with potential to be incorporated into semisolid dosage form (gel). Quality target product profile (QTPP) and critical quality attributes (CQA) were defined and identified, accordingly. Critical material attributes (CMA) and Critical process parameters (CPP) were identified using quality risk management (QRM) tool, failure mode, effects and criticality analysis (FMECA). CMA and CPP were identified based on results obtained from principal component analysis (PCA-X&Y) and partial least squares (PLS) statistical analysis along with literature data, product and process knowledge and understanding. FMECA identified amount of ethylcellulose, chitosan, acetone, dichloromethane, span 80, tween 80 and water ratio in primary/multiple emulsions as CMA and rotation speed and stirrer type used for organic solvent removal as CPP. The relationship between identified CPP and particle size as CQA was described in the design space using design of experiments - one-factor response surface method. Obtained results from statistically designed experiments enabled establishment of mathematical models and equations that were used for detailed characterization of influence of identified CPP upon MDDC particle size and particle size distribution and their subsequent optimization. Copyright © 2015 Elsevier B.V. All rights reserved.

PHEA-PLA biocompatible nanoparticles by technique of solvent evaporation from multiple emulsions.

PubMed

Cavallaro, Gennara; Craparo, Emanuela Fabiola; Sardo, Carla; Lamberti, Gaetano; Barba, Anna Angela; Dalmoro, Annalisa

2015-11-30

Nanocarriers of amphiphilic polymeric materials represent versatile delivery systems for poorly water soluble drugs. In this work the technique of solvent evaporation from multiple emulsions was applied to produce nanovectors based on new amphiphilic copolymer, the α,β-poly(N-2-hydroxyethyl)-DL-aspartamide-polylactic acid (PHEA-PLA), purposely synthesized to be used in the controlled release of active molecules poorly soluble in water. To this aim an amphiphilic derivative of PHEA, a hydrophilic polymer, was synthesized by derivatization of the polymeric backbone with hydrophobic grafts of polylactic acid (PLA). The achieved copolymer was thus used to produce nanoparticles loaded with α tocopherol (vitamin E) adopted as lipophilic model molecule. Applying a protocol based on solvent evaporation from multiple emulsions assisted by ultrasonic energy and optimizing the emulsification process (solvent selection/separation stages), PHEA-PLA nanostructured particles with total α tocopherol entrapment efficiency (100%), were obtained. The drug release is expected to take place in lower times with respect to PLA due to the presence of the hydrophilic PHEA, therefore the produced nanoparticles can be used for semi-long term release drug delivery systems. Copyright © 2015 Elsevier B.V. All rights reserved.

Creating nanoscale emulsions using condensation.

PubMed

Guha, Ingrid F; Anand, Sushant; Varanasi, Kripa K

2017-11-08

Nanoscale emulsions are essential components in numerous products, ranging from processed foods to novel drug delivery systems. Existing emulsification methods rely either on the breakup of larger droplets or solvent exchange/inversion. Here we report a simple, scalable method of creating nanoscale water-in-oil emulsions by condensing water vapor onto a subcooled oil-surfactant solution. Our technique enables a bottom-up approach to forming small-scale emulsions. Nanoscale water droplets nucleate at the oil/air interface and spontaneously disperse within the oil, due to the spreading dynamics of oil on water. Oil-soluble surfactants stabilize the resulting emulsions. We find that the oil-surfactant concentration controls the spreading behavior of oil on water, as well as the peak size, polydispersity, and stability of the resulting emulsions. Using condensation, we form emulsions with peak radii around 100 nm and polydispersities around 10%. This emulsion formation technique may open different routes to creating emulsions, colloidal systems, and emulsion-based materials.

Continuous shear rheometry of o/w emulsions; control of evaporation in cone/plate geometry.

PubMed

Orafidiya, L O

1989-05-01

Volatile solvents may evaporate during cone/plate viscometry so that false rheograms develop. This surface evaporation was prevented in a cod-liver oil-in-water emulsion stabilized with zanthoxylum gum by layering a film of cod-liver oil on the exposed surface of the emulsion test sample. The oil layer effectively prevented evaporation and did not alter significantly the rheological behaviour of the test material.

Effect of formulation and processing variables on the characteristics of microspheres for water-soluble drugs prepared by w/o/o double emulsion solvent diffusion method.

PubMed

Lee, J; Park, T G; Choi, H

2000-02-25

80% except for acetaminophen, due to its lower solubility in water and higher solubility in corn oil. The release profile of the drug was pH dependent. In acidic medium, the release rate was much slower, however, the drug was released quickly at pH 7.4. Tacrine showed unexpected release profiles, probably due to ionic interaction with polymer matrix and the shell structure and the highest release rate was obtained at pH 2.0. The prepared microspheres had a sponge-like inner structure with or without central hollow core and the surface was dense with no apparent pores.

Effect of molecular exchange on water droplet size analysis as determined by diffusion NMR: The W/O/W double emulsion case.

PubMed

Vermeir, Lien; Sabatino, Paolo; Balcaen, Mathieu; Declerck, Arnout; Dewettinck, Koen; Martins, José C; Guthausen, Gisela; Van der Meeren, Paul

2016-08-01

The accuracy of the inner water droplet size determination of W/O/W emulsions upon water diffusion measurement by diffusion NMR was evaluated. The resulting droplet size data were compared to the results acquired from the diffusion measurement of a highly water soluble marker compound with low permeability in the oil layer of a W/O/W emulsion, which provide a closer representation of the actual droplet size. Differences in droplet size data obtained from water and the marker were ascribed to extra-droplet water diffusion. The diffusion data of the tetramethylammonium cation marker were measured using high-resolution pulsed field gradient NMR, whereas the water diffusion was measured using both low-resolution and high-resolution NMR. Different data analysis procedures were evaluated to correct for the effect of extra-droplet water diffusion on the accuracy of water droplet size analysis. Using the water diffusion data, the use of a low measurement temperature and diffusion delay Δ could reduce the droplet size overestimation resulting from extra-droplet water diffusion, but this undesirable effect was inevitable. Detailed analysis of the diffusion data revealed that the extra-droplet diffusion effect was due to an exchange between the inner water phase and the oil phase, rather than by exchange between the internal and external aqueous phase. A promising data analysis procedure for retrieving reliable size data consisted of the application of Einstein's diffusion law to the experimentally determined diffusion distances. This simple procedure allowed determining the inner water droplet size of W/O/W emulsions upon measurement of water diffusion by low-resolution NMR at or even above room temperature. Copyright © 2016 Elsevier Inc. All rights reserved.

Pickering-type water-in-oil-in-water multiple emulsions toward multihollow nanocomposite microspheres.

PubMed

Maeda, Hayata; Okada, Masahiro; Fujii, Syuji; Nakamura, Yoshinobu; Furuzono, Tsutomu

2010-09-07

Multihollow hydroxyapatite (HAp)/poly(L-lactic acid) (PLLA) nanocomposite microspheres were readily fabricated by solvent evaporation from a "Pickering-type" water-in-(dichloromethane solution of PLLA)-in-water multiple emulsion stabilized with HAp nanoparticles. The multiple emulsion was stabilized with the aid of PLLA molecules used as a wettability modifier for HAp nanoparticles, although HAp nanoparticles did not work solely as particulate emulsifiers for Pickering-type emulsions consisting of pure dichloromethane and water. The interaction between PLLA and HAp nanoparticles at the oil-water interfaces plays a crucial role toward the preparation of stable multiple emulsion and multihollow microspheres.

One-step production of multiple emulsions: microfluidic, polymer-stabilized and particle-stabilized approaches.

PubMed

Clegg, Paul S; Tavacoli, Joe W; Wilde, Pete J

2016-01-28

Multiple emulsions have great potential for application in food science as a means to reduce fat content or for controlled encapsulation and release of actives. However, neither production nor stability is straightforward. Typically, multiple emulsions are prepared via two emulsification steps and a variety of approaches have been deployed to give long-term stability. It is well known that multiple emulsions can be prepared in a single step by harnessing emulsion inversion, although the resulting emulsions are usually short lived. Recently, several contrasting methods have been demonstrated which give rise to stable multiple emulsions via one-step production processes. Here we review the current state of microfluidic, polymer-stabilized and particle-stabilized approaches; these rely on phase separation, the role of electrolyte and the trapping of solvent with particles respectively.

Versatile Methodology to Encapsulate Gold Nanoparticles in PLGA Nanoparticles Obtained by Nano-Emulsion Templating.

PubMed

Fornaguera, Cristina; Feiner-Gracia, Natàlia; Dols-Perez, Aurora; García-Celma, Maria José; Solans, Conxita

2017-05-01

Gold nanoparticles have been proved useful for many biomedical applications, specifically, for their use as advanced imaging systems. However, they usually present problems related with stability and toxicity. In the present work, gold-nanoparticles have been encapsulated in polymeric nanoparticles using a novel methodology based on nano-emulsion templating. Firstly, gold nanoparticles have been transferred from water to ethyl acetate, a solvent classified as class III by the NIH guidelines (low toxic potential). Next, the formation of nano-emulsions loaded with gold nanoparticles has been performed using a low-energy, the phase inversion composition (PIC) emulsification method, followed by solvent evaporation giving rise to polymeric nanoparticles. Using this methodology, high concentrations of gold nanoparticles (>100 pM) have been encapsulated. Increasing gold nanoparticle concentration, nano-emulsion and nanoparticle sizes increase, resulting in a decrease on the stability. It is noteworthy that the designed nanoparticles did not produce cytotoxicity neither hemolysis at the required concentration. Therefore, it can be concluded that a novel and very versatile methodology has been developed for the production of polymeric nanoparticles loaded with gold nanoparticles. Graphical Abstract Schematic representation of AuNP-loaded polymeric nanoparticles preparation from nano-emulsion templating.

Water with low concentration of surfactant in dispersed solvent-assisted emulsion dispersive liquid-liquid microextraction for the determination of fungicides in wine.

PubMed

Tseng, Wan-Chi; Chu, Shang-Ping; Kong, Po-Hsin; Huang, Chun-Kai; Chen, Jung-Hsuan; Chen, Pai-Shan; Huang, Shang-Da

2014-09-17

A sample preparation method, dispersive liquid-liquid microextraction assisted by an emulsion with low concentration of a surfactant in water and dispersed solvent coupled with gas chromatography-mass spectrometry, was developed for the analysis of the fungicides cyprodinil, procymidone, fludioxonil, flusilazole, benalaxyl, and tebuconazole in wine. A microsyringe was used to withdraw and discharge a mixture of extraction solvent and 240 μL of an aqueous solution of Triton X-100 (the dispersed agent) four times within 10 s to form a cloudy emulsion in the syringe. This emulsion was then injected into a 5 mL wine sample spiked with all of the above fungicides. The total extraction time was approximately 0.5 min. Under optimum conditions using 1-octanol (12 μL) as extraction solvent, the linear range of the method in analysis of all six fungicides was 0.05-100 μg L(-1), and the limit of detection ranged from 0.013 to 0.155 μg L(-1). The absolute recoveries (n = 3) and relative recoveries (n = 3) were 30-83 and 81-108% for white wine at 0.5, 5, and 5 μg L(-1), and 30-92 and 81-110% for red wine, respectively. The intraday (n = 7) and interday (n = 6) relative standard deviations ranged from 4.4 to 8.8% and from 4.3 to 11.2% at 0.5 μg L(-1), respectively. The method achieved high enrichment factors. It is an alternative sample preparation technique with good performance.

Emulsified Zero-Valent Nano-Scale Iron Treatment of Chlorinated Solvent DNAPL Source Areas

DTIC Science & Technology

2010-04-01

The EZVI is composed of food-grade surfactant, biodegradable oil , water, and ZVI particles (either nano- or micro-scale iron), which form...emulsion particles (Figure 2-1). Each emulsion particle or droplet contains ZVI particles in water surrounded by an oil -liquid membrane. Since the...exterior oil membrane of the emulsion droplet has hydrophobic properties similar to that of DNAPL, the droplets are miscible with DNAPL. It is believed

Calixarene cleansing formulation for uranium skin contamination.

PubMed

Phan, Guillaume; Semili, Naïma; Bouvier-Capely, Céline; Landon, Géraldine; Mekhloufi, Ghozlene; Huang, Nicolas; Rebière, François; Agarande, Michelle; Fattal, Elias

2013-10-01

An oil-in-water cleansing emulsion containing calixarene molecule, an actinide specific chelating agent, was formulated in order to improve the decontamination of uranium from the skin. Commonly commercialized cosmetic ingredients such as surfactants, mineral oil, or viscosifying agents were used in preparing the calixarene emulsion. The formulation was characterized in terms of size and apparent viscosity measurements and then was tested for its ability to limit uranyl ion permeation through excoriated pig-ear skin explants in 24-h penetration studies. Calixarene emulsion effectiveness was compared with two other reference treatments consisting of DTPA and EHBP solutions. Application of calixarene emulsion induced the highest decontamination effect with an 87% decrease in uranium diffusion flux. By contrast, EHBP and DTPA solutions only allowed a 50% and 55% reduction of uranium permeation, respectively, and had the same effect as a simple dilution of the contamination by pure water. Uranium diffusion decrease was attributed to uranyl ion-specific chelation by calixarene within the formulation, since no significant effect was obtained after application of the same emulsion without calixarene. Thus, calixarene cleansing emulsion could be considered as a promising treatment in case of accidental contamination of the skin by highly diffusible uranium compounds.

Design and evaluation of a novel nanoparticulate-based formulation encapsulating a HIP complex of lysozyme.

PubMed

Gaudana, Ripal; Gokulgandhi, Mitan; Khurana, Varun; Kwatra, Deep; Mitra, Ashim K

2013-01-01

Formulation development of protein therapeutics using polymeric nanoparticles has found very little success in recent years. Major formulation challenges include rapid denaturation, susceptibility to lose bioactivity in presence of organic solvents and poor encapsulation in polymeric matrix. In the present study, we have prepared hydrophobic ion pairing (HIP) complex of lysozyme, a model protein, using dextran sulfate (DS) as a complexing polymer. We have optimized the process of formation and dissociation of HIP complex between lysozyme and DS. The effect of HIP complexation on enzymatic activity of lysozyme was also studied. Nanoparticles were prepared and characterized using spontaneous emulsion solvent diffusion method. Furthermore, we have also investigated release of lysozyme from nanoparticles along with its enzymatic activity. Results of this study indicate that nanoparticles can sustain the release of lysozyme without compromising its enzymatic activity. HIP complexation using a polymer may also be employed to formulate sustained release dosage forms of other macromolecules with enhanced encapsulation efficiency.

Factors influencing the stability and type of hydroxyapatite stabilized Pickering emulsion.

PubMed

Zhang, Ming; Wang, Ai-Juan; Li, Jun-Ming; Song, Na; Song, Yang; He, Rui

2017-01-01

Hydroxyapatite (HAp) nanoparticle stabilized Pickering emulsion was fabricated with poly(l-lactic acid) dissolved in dichloromethane (CH 2 Cl 2 ) solution as oil phase and HAp aqueous dispersion as aqueous phase. Pickering emulsion was cured via in situ solvent evaporation method. Effect of PLLA concentrations, pH value, HAp concentrations, oil-water ratio, emulsification rates and times were studied on emulsion stability and emulsion type, etc. The results indicated emulsion stability increased with the increase of HAp concentration, emulsification rate and time; it is very stable when pH value of aqueous phase was adjusted to 10. Stable W/O and O/W emulsions were fabricated successfully using as-received HAp particles as stabilizer by adjusting the fabricating parameters. The interaction between HAp and PLLA played an important role to stabilize Pickering emulsions. SEM results indicated that both microsphere and porous materials were fabricated using emulsion stabilized by unmodified HAp nanoparticles, implying that both W/O and O/W emulsion type were obtained. Copyright © 2016 Elsevier B.V. All rights reserved.

Polymer/Pristine graphene based composites: from emulsions to strong, electrically conducting foams

DOE PAGES

Woltornist, Steven J.; Carrillo, Jan-Michael Y.; Xu, Thomas O.; ...

2015-01-21

The unique electrical, thermal, and mechanical properties of graphene make it a perfect candidate for applications in graphene/graphite based polymer composites, yet challenges due to the lack of solubility of pristine graphene/graphite in water and common organic solvents have limited its practical utilization. In this paper, we report a scalable and environmentally friendly technique to form water-in-oil type emulsions stabilized by overlapping pristine graphene sheets, enabling the synthesis of open cell foams containing a continuous graphitic network. Our approach utilizes the insolubility of graphene/graphite in both water and organic solvents and so does not require oxidation, reduction, surfactants, high boilingmore » solvents, chemical functionalization, or the input of large amounts of mechanical energy or heat. At the heart of our technique is the strong attraction of graphene to high-energy oil and water interfaces. This allows for the creation of stable water-in-oil emulsions with controlled droplet size and overlapping graphene sheets playing the role of surfactant by covering the droplet surface and stabilizing the interfaces with a thin graphitic skin. Finally, these emulsions are used as templates for the synthesis of open cell foams with densities below 0.35 g/cm 3 that exhibit remarkable mechanical and electrical properties including compressive moduli up to ~100 MPa, compressive strengths of over 8.3 MPa (1200 psi), and bulk conductivities approaching 7 S/m.« less

Water-in-oil Pickering emulsions stabilized by stearoylated microcrystalline cellulose.

PubMed

Pang, Bo; Liu, Huan; Liu, Peiwen; Peng, Xinwen; Zhang, Kai

2018-03-01

Hydrophobic particles with static water contact angles larger than 90° are more like to stabilize W/O Pickering emulsions. In particular, high internal phase Pickering emulsions (HIPEs) are of great interest for diverse applications. However, W/O HIPEs have rarely been realized using sustainable biopolymers. Herein, we used stearoylated microcrystalline cellulose (SMCC) to stabilize W/O Pickering emulsions and especially, W/O HIPEs. Moreover, these W/O HIPEs can be further used as platforms for the preparation of porous materials, such as porous foams. Stearoylated microcrystalline cellulose (SMCC) was prepared by modifying MCC with stearoyl chloride under heterogeneous conditions. Using SMCC as emulsifiers, W/O medium and high internal phase Pickering emulsions (MIPEs and HIPEs) with various organic solvents as continuous phases were prepared using one-step and two-step methods, respectively. Polystyrene (PS) foams were prepared after polymerization of oil phase using HIPEs as templates and their oil/water separation capacity were studied. SMCC could efficiently stabilize W/O Pickering emulsions and HIPEs could only be prepared via the two-step method. The internal phase volume fraction of the SMCC-stabilized HIPEs reached as high as 89%. Diverse internal phase volume fractions led to distinct inner structures of foams with closed or open cells. These macroporous polystyrene (PS) foams demonstrated great potential for the effective absorption of organic solvents from underwater. Copyright © 2017 Elsevier Inc. All rights reserved.

Diffusion of Small Solute Particles in Viscous Liquids: Cage Diffusion, a Result of Decoupling of Solute-Solvent Dynamics, Leads to Amplification of Solute Diffusion.

PubMed

Acharya, Sayantan; Nandi, Manoj K; Mandal, Arkajit; Sarkar, Sucharita; Bhattacharyya, Sarika Maitra

2015-08-27

We study the diffusion of small solute particles through solvent by keeping the solute-solvent interaction repulsive and varying the solvent properties. The study involves computer simulations, development of a new model to describe diffusion of small solutes in a solvent, and also mode coupling theory (MCT) calculations. In a viscous solvent, a small solute diffuses via coupling to the solvent hydrodynamic modes and also through the transient cages formed by the solvent. The model developed can estimate the independent contributions from these two different channels of diffusion. Although the solute diffusion in all the systems shows an amplification, the degree of it increases with solvent viscosity. The model correctly predicts that when the solvent viscosity is high, the solute primarily diffuses by exploiting the solvent cages. In such a scenario the MCT diffusion performed for a static solvent provides a correct estimation of the cage diffusion.

Different magnesium release profiles from W/O/W emulsions based on crystallized oils.

PubMed

Herzi, Sameh; Essafi, Wafa

2018-01-01

Water-in-oil-in-water (W/O/W) double emulsions based on crystallized oils were prepared and the release kinetics of magnesium ions from the internal to the external aqueous phase was investigated at T=4°C, for different crystallized lipophilic matrices. All the emulsions were formulated using the same surface-active species, namely polyglycerol polyricinoleate (oil-soluble) and sodium caseinate (water-soluble). The external aqueous phase was a lactose or glucose solution at approximately the same osmotic pressure as that of the inner droplets, in order to avoid osmotic water transfer phenomena. We investigated two types of crystallized lipophilic systems: one based on blends of cocoa butter and miglyol oil, exploring a solid fat content from 0 to 90% and the other system based on milk fat fractions for which the solid fat content varies between 54 and 86%. For double emulsions based on cocoa butter/miglyol oil, the rate of magnesium release was gradually lowered by increasing the % of fat crystals i.e. cocoa butter, in agreement with a diffusion/permeation mechanism. However for double emulsions based on milk fat fractions, the rate of magnesium release was independent of the % of fat crystals and remains the one at t=0. This difference in diffusion patterns, although the solid content is of the same order, suggests a different distribution of fat crystals within the double globules: a continuous fat network acting as a physical barrier for the diffusion of magnesium for double emulsions based on cocoa butter/miglyol oil and double globule/water interfacial distribution for milk fat fractions based double emulsions, through the formation of a crystalline shell allowing an effective protection of the double globules against diffusion of magnesium to the external aqueous phase. Copyright © 2017 Elsevier Inc. All rights reserved.

Nanoscale and Microscale Iron Emulsions for Treating DNAPL

NASA Technical Reports Server (NTRS)

Geiger, Cherie L.

2002-01-01

This study demonstrated the feasibility of using emulsified nanoscale and microscale iron particles to enhance dehalogenation of (Dense Non-Aqueous Phase Liquid) DNAPL free-phase. The emulsified system consisted of a surfactant-stabilized, biodegradable oil-in-water emulsion with nanoscale or microscale iron particles contained within the emulsion droplets. It was demonstrated that DNAPLs, such as trichloroethene (TCE), diffuse through the oil membrane of the emulsion particle whereupon they reach an aqueous interior and the surface of an iron particle where dehalogenation takes place. The hydrocarbon reaction by-products of the dehalogenation reaction, primarily ethene (no chlorinated products detected), diffuse out of the emulsion droplet. This study also demonstrated that an iron-emulsion system could be delivered in-situ to the DNAPL pool in a soil matrix by using a simulated push well technique. Iron emulsions degraded pure TCE at a rate comparable to the degradation of dissolved phase TCE by iron particles, while pure iron had a very low degradation rate for free-phase TCE. The iron-emulsion systems can be injected into a sand matrix where they become immobilized and are not moved by flowing water. It has been documented that surfactant micelles possess the ability to pull pooled TCE into emulsion droplets where degradation of TCE takes place.

Particle formation in the emulsion-solvent evaporation process.

PubMed

Staff, Roland H; Schaeffel, David; Turshatov, Andrey; Donadio, Davide; Butt, Hans-Jürgen; Landfester, Katharina; Koynov, Kaloian; Crespy, Daniel

2013-10-25

The mechanism of particle formation from submicrometer emulsion droplets by solvent evaporation is revisited. A combination of dynamic light scattering, fluorescence resonance energy transfer, zeta potential measurements, and fluorescence cross-correlation spectroscopy is used to analyze the colloids during the evaporation process. It is shown that a combination of different methods yields reliable and quantitative data for describing the fate of the droplets during the process. The results indicate that coalescence plays a minor role during the process; the relatively large size distribution of the obtained polymer colloids can be explained by the droplet distribution after their formation. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Preparation and characterization of biodegradable magnetic carriers by single emulsion-solvent evaporation

NASA Astrophysics Data System (ADS)

Liu, Xianqiao; Kaminski, Michael D.; Riffle, Judy S.; Chen, Haitao; Torno, Michael; Finck, Martha R.; Taylor, LaToyia; Rosengart, Axel J.

2007-04-01

This paper describes a single emulsion-solvent evaporation protocol to prepare PEGylated biodegradable/biocompatible magnetic carriers by utilizing hydrophobic magnetite and a mixture of poly( D,L lactide-co-glycolide) (PLGA) and poly(lactic acid-block-polyethylene glycol) (PLA-PEG) (26:1 by mass) polymers. We characterized the magnetic microspheres in terms of morphology, composite microstructure, size and size distribution, and magnetic properties. Results show that the preparation produces magnetic microspheres with a good spherical morphology, small size (mean diameter of 1.2-1.5 μm) by means of large size distributions, and magnetizations up to 20-30 emu/g of microspheres.

Computation of shear-induced collective-diffusivity in emulsions

NASA Astrophysics Data System (ADS)

Malipeddi, Abhilash Reddy; Sarkar, Kausik

2017-11-01

The shear-induced collective-diffusivity of drops in an emulsion is calculated through simulation. A front-tracking finite difference method is used to integrate the Navier-Stokes equations. When a cloud of drops is subjected to shear flow, after a certain time, the width of the cloud increases with the 1/3 power of time. This scaling of drop-cloud-width with time is characteristic of (sub-)diffusion that arises from irreversible two-drop interactions. The collective diffusivity is calculated from this relationship. A feature of the procedure adopted here is the modest computational requirement, wherein, a few drops ( 70) in shear for short time ( 70 strain) is found to be sufficient to get a good estimate. As far as we know, collective-diffusivity has not been calculated for drops through simulation till now. The computed values match with experimental measurements reported in the literature. The diffusivity in emulsions is calculated for a range of Capillary (Ca) and Reynolds (Re) numbers. It is found to be a unimodal function of Ca , similar to self-diffusivity. A sub-linear increase of the diffusivity with Re is seen for Re < 5 . This work has been limited to a viscosity matched case.

In situ quantification of β-carotene partitioning in oil-in-water emulsions by confocal Raman microscopy.

PubMed

Wan Mohamad, W A Fahmi; Buckow, Roman; Augustin, MaryAnn; McNaughton, Don

2017-10-15

Confocal Raman microscopy (CRM) was able to quantify the β-carotene concentration in oil droplets and determine the partitioning characteristics of β-carotene within the emulsion system in situ. The results were validated by a conventional method involving solvent extraction of β-carotene separately from the total emulsion as well as the aqueous phase separated by centrifugation, and quantification by absorption spectrophotometry. CRM also enabled the localization of β-carotene in an emulsion. From the Raman image, the β-carotene partitioning between the aqueous and oil phases of palm olein-in-water emulsions stabilized by whey protein isolate (WPI) was observed. Increasing the concentration of β-carotene in an emulsion (from 0.1 to 0.3g/kg emulsion) with a fixed gross composition (10% palm olein:2% WPI) decreased the concentration of β-carotene in the oil droplet. CRM is a powerful tool for in situ analyses of components in heterogeneous systems such as emulsions. Copyright © 2017 Elsevier Ltd. All rights reserved.

Optimization of perfluoro nano-scale emulsions: the importance of particle size for enhanced oxygen transfer in biomedical applications.

PubMed

Fraker, Christopher A; Mendez, Armando J; Inverardi, Luca; Ricordi, Camillo; Stabler, Cherie L

2012-10-01

Nano-scale emulsification has long been utilized by the food and cosmetics industry to maximize material delivery through increased surface area to volume ratios. More recently, these methods have been employed in the area of biomedical research to enhance and control the delivery of desired agents, as in perfluorocarbon emulsions for oxygen delivery. In this work, we evaluate critical factors for the optimization of PFC emulsions for use in cell-based applications. Cytotoxicity screening revealed minimal cytotoxicity of components, with the exception of one perfluorocarbon utilized for emulsion manufacture, perfluorooctylbromide (PFOB), and specific w% limitations of PEG-based surfactants utilized. We optimized the manufacture of stable nano-scale emulsions via evaluation of: component materials, emulsification time and pressure, and resulting particle size and temporal stability. The initial emulsion size was greatly dependent upon the emulsion surfactant tested, with pluronics providing the smallest size. Temporal stability of the nano-scale emulsions was directly related to the perfluorocarbon utilized, with perfluorotributylamine, FC-43, providing a highly stable emulsion, while perfluorodecalin, PFD, coalesced over time. The oxygen mass transfer, or diffusive permeability, of the resulting emulsions was also characterized. Our studies found particle size to be the critical factor affecting oxygen mass transfer, as increased micelle size resulted in reduced oxygen diffusion. Overall, this work demonstrates the importance of accurate characterization of emulsification parameters in order to generate stable, reproducible emulsions with the desired bio-delivery properties. Copyright © 2012 Elsevier B.V. All rights reserved.

Formation of random and regular relief-phase structures on silver halide photographic emulsions by holographic methods

NASA Astrophysics Data System (ADS)

Ganzherli, N. M.; Gulyaev, S. N.; Gurin, A. S.; Kramushchenko, D. D.; Maurer, I. A.; Chernykh, D. F.

2009-07-01

The formation of diffusers and microlens rasters on silver halide emulsions by holographic methods is considered. Two techniques for converting amplitude holographic recording to relief-phase recording, selective curing and irradiation of the emulsion gelatin by short-wavelength UV radiation, are compared.

Self-Diffusion of Drops in a Dilute Sheared Emulsion

NASA Technical Reports Server (NTRS)

Loewenberg, Michael; Hinch, E. J.

1996-01-01

Self-diffusion coefficients that describe cross-flow migration of non-Brownian drops in a dilute sheared emulsion were obtained by trajectory calculations. A boundary integral formulation was used to describe pairwise interactions between deformable drops; interactions between undeformed drops were described with mobility functions for spherical drops. The results indicate that drops have large anisotropic self-diffusivities which depend strongly on the drop viscosity and modestly on the shear-rate. Pairwise interactions between drops in shear-flow do not appreciably promote drop breakup.

Oil-in-oil emulsions: a unique tool for the formation of polymer nanoparticles.

PubMed

Klapper, Markus; Nenov, Svetlin; Haschick, Robert; Müller, Kevin; Müllen, Klaus

2008-09-01

Polymer latex particles are nanofunctional materials with widespread applications including electronics, pharmaceuticals, photonics, cosmetics, and coatings. These materials are typically prepared using waterborne heterogeneous systems such as emulsion, miniemulsion, and suspension polymerization. However, all of these processes are limited to water-stable catalysts and monomers mainly polymerizable via radical polymerization. In this Account, we describe a method to overcome this limitation: nonaqueous emulsions can serve as a versatile tool for the synthesis of new types of polymer nanoparticles. To form these emulsions, we first needed to find two nonmiscible nonpolar/polar aprotic organic solvents. We used solvent mixtures of either DMF or acetonitrile in alkanes and carefully designed amphiphilic block and statistical copolymers, such as polyisoprene- b-poly(methyl methacrylate) (PI- b-PMMA), as additives to stabilize these emulsions. Unlike aqueous emulsions, these new emulsion systems allowed the use of water-sensitive monomers and catalysts. Although polyaddition and polycondensation reactions usually lead to a large number of side products and only to oligomers in the aqueous phase, these new conditions resulted in high-molecular-weight, defect-free polymers. Furthermore, conducting nanoparticles were produced by the iron(III)-induced synthesis of poly(ethylenedioxythiophene) (PEDOT) in an emulsion of acetonitrile in cyclohexane. Because metallocenes are sensitive to nitrile and carbonyl groups, the acetonitrile and DMF emulsions were not suitable for carrying out metallocene-catalyzed olefin polymerization. Instead, we developed a second system, which consists of alkanes dispersed in perfluoroalkanes. In this case, we designed a new amphipolar polymeric emulsifier with fluorous and aliphatic side chains to stabilize the emulsions. Such heterogeneous mixtures facilitated the catalytic polymerization of ethylene or propylene to give spherical nanoparticles of high molecular weight polyolefins. These nonaqueous systems also allow for the combination of different polymerization techniques to obtain complex architectures such as core-shell structures. Previously, such structures primarily used vinylic monomers, which greatly limited the number of polymer combinations. We have demonstrated how nonaqueous emulsions allow the use of a broad variety of hydrolyzable monomers and sensitive catalysts to yield polyester, polyurethane, polyamide, conducting polymers, and polyolefin latex particles in one step under ambient reaction conditions. This nonpolar emulsion strategy dramatically increases the chemical palette of polymers that can form nanoparticles via emulsion polymerization.

Characterization of nitric oxide-releasing microparticles for the mucosal delivery.

PubMed

Yoo, Jin-Wook; Lee, Jae-Suk; Lee, Chi H

2010-03-15

For the treatment of female sexual arousal disorder (FSAD), we developed microparticles made of PLGA containing nitric oxide (NO) donor (DETA NONOate) to efficiently deliver NO to vaginal mucosa. The NO-releasing microparticles were prepared by various emulsion methods. SEM and DSC studies were performed to examine the microparticles. The release studies were conducted under various conditions to optimize the loading dose in the microparticles. NO diffusivity through vaginal epithelial cells was evaluated and pharmacological activity of NO-releasing microparticles was examined by assessment of intracellular cGMP level in vaginal cells. Through the modified double emulsion solvent evaporation method (w/o/w(a)), the acid labile DETA NONOate was stabilized during the fabrication process and homogenous morphology and high entrapment efficiency were achieved. DETA NONOate was protected under the acidic conditions of the vagina and NO was released from the microparticles in a controlled manner. A significant amount of NO produced from DETA NONOate penetrated through the vaginal epithelial cells. The intracellular cGMP level increased with the treatment of NO-releasing microparticles in vaginal cells. These findings suggest that NO-releasing microparticles could improve the vaginal blood perfusion and open up the possibilities of novel treatment of FSAD. (c) 2009 Wiley Periodicals, Inc.

Influence of the ratio of amphiphilic copolymers used as emulsifiers on the microstructure, physical stability and rheology of α-pinene emulsions stabilized with gellan gum.

PubMed

García, Maria Carmen; Alfaro, Maria Carmen; Muñoz, José

2015-11-01

α-Pinene is a terpenic solvent whose use in the formulation of emulsions entails a double benefit from the environmental point of view since it is a green solvent, easily biodegradable, which also has certain antimicrobial properties. In this work a combination of Atlas™ G-5000 and Atlox™ 4913 amphiphilic copolymers was used to obtain O/W emulsions formulated with α-pinene and gellan gum. These emulsions may find applications related to the design of complex biotechnological systems with different uses. In order to investigate the microstructure and the physical stability of these emulsions, a combination of different techniques such as rheology, microscopy, laser diffraction and multiple light scattering turn out to be a useful methodology. The results demonstrated the need to include a minimum amount of Atlas™ G-5000 copolymer in the formulation of these emulsions to improve their stability. These results were supported by the information revealed by optical micrographs, according to which Atlas™ G-5000 is directed to the continuous medium to structure water (this surfactant is particularly effective at forming hydrogen bonds with water). On the other hand Atlox™ 4913 is preferentially adsorbed at the α-pinene-water interface, such that a high Atlox™ 4913/Atlas™ G-5000 mass ratio slows down the kinetics of coalescence as shown by multiple light scattering. However, a very low relative concentration of Atlas™ G-5000 causes creaming to become the dominant destabilization mechanism. Increasing the Atlas™ G-5000/Atlox™ 4913 mass ratio yields emulsions with enhanced viscosity and viscoelasticity. Copyright © 2015 Elsevier B.V. All rights reserved.

Development and rheological properties of ecological emulsions formulated with a biosolvent and two microbial polysaccharides.

PubMed

Trujillo-Cayado, L A; Alfaro, M C; Muñoz, J; Raymundo, A; Sousa, I

2016-05-01

The influence of gum concentration and rhamsan/welan gum ratio on rheological properties, droplet size distribution and physical stability of eco-friendly O/W emulsions stabilized by an ecological surfactant were studied in the present work. The emulsions were prepared with 30wt% α-pinene, a terpenic solvent and an ecological alternative for current volatile organic compounds. Rheological properties of emulsions showed an important dependence on the two studied variables. Flow curves were fitted to the Cross model and no synergistic effect between rhamsan and welan gums was demonstrated. Emulsions with submicron mean diameters were obtained regardless of the gum concentration or the rhamsan/welan ratio used. Multiple light scattering illustrated that creaming was practically eliminated by the incorporation of polysaccharides. The use of rhamsan and welan gums as stabilizers lead to apparent enhancements in emulsion rheology and physical stability. Copyright © 2016. Published by Elsevier B.V.

Fabrication of Janus particles composed of poly (lactic-co-glycolic) acid and hard fat using a solvent evaporation method.

PubMed

Matsumoto, Akihiro; Murao, Satoshi; Matsumoto, Michiko; Watanabe, Chie; Murakami, Masahiro

The feasibility of fabricating Janus particles based on phase separation between a hard fat and a biocompatible polymer was investigated. The solvent evaporation method used involved preparing an oil-in-water (o/w) emulsion with a mixture of poly (lactic-co-glycolic) acid (PLGA), hard fat, and an organic solvent as the oil phase and a polyvinyl alcohol aqueous solution as the water phase. The Janus particles were formed when the solvent was evaporated to obtain certain concentrations of PLGA and hard fat in the oil phase, at which phase separation was estimated to occur based on the phase diagram analysis. The hard fat hemisphere was proven to be the oil phase using a lipophilic dye Oil Red O. When the solvent evaporation process was performed maintaining a specific volume during the emulsification process; Janus particles were formed within 1.5 h. However, the formed Janus particles were destroyed by stirring for over 6 h. In contrast, a few Janus particles were formed when enough water to dissolve the oil phase solvent was added to the emulsion immediately after the emulsification process. The optimized volume of the solvent evaporation medium dominantly formed Janus particles and maintained the conformation for over 6 h with stirring. These results indicate that the formation and stability of Janus particles depend on the rate of solvent evaporation. Therefore, optimization of the solvent evaporation rate is critical to obtaining stable PLGA and hard fat Janus particles.

3D confocal Raman imaging of oil-rich emulsion from enzyme-assisted aqueous extraction of extruded soybean powder.

PubMed

Wu, Longkun; Wang, Limin; Qi, Baokun; Zhang, Xiaonan; Chen, Fusheng; Li, Yang; Sui, Xiaonan; Jiang, Lianzhou

2018-05-30

The understanding of the structure morphology of oil-rich emulsion from enzyme-assisted extraction processing (EAEP) was a critical step to break the oil-rich emulsion structure in order to recover oil. Albeit EAEP method has been applied as an alternative way to conventional solvent extraction method, the structure morphology of oil-rich emulsion was still unclear. The current study aimed to investigate the structure morphology of oil-rich emulsion from EAEP using 3D confocal Raman imaging technique. With increasing the enzymatic hydrolysis duration from 1 to 3 h, the stability of oil-rich emulsion was decreased as visualized in the 3D confocal Raman images that the protein and oil were mixed together. The subsequent Raman spectrum analysis further revealed that the decreased stability of oil-rich emulsion was due to the protein aggregations via SS bonds or protein-lipid interactions. The conformational transfer in protein indicated the formation of a compact structure. Copyright © 2017 Elsevier Ltd. All rights reserved.

Release behavior and kinetic evaluation of berberine hydrochloride from ethyl cellulose/chitosan microspheres

NASA Astrophysics Data System (ADS)

Zhou, Hui-Yun; Cao, Pei-Pei; Zhao, Jie; Wang, Zhi-Ying; Li, Jun-Bo; Zhang, Fa-Liang

2014-12-01

Novel ethyl cellulose/chitosan microspheres (ECCMs) were prepared by the method of w/o/w emulsion and solvent evaporation. The microspheres were spherical, adhesive, and aggregated loosely with a size not bigger than 5 μm. The drug loading efficiency of berberine hydrochloride (BH) loaded in microspheres were affected by chitosan (CS) concentration, EC concentration and the volume ratio of V(CS)/ V(EC). ECCMs prepared had sustained release efficiency on BH which was changed with different preparation parameters. In addition, the pH value of release media had obvious effect on the release character of ECCMs. The release rate of BH from sample B was only a little more than 30% in diluted hydrochloric acid (dHCl) and that was almost 90% in PBS during 24 h. Furthermore, the drug release data were fitted to different kinetic models to analyze the release kinetics and the mechanism from the microspheres. The released results of BH indicated that ECCMs exhibited non-Fickian diffusion mechanism in dHCl and diffusion-controlled drug release based on Fickian diffusion in PBS. So the ECCMs might be an ideal sustained release system especially in dHCl and the drug release was governed by both diffusion of the drug and dissolution of the polymeric network.

Continuous nanoparticle production by microfluidic-based emulsion, mixing and crystallization

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

Su, Y.-F.; Kim, H.; Kovenklioglu, S.

2007-09-15

BaSO{sub 4} and 2,2'-dipyridylamine (DPA) nanoparticles were synthesized as reactive crystallization and anti-solvent recrystallization examples, respectively, of using the microfluidic-based emulsion and mixing approach as a new avenue of continuously producing inorganic and organic nanoparticles. BaSO{sub 4} nanoparticles in the size range of 15-100 nm were reactively precipitated within the confinement of an aqueous droplet which was coalesced from two separate aqueous droplets containing BaCl{sub 2} and (NH{sub 4}){sub 2}SO{sub 4} using a three T-junction micromixer configuration constructed with commercially available simple tubing and fitting supplies. Also, DPA nanoparticles of about 200 nm were crystallized by combining DPA+ethanol and watermore » droplets using the same micromixer configuration. - Graphical abstract: BaSO{sub 4} and 2,2'-dipyridylamine (DPA) nanoparticles were synthesized as reactive crystallization and anti-solvent recrystallization examples, respectively, of using the microfluidic-based emulsion and mixing approach as a new avenue of continuously producing inorganic and organic nanoparticles.« less

Effect of the degree of substitution of octenyl succinic anhydride-banana starch on emulsion stability.

PubMed

Bello-Pérez, Luis A; Bello-Flores, Christopher A; Nuñez-Santiago, María del Carmen; Coronel-Aguilera, Claudia P; Alvarez-Ramirez, J

2015-11-05

Banana starch was esterified with octenylsuccinic anhydride (OSA) at different degree substitution (DS) and used to stabilize emulsions. Morphology, emulsion stability, emulsification index, rheological properties and particle size distribution of the emulsions were tested. Emulsions dyed with Solvent Red 26 showed affinity for the oil phase. Backscattering light showed three regions in the emulsion where the emulsified region was present. Starch concentration had higher effect in the emulsification index (EI) than the DS used in the study because similar values were found with OSA-banana and native starches. However, OSA-banana presented greater stability of the emulsified region. Rheological tests in emulsions with OSA-banana showed G'>G" values and low dependence of G' with the frequency, indicating a dominant elastic response to shear. When emulsions were prepared under high-pressure conditions, the emulsions with OSA-banana starch with different DS showed a bimodal distribution of particle size. The emulsion with OSA-banana starch and the low DS showed similar mean droplet diameter than its native counterpart. In contrast, the highest DS led to the highest mean droplet diameter. It is concluded that OSA-banana starch with DS can be used to stabilize specific emulsion types. Copyright © 2015 Elsevier Ltd. All rights reserved.

Friction and Wear Management Using Solvent Partitioning of Hydrophilic-Surface-Interactive Chemicals Contained in Boundary Layer-Targeted Emulsions

NASA Technical Reports Server (NTRS)

Richmond, Robert Chaffee (Inventor); Schramm, Jr., Harry F. (Inventor); Defalco, Francis G. (Inventor)

2015-01-01

Lubrication additives of the current invention require formation of emulsions in base lubricants, created with an aqueous salt solution plus a single-phase compound such that partitioning within the resulting emulsion provides thermodynamically targeted compounds for boundary layer organization thus establishing anti-friction and/or anti-wear. The single-phase compound is termed "boundary layer organizer", abbreviated BLO. These emulsion-contained compounds energetically favor association with tribologic surfaces in accord with the Second Law of Thermodynamics, and will organize boundary layers on those surfaces in ways specific to the chemistry of the salt and BLO additives. In this way friction modifications may be provided by BLOs targeted to boundary layers via emulsions within lubricating fluids, wherein those lubricating fluids may be water-based or oil-based.

Biomimetic DNA emulsions: specific, thermo-reversible and adjustable binding from a liquid-like DNA layer

NASA Astrophysics Data System (ADS)

Pontani, Lea-Laetitia; Feng, Lang; Dreyfus, Remi; Seeman, Nadrian; Chaikin, Paul; Brujic, Jasna

2013-03-01

We develop micron-sized emulsions coated with specific DNA sequences and complementary sticky ends. The emulsions are stabilized with phospholipids on which the DNA strands are grafted through biotin-streptavidin interactions, which allows the DNA to diffuse freely on the surface. We produce two complementary emulsions: one is functionalized with S sticky ends and dyed with red streptavidin, the other displays the complementary S' sticky ends and green streptavidin. Mixing those emulsions reveals specific adhesion between them due to the short-range S-S' hybridization. As expected this interaction is thermo-reversible: the red-green adhesive droplets dissociate upon heating and reassemble after cooling. Here the fluid phospholipids layer also leads to diffusive adhesion patches, which allows the bound droplets to rearrange throughout the packing structure. We quantify the adhesion strength between two droplets and build a theoretical framework that captures the observed trends through parameters such as the size of the droplets, the DNA surface density, the various DNA constructs or the temperature. This colloidal-scale, specific, thermo-reversible biomimetic emulsion offers a new versatile and powerful tool for the development of complex self-assembled materials.

FTIR Imaging Coupled with Multivariate Analysis for Study of Initial Diffusion of Different Solvents in Cellulose Acetate Butyrate Films

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

Lindblad, M.S.; Keyes, B.; Gedvilas, L.

Fourier transform infrared (FTIR) spectroscopic imaging was used to study the initial diffusion of different solvents in cellulose acetate butyrate (CAB) films containing different amounts of acetyl and butyryl substituents. Different solvents and solvent/non-solvent mixtures were also studied. The FTIR imaging system allowed acquisition of sequential images of the CAB films as solvent penetration proceeded without disturbing the system. The interface between the non-swollen polymer and the initial swelling front could be identified using multivariate data analysis tools. For a series of ketone solvents the initial diffusion coefficients and diffusion rates could be quantified and were found to be relatedmore » to the polar and hydrogen interaction parameters in the Hansen solubility parameters of the solvents. For the solvent/non-solvent system the initial diffusion rate decreased less than linearly with the weight-percent of non-solvent present in the solution, which probably was due to the swelling characteristic of the non-solvent. For a given solvent, increasing the butyryl content of the CAB increased the initial diffusion rate. Increasing the butyryl content from 17 wt.% butyryl to 37 wt.% butyryl produced a considerably larger increase in initial diffusion rate compared to an increase in butyryl content from 37 wt.% to 50 wt.% butyryl.« less

Preparation of surfactant-free nanoparticles of methacrylic acid copolymers used for film coating.

PubMed

Nguyen, Cung An; Konan-Kouakou, Yvette Niamien; Allémann, Eric; Doelker, Eric; Quintanar-Guerrero, David; Fessi, Hatem; Gurny, Robert

2006-07-28

The aim of the present study was to prepare surfactant-free pseudolatexes of various methacrylic acid copolymers. These aqueous colloidal dispersions of polymeric materials for oral administration are intended for film coating of solid dosage forms or for direct manufacturing of nanoparticles. Nanoparticulate dispersions were produced by an emulsification-diffusion method involving the use of partially water-miscible solvents and the mutual saturation of the aqueous and organic phases prior to the emulsification in order to reduce the initial thermodynamic instability of the emulsion. Because of the self-emulsifying properties of the methacrylic acid copolymers, it was possible to prepare aqueous dispersions of colloidal size containing up to 30% wt/vol of Eudragit RL, RS, and E using 2-butanone or methyl acetate as partially water-miscible solvents, but without any surfactant. However, in the case of the cationic Eudragit E, protonation of the tertiary amine groups by acidification of the aqueous phase was necessary to improve the emulsion stability in the absence of surfactant and subsequently to prevent droplet coalescence during evaporation. In addition, a pseudolatex of Eudragit E was used to validate the coating properties of the formulation for solid dosage forms. Film-coated tablets of quinidine sulfate showed a transparent glossy continuous film that was firmly attached to the tablet. The dissolution profile of quinidine sulfate from the tablets coated with the Eudragit E pseudolatex was comparable to that of tablets coated with an acetonic solution of Eudragit E. Furthermore, both types of coating ensured similar taste masking. The emulsification-evaporation method used was shown to be appropriate for the preparation of surfactant-free colloidal dispersions of the 3 types of preformed methacrylic acid copolymers; the dispersions can subsequently be used for film coating of solid dosage forms.

New Method to Prepare Mitomycin C Loaded PLA-Nanoparticles with High Drug Entrapment Efficiency

NASA Astrophysics Data System (ADS)

Hou, Zhenqing; Wei, Heng; Wang, Qian; Sun, Qian; Zhou, Chunxiao; Zhan, Chuanming; Tang, Xiaolong; Zhang, Qiqing

2009-07-01

The classical utilized double emulsion solvent diffusion technique for encapsulating water soluble Mitomycin C (MMC) in PLA nanoparticles suffers from low encapsulation efficiency because of the drug rapid partitioning to the external aqueous phase. In this paper, MMC loaded PLA nanoparticles were prepared by a new single emulsion solvent evaporation method, in which soybean phosphatidylcholine (SPC) was employed to improve the liposolubility of MMC by formation of MMC-SPC complex. Four main influential factors based on the results of a single-factor test, namely, PLA molecular weight, ratio of PLA to SPC (wt/wt) and MMC to SPC (wt/wt), volume ratio of oil phase to water phase, were evaluated using an orthogonal design with respect to drug entrapment efficiency. The drug release study was performed in pH 7.2 PBS at 37 °C with drug analysis using UV/vis spectrometer at 365 nm. MMC-PLA particles prepared by classical method were used as comparison. The formulated MMC-SPC-PLA nanoparticles under optimized condition are found to be relatively uniform in size (594 nm) with up to 94.8% of drug entrapment efficiency compared to 6.44 μm of PLA-MMC microparticles with 34.5% of drug entrapment efficiency. The release of MMC shows biphasic with an initial burst effect, followed by a cumulated drug release over 30 days is 50.17% for PLA-MMC-SPC nanoparticles, and 74.1% for PLA-MMC particles. The IR analysis of MMC-SPC complex shows that their high liposolubility may be attributed to some weak physical interaction between MMC and SPC during the formation of the complex. It is concluded that the new method is advantageous in terms of smaller size, lower size distribution, higher encapsulation yield, and longer sustained drug release in comparison to classical method.

Indinavir-loaded pH-sensitive microparticles for taste masking: toward extemporaneous pediatric anti-HIV/AIDS liquid formulations with improved patient compliance.

PubMed

Chiappetta, Diego A; Carcaboso, Angel M; Bregni, Carlos; Rubio, Modesto; Bramuglia, Guillermo; Sosnik, Alejandro

2009-01-01

The aim of this work was to develop indinavir pediatric anti-HIV/AIDS formulations enabling convenient dose adjustment, ease of oral administration, and improved organoleptic properties by means of the generation of drug-loaded microparticles made of a polymer that is insoluble under intake conditions and dissolves fast in the stomach in order to completely release the active agent. Indinavir-loaded microparticles made of a pH-dependent polymeric excipient soluble at pH < 5, Eudragit E100, were prepared using a double emulsion solvent diffusion technique and the in vitro release profiles characterized. Finally, taste masking properties were evaluated in blind randomized sensory experiments by ten healthy human volunteers. The use of a w/o/o emulsion system resulted in indinavir loads around 90%. Thermal analysis of the microparticles by differential scanning calorimetry revealed that indinavir appeared mainly dispersed at the molecular level. Concentrations of residual organic solvents as determined by gas chromatography were below the upper limits specified by the European Pharmacopeia for pharmaceutical oral formulations. Then, the behavior of drug-containing microparticles in aqueous media at different pH values was assessed. While they selectively dissolved in gastric-like medium, in tap water (intake conditions), the matrix remained almost unchanged and efficiently prevented drug dissolution. Finally, sensoring taste tests performed by volunteers indicated that systems with indinavir loads approximately 15% displayed acceptable taste. This work explored the production of indinavir-containing microparticles based on a common pharmaceutical excipient as a means for the improvement of medicines of drugs involved in the treatment of HIV/AIDS. For systems containing about 15% drug, taste studies confirmed the acceptability of the formulation. In pediatric regimes, this composition would require an acceptable amount of formulation (0.7-1.5 g).

Rejuvenation of Spent Media via Supported Emulsion Liquid Membranes

NASA Technical Reports Server (NTRS)

Wiencek, John M.

2002-01-01

The overall goal of this project is to maximize the reuseability of spent fermentation media. Supported emulsion liquid membrane separation, a highly efficient extraction technique, is used to remove inhibitory byproducts during fermentation; thus, improving the yield while reducing the need for fresh water. The key objectives of this study are: Develop an emulsion liquid membrane system targeting low molecular weight organic acids which has minimal toxicity on a variety of microbial systems; Conduct mass transfer studies to allow proper modeling and design of a supported emulsion liquid membrane system; Investigate the effect of gravity on emulsion coalescence within the membrane unit; Access the effect of water re-use on fermentation yields in a model microbial system; Develop a perfusion-type fermentor utilizing a supported emulsion liquid membrane system to control inhibitory fermentation byproducts; Work for the coming year will focus on the determination of toxicity of various solvents, selection of the emulsifying agents, as well as characterizing the mass transfer of hollow-fiber contactors.

Factors that affect Pickering emulsions stabilized by graphene oxide.

PubMed

He, Yongqiang; Wu, Fei; Sun, Xiying; Li, Ruqiang; Guo, Yongqin; Li, Chuanbao; Zhang, Lu; Xing, Fubao; Wang, Wei; Gao, Jianping

2013-06-12

Stable Pickering emulsions were prepared using only graphene oxide (GO) as a stabilizer, and the effects of the type of oil, the sonication time, the GO concentration, the oil/water ratio, and the pH value on the stability, type, and morphology of these emulsions were investigated. In addition, the effects of salt and the extent of GO reduction on emulsion formation and stability were studied and discussed. The average droplet size decreased with sonication time and with GO concentration, and the emulsions tended to achieve good stability at intermediate oil/water ratios and at low pH values. In all solvents, the emulsions were of the oil-in-water type, but interestingly, some water-in-oil-in-water (w/o/w) multiple emulsion droplets were also observed with low GO concentrations, low pH values, high oil/water ratios, high salt concentrations, or moderately reduced GO in the benzyl chloride-water system. A Pickering emulsion stabilized by Ag/GO was also prepared, and its catalytic performance for the reduction of 4-nitrophenol was investigated. This research paves the way for the fabrication of graphene-based functional materials with novel nanostructures and microstructures.

Topical delivery of acetyl hexapeptide-8 from different emulsions: influence of emulsion composition and internal structure.

PubMed

Hoppel, Magdalena; Reznicek, Gottfried; Kählig, Hanspeter; Kotisch, Harald; Resch, Günter P; Valenta, Claudia

2015-02-20

Acetyl hexapeptide-8 (AH-8) is a well-known component of anti-aging products and was recently explored as a promising topical treatment of blepharospasm. Although AH-8 appears in a variety of cosmetic products, its skin penetration is sparsely studied and controversially discussed. Therefore, the aim of the present study was to investigate the influence of the vehicle type on the AH-8 delivery to the skin. Besides skin permeation experiments with Franz type diffusion cells, the spatial distribution of AH-8 in the stratum corneum after a real in-use application was investigated by in vitro tape stripping on porcine ear skin. By applying LC-MS/MS for quantification of AH-8, we demonstrated that a multiple water-in-oil-in-water (W/O/W) emulsion can significantly increase penetration of AH-8 into porcine skin compared to simple O/W and W/O emulsions. The internal structure of the developed multiple emulsion was confirmed by electron microscopic investigations and NMR self diffusion studies. In general, a clear superiority of water-rich W/O/W and O/W emulsions over an oil-rich W/O emulsion in terms of dermal delivery of AH-8 was found. This enhanced delivery of AH-8 could be explained by an increased absorption of the water-rich emulsions into the skin, confirmed by combined ATR-FTIR and tape stripping experiments. Copyright © 2014 Elsevier B.V. All rights reserved.

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

Woltornist, Steven J.; Carrillo, Jan-Michael Y.; Xu, Thomas O.

The unique electrical, thermal, and mechanical properties of graphene make it a perfect candidate for applications in graphene/graphite based polymer composites, yet challenges due to the lack of solubility of pristine graphene/graphite in water and common organic solvents have limited its practical utilization. In this paper, we report a scalable and environmentally friendly technique to form water-in-oil type emulsions stabilized by overlapping pristine graphene sheets, enabling the synthesis of open cell foams containing a continuous graphitic network. Our approach utilizes the insolubility of graphene/graphite in both water and organic solvents and so does not require oxidation, reduction, surfactants, high boilingmore » solvents, chemical functionalization, or the input of large amounts of mechanical energy or heat. At the heart of our technique is the strong attraction of graphene to high-energy oil and water interfaces. This allows for the creation of stable water-in-oil emulsions with controlled droplet size and overlapping graphene sheets playing the role of surfactant by covering the droplet surface and stabilizing the interfaces with a thin graphitic skin. Finally, these emulsions are used as templates for the synthesis of open cell foams with densities below 0.35 g/cm 3 that exhibit remarkable mechanical and electrical properties including compressive moduli up to ~100 MPa, compressive strengths of over 8.3 MPa (1200 psi), and bulk conductivities approaching 7 S/m.« less

Spherical crystallization: A technique use to reform solubility and flow property of active pharmaceutical ingredients.

PubMed

Chatterjee, Arindam; Gupta, Madan Mohan; Srivastava, Birendra

2017-01-01

Tablets have been choice of manufacturers over the years due to their comparatively low cost of manufacturing, packaging, shipping, and ease of administration; also have better stability and can be considered virtually tamper proof. A major challenge in formulation development of the tablets extends from lower solubility of the active agent to the elaborated manufacturing procedures for obtaining a compressible granular material. Moreover, the validation and documentation increases, as the numbers of steps increases for an industrially acceptable granulation process. Spherical crystallization (SC) is a promising technique, which encompass the crystallization, agglomeration, and spheronization phenomenon in a single step. Initially, two methods, spherical agglomeration, and emulsion solvent diffusion, were suggested to get a desired result. Later on, the introduction of modified methods such as crystallo-co-agglomeration, ammonia diffusion system, and neutralization techniques overcame the limitations of the older techniques. Under controlled conditions such as solvent composition, mixing rate and temperature, spherical dense agglomerates cluster from particles. Application of the SC technique includes production of compacted spherical particles of drug having improved uniformity in shape and size of particles, good bulk density, better flow properties as well as better solubility so SC when used on commercial scale will bring down the production costs of pharmaceutical tablet and will increase revenue for the pharmaceutical industries in the competitive market. This review summarizes the technologies available for SC and also suggests the parameters for evaluation of a viable product.

Natural polymer-stabilized multiple water-in-oil-in-water emulsions: a novel dermal drug delivery system for 5-fluorouracil.

PubMed

Hoppel, Magdalena; Mahrhauser, Denise; Stallinger, Christina; Wagner, Florian; Wirth, Michael; Valenta, Claudia

2014-05-01

The aim of this study was to create multiple water-in-oil-in-water (W/O/W) emulsions with an increased long-term stability as skin delivery systems for the hydrophilic model drug 5-fluorouracil. Multiple W/O/W emulsions were prepared in a one-step emulsification process, and were characterized regarding particle size, microstructure and viscosity. In-vitro studies on porcine skin with Franz-type diffusion cells, tape stripping experiments and attenuated total reflectance-fourier transform infrared spectroscopy (ATR-FTIR) were performed. The addition of Solagum AX, a natural polymer mixture of acacia and xanthan gum, led to multiple W/O/W emulsions with a remarkably increased long-term stability in comparison to formulations without a thickener. The higher skin diffusion of 5-fluorouracil from the multiple emulsions compared with an O/W-macroemulsion could be explained by ATR-FTIR. Shifts to higher wave numbers and increase of peak areas of the asymmetric and symmetric CH2 stretching vibrations confirmed a transition of parts of the skin lipids from an ordered to a disordered state after impregnation of porcine skin with the multiple emulsions. Solagum AX is highly suitable for stabilization of the created multiple emulsions. Moreover, these formulations showed superiority over a simple O/W-macroemulsion regarding skin permeation and penetration of 5-fluorouracil. © 2013 Royal Pharmaceutical Society.

Flash nano-precipitation of polymer blends: a role for fluid flow?

NASA Astrophysics Data System (ADS)

Grundy, Lorena; Mason, Lachlan; Chergui, Jalel; Juric, Damir; Craster, Richard V.; Lee, Victoria; Prudhomme, Robert; Priestley, Rodney; Matar, Omar K.

2017-11-01

Porous structures can be formed by the controlled precipitation of polymer blends; ranging from porous matrices, with applications in membrane filtration, to porous nano-particles, with applications in catalysis, targeted drug delivery and emulsion stabilisation. Under a diffusive exchange of solvent for non-solvent, prevailing conditions favour the decomposition of polymer blends into multiple phases. Interestingly, dynamic structures can be `trapped' via vitrification prior to thermodynamic equilibrium. A promising mechanism for large-scale polymer processing is flash nano-precipitation (FNP). FNP particle formation has recently been modelled using spinodal decomposition theory, however the influence of fluid flow on structure formation is yet to be clarified. In this study, we couple a Navier-Stokes equation to a Cahn-Hilliard model of spinodal decomposition. The framework is implemented using Code BLUE, a massively scalable fluid dynamics solver, and applied to flows within confined impinging jet mixers. The present method is valid for a wide range of mixing timescales spanning FNP and conventional immersion precipitation processes. Results aid in the fabrication of nano-scale polymer particles with tuneable internal porosities. EPSRC, UK, MEMPHIS program Grant (EP/K003976/1), RAEng Research Chair (OKM), PETRONAS.

Enzymatically structured emulsions in simulated gastrointestinal environment: impact on interfacial proteolysis and diffusion in intestinal mucus.

PubMed

Macierzanka, Adam; Böttger, Franziska; Rigby, Neil M; Lille, Martina; Poutanen, Kaisa; Mills, E N Clare; Mackie, Alan R

2012-12-18

Fundamental knowledge of physicochemical interactions in the gastrointestinal environment is required in order to support rational designing of protein-stabilized colloidal food and pharmaceutical delivery systems with controlled behavior. In this paper, we report on the colloidal behavior of emulsions stabilized with the milk protein sodium caseinate (Na-Cas), and exposed to conditions simulating the human upper gastrointestinal tract. In particular, we looked at how the kinetics of proteolysis was affected by adsorption to an oil-water interface in emulsion and whether the proteolysis and the emulsion stability could be manipulated by enzymatic structuring of the interface. After cross-linking with the enzyme transglutaminase, the protein was digested with use of an in vitro model of gastro-duodenal proteolysis in the presence or absence of physiologically relevant surfactants (phosphatidylcholine, PC; bile salts, BS). Significant differences were found between the rates of digestion of Na-Cas cross-linked in emulsion (adsorbed protein) and in solution. In emulsion, the digestion of a population of polypeptides of M(r) ca. 50-100 kDa was significantly retarded through the gastric digestion. The persistent interfacial polypeptides maintained the original emulsion droplet size and prevented the system from phase separating. Rapid pepsinolysis of adsorbed, non-cross-linked Na-Cas and its displacement by PC led to emulsion destabilization. These results suggest that structuring of emulsions by enzymatic cross-linking of the interfacial protein may affect the phase behavior of emulsion in the stomach and the gastric digestion rate in vivo. Measurements of ζ-potential revealed that BS displaced the remaining protein from the oil droplets during the simulated duodenal phase of digestion. Diffusion of the postdigestion emulsion droplets through ex vivo porcine intestinal mucus was only significant in the presence of BS due to the high negative charge these biosurfactants imparted to the droplets. This implies that the electrostatic repulsion produced can prevent the droplets from being trapped by the mucus matrix and facilitate their transport across the small intestine mucosal barrier.

Food emulsions as delivery systems for flavor compounds: A review.

PubMed

Mao, Like; Roos, Yrjö H; Biliaderis, Costas G; Miao, Song

2017-10-13

Food flavor is an important attribute of quality food, and it largely determines consumer food preference. Many food products exist as emulsions or experience emulsification during processing, and therefore, a good understanding of flavor release from emulsions is essential to design food with desirable flavor characteristics. Emulsions are biphasic systems, where flavor compounds are partitioning into different phases, and the releases can be modulated through different ways. Emulsion ingredients, such as oils, emulsifiers, thickening agents, can interact with flavor compounds, thus modifying the thermodynamic behavior of flavor compounds. Emulsion structures, including droplet size and size distribution, viscosity, interface thickness, etc., can influence flavor component partition and their diffusion in the emulsions, resulting in different release kinetics. When emulsions are consumed in the mouth, both emulsion ingredients and structures undergo significant changes, resulting in different flavor perception. Special design of emulsion structures in the water phase, oil phase, and interface provides emulsions with great potential as delivery systems to control flavor release in wider applications. This review provides an overview of the current understanding of flavor release from emulsions, and how emulsions can behave as delivery systems for flavor compounds to better design novel food products with enhanced sensorial and nutritional attributes.

Fabrication and characterization of Pickering emulsions and oil gels stabilized by highly charged zein/chitosan complex particles (ZCCPs).

PubMed

Wang, Li-Juan; Yin, Shou-Wei; Wu, Lei-Yan; Qi, Jun-Ru; Guo, Jian; Yang, Xiao-Quan

2016-12-15

Herein, we reported a facile method to fabricate ultra-stable, surfactant- and antimicrobial-free Pickering emulsions by designing and modulating emulsions' interfaces via zein/chitosan colloid particles (ZCCPs). Highly charged ZCCPs with neutral wettability were produced by a facile anti-solvent procedure. The ZCCPs were shown to be effective Pickering emulsifiers because the emulsions formed were highly resistant to coalescence over a 9-month storage period. The ZCCPs were adsorbed irreversibly at the interface during emulsification, forming a hybrid network framework in which zein particles were embedded within the chitosan network, yielding ultra-stable food-grade zein/chitosan colloid particles stabilized Pickering emulsions (ZCCPEs). Moreover, stable surfactant-free oil gels were obtained by a one-step freeze-drying process of the precursor ZCCPEs. This distinctive interfacial architecture accounted for the favourable physical performance, and potentially oxidative and microbial stability of the emulsions and/or oil gels. This work opens up a promising route via a food-grade Pickering emulsion-template approach to transform liquid oil into solid-like fats with zero trans-fat formation. Copyright © 2016 Elsevier Ltd. All rights reserved.

Arrested of coalescence of emulsion droplets of arbitrary size

NASA Astrophysics Data System (ADS)

Mbanga, Badel L.; Burke, Christopher; Blair, Donald W.; Atherton, Timothy J.

2013-03-01

With applications ranging from food products to cosmetics via targeted drug delivery systems, structured anisotropic colloids provide an efficient way to control the structure, properties and functions of emulsions. When two fluid emulsion droplets are brought in contact, a reduction of the interfacial tension drives their coalescence into a larger droplet of the same total volume and reduced exposed area. This coalescence can be partially or totally hindered by the presence of nano or micron-size particles that coat the interface as in Pickering emulsions. We investigate numerically the dependance of the mechanical stability of these arrested shapes on the particles size, their shape anisotropy, their polydispersity, their interaction with the solvent, and the particle-particle interactions. We discuss structural shape changes that can be induced by tuning the particles interactions after arrest occurs, and provide design parameters for the relevant experiments.

Aqueous enzymatic extraction of Moringa oleifera oil.

PubMed

Mat Yusoff, Masni; Gordon, Michael H; Ezeh, Onyinye; Niranjan, Keshavan

2016-11-15

This paper reports on the extraction of Moringa oleifera (MO) oil by using aqueous enzymatic extraction (AEE) method. The effect of different process parameters on the oil recovery was discovered by using statistical optimization, besides the effect of selected parameters on the formation of its oil-in-water cream emulsions. Within the pre-determined ranges, the use of pH 4.5, moisture/kernel ratio of 8:1 (w/w), and 300stroke/min shaking speed at 40°C for 1h incubation time resulted in highest oil recovery of approximately 70% (goil/g solvent-extracted oil). These optimized parameters also result in a very thin emulsion layer, indicating minute amount of emulsion formed. Zero oil recovery with thick emulsion were observed when the used aqueous phase was re-utilized for another AEE process. The findings suggest that the critical selection of AEE parameters is key to high oil recovery with minimum emulsion formation thereby lowering the load on the de-emulsification step. Copyright © 2016 Elsevier Ltd. All rights reserved.

Synthesis of PLGA-Lipid Hybrid Nanoparticles for siRNA Delivery Using the Emulsion Method PLGA-PEG-Lipid Nanoparticles for siRNA Delivery.

PubMed

Wang, Lei; Griffel, Benjamin; Xu, Xiaoyang

2017-01-01

The effective delivery of small interfering RNA (siRNA) to tumor cells remains a challenge for applications in cancer therapy. The development of polymeric nanoparticles with high siRNA loading efficacy has shown great potential for cancer targets. Double emulsion solvent evaporation technique is a useful tool for encapsulation of hydrophilic molecules (e.g., siRNA). Here we describe a versatile platform for siRNA delivery based on PLGA-PEG-cationic lipid nanoparticles by using the double emulsion method. The resulting nanoparticles show high encapsulation efficiency for siRNA (up to 90%) and demonstrate effective downregulation of the target genes in vitro and vivo.

Modified two-step emulsion solvent evaporation technique for fabricating biodegradable rod-shaped particles in the submicron size range.

PubMed

Safari, Hanieh; Adili, Reheman; Holinstat, Michael; Eniola-Adefeso, Omolola

2018-05-15

Though the emulsion solvent evaporation (ESE) technique has been previously modified to produce rod-shaped particles, it cannot generate small-sized rods for drug delivery applications due to the inherent coupling and contradicting requirements for the formation versus stretching of droplets. The separation of the droplet formation from the stretching step should enable the creation of submicron droplets that are then stretched in the second stage by manipulation of the system viscosity along with the surface-active molecule and oil-phase solvent. A two-step ESE protocol is evaluated where oil droplets are formed at low viscosity followed by a step increase in the aqueous phase viscosity to stretch droplets. Different surface-active molecules and oil phase solvents were evaluated to optimize the yield of biodegradable PLGA rods. Rods were assessed for drug loading via an imaging agent and vascular-targeted delivery application via blood flow adhesion assays. The two-step ESE method generated PLGA rods with major and minor axis down to 3.2 µm and 700 nm, respectively. Chloroform and sodium metaphosphate was the optimal solvent and surface-active molecule, respectively, for submicron rod fabrication. Rods demonstrated faster release of Nile Red compared to spheres and successfully targeted an inflamed endothelium under shear flow in vitro and in vivo. Copyright © 2018 Elsevier Inc. All rights reserved.

pH-sensitive poly(lactide-co-glycolide) nanoparticle composite microcapsules for oral delivery of insulin

PubMed Central

Sun, Shaoping; Liang, Na; Yamamoto, Hiromitsu; Kawashima, Yoshiaki; Cui, Fude; Yan, Pengfei

2015-01-01

This study proposes a new concept of pH-sensitive poly(lactide-co-glycolide) (PLGA) nanoparticle composite microcapsules for oral delivery of insulin. Firstly, insulin–sodium oleate complex was prepared by the hydrophobic ion pairing method and then encapsulated into PLGA nanoparticles by the emulsion solvent diffusion method. In order to reduce the burst release of insulin from PLGA nanoparticles and deliver insulin to specific gastrointestinal regions, hence to enhance bioavailability of insulin, the PLGA nanoparticles were further encapsulated into Eudragit® FS 30D to prepare PLGA nanoparticle composite microcapsules by organic spray-drying method. The preparation was evaluated in vitro and in vivo, and the absorption mechanism was discussed. The in vitro drug release studies revealed that the drug release was pH dependent, and the in vivo results demonstrated that the formulation of PLGA nanoparticle composite microcapsules was an effective candidate for oral insulin delivery. PMID:25999713

pH-sensitive poly(lactide-co-glycolide) nanoparticle composite microcapsules for oral delivery of insulin.

PubMed

Sun, Shaoping; Liang, Na; Yamamoto, Hiromitsu; Kawashima, Yoshiaki; Cui, Fude; Yan, Pengfei

2015-01-01

This study proposes a new concept of pH-sensitive poly(lactide-co-glycolide) (PLGA) nanoparticle composite microcapsules for oral delivery of insulin. Firstly, insulin-sodium oleate complex was prepared by the hydrophobic ion pairing method and then encapsulated into PLGA nanoparticles by the emulsion solvent diffusion method. In order to reduce the burst release of insulin from PLGA nanoparticles and deliver insulin to specific gastrointestinal regions, hence to enhance bioavailability of insulin, the PLGA nanoparticles were further encapsulated into Eudragit(®) FS 30D to prepare PLGA nanoparticle composite microcapsules by organic spray-drying method. The preparation was evaluated in vitro and in vivo, and the absorption mechanism was discussed. The in vitro drug release studies revealed that the drug release was pH dependent, and the in vivo results demonstrated that the formulation of PLGA nanoparticle composite microcapsules was an effective candidate for oral insulin delivery.

Role of solvent in metal-on-metal surface diffusion: A case for rational solvent selection for materials synthesis

NASA Astrophysics Data System (ADS)

Imandi, Venkataramana; Jagannath, Mantha Sai Pavan; Chatterjee, Abhijit

2018-09-01

The effect of solvent on diffusion at metal surfaces is poorly understood despite its importance to morphological evolution during materials processing, corrosion and catalysis. In this article, we probe the metal-solvent interfacial structure, effective nature of interactions and dynamics when a solvent is in contact with a metal using a novel accelerated molecular dynamics simulation technique called temperature programmed molecular dynamics (TPMD). TPMD simulations reveal that surface diffusion of metal-on-metal can be made to vary over orders-of-magnitude by tuning the metal-solvent interaction. Ultimately, the solvent can have an indirect effect on diffusion. As the solvent tugs at the metal surface the separation between the adsorbed metal atom (adatom) and the surface layer can be modulated via metal-solvent interactions. The resulting adatom-surface separation can cause stronger/weaker binding of the adatom to the metal surface, which in turn results in the observed slower/enhanced diffusion in the presence of solvent. We believe this effect is ubiquitous in pure metal and metal alloys and in principle one could rationally select solvent to control the material structural evolution. Implications on materials synthesis are discussed in the context of formation of nanoporous materials.

Tunable Pickering Emulsions with Environmentally Responsive Hairy Silica Nanoparticles.

PubMed

Liu, Min; Chen, Xiaoli; Yang, Zongpeng; Xu, Zhou; Hong, Liangzhi; Ngai, To

2016-11-30

Surface modification of the nanoparticles using surface anchoring of amphiphilic polymers offers considerable scope for the design of a wide range of brush-coated hybrid nanoparticles with tunable surface wettability that may serve as new class of efficient Pickering emulsifiers. In the present study, we prepared mixed polymer brush-coated nanoparticles by grafting ABC miktoarm star terpolymers consisting of poly(ethylene glycol), polystyrene, and poly[(3-triisopropyloxysilyl)propyl methacrylate] (μ-PEG-b-PS-b-PIPSMA) on the surface of silica nanoparticles. The wettability of the as-prepared nanoparticles can be precisely tuned by a change of solvent or host-guest complexation. 1 H NMR result confirmed that such wettability change is due to the reorganization of the polymer chain at the grafted layer. We show that this behavior can be used for stabilization and switching between water-in-oil (W/O) and oil-in-water (O/W) emulsions. For hairy particles initially dispersed in oil, W/O emulsions were always obtained with collapsed PEG chains and mobile PS chains at the grafted layer. However, initially dispersing the hairy particles in water resulted in O/W emulsions with collapsed PS chains and mobile PEG chains. When a good solvent for both PS and PEG blocks such as toluene was used, W/O emulsions were always obtained no matter where the hairy particles were dispersed. The wettability of the mixed polymer brush-coated silica particles can also be tuned by host-guest complexation between PEG block and α-CD. More importantly, our result showed that surprisingly the resultant mixed brush-coated hairy nanoparticles can be employed for the one-step production of O/W/O multiple emulsions that are not attainable from conventional Pickering emulsifiers. The functionalized hairy silica nanoparticles at the oil-water interface can be further linked together utilizing poly(acrylic acid) as the reversible linker to form supramolecular colloidosomes, which show pH-dependent release of cargo.

Molecular Design of Squalene/Squalane Countertypes via the Controlled Oligomerization of Isoprene and Evaluation of Vaccine Adjuvant Applications.

PubMed

Adlington, Kevin; El Harfi, Jaouad; Li, Jianing; Carmichael, Kim; Guderian, Jeffrey A; Fox, Christopher B; Irvine, Derek J

2016-01-11

The potential to replace shark-derived squalene in vaccine adjuvant applications with synthetic squalene/poly(isoprene) oligomers, synthesized by the controlled oligomerization of isoprene is demonstrated. Following on from our previous work regarding the synthesis of poly(isoprene) oligomers, we demonstrate the ability to tune the molecular weight of the synthetic poly(isoprene) material beyond that of natural squalene, while retaining a final backbone structure that contained a minimum of 75% of 1,4 addition product and an acceptable polydispersity. The synthesis was successfully scaled from the 2 g to the 40 g scale both in the bulk (i.e., solvent free) and with the aid of additional solvent by utilizing catalytic chain transfer polymerization (CCTP) as the control method, such that the target molecular weight, acceptable dispersity levels, and the desired level of 1,4 addition in the backbone structure and an acceptable yield (∼60%) are achieved. Moreover, the stability and in vitro bioactivity of nanoemulsion adjuvant formulations manufactured with the synthetic poly(isoprene) material are evaluated in comparison to emulsions made with shark-derived squalene. Emulsions containing the synthetic poly(isoprene) achieved smaller particle size and equivalent or enhanced bioactivity (stimulation of cytokine production in human whole blood) compared to corresponding shark squalene emulsions. However, as opposed to the shark squalene-based emulsions, the poly(isoprene) emulsions demonstrated reduced long-term size stability and induced hemolysis at high concentrations. Finally, we demonstrate that the synthetic oligomeric poly(isoprene) material could successfully be hydrogenated such that >95% of the double bonds were successfully removed to give a representative poly(isoprene)-derived squalane mimic.

To Model Chemical Reactivity in Heterogeneous Emulsions, Think Homogeneous Microemulsions.

PubMed

Bravo-Díaz, Carlos; Romsted, Laurence Stuart; Liu, Changyao; Losada-Barreiro, Sonia; Pastoriza-Gallego, Maria José; Gao, Xiang; Gu, Qing; Krishnan, Gunaseelan; Sánchez-Paz, Verónica; Zhang, Yongliang; Dar, Aijaz Ahmad

2015-08-25

Two important and unsolved problems in the food industry and also fundamental questions in colloid chemistry are how to measure molecular distributions, especially antioxidants (AOs), and how to model chemical reactivity, including AO efficiency in opaque emulsions. The key to understanding reactivity in organized surfactant media is that reaction mechanisms are consistent with a discrete structures-separate continuous regions duality. Aggregate structures in emulsions are determined by highly cooperative but weak organizing forces that allow reactants to diffuse at rates approaching their diffusion-controlled limit. Reactant distributions for slow thermal bimolecular reactions are in dynamic equilibrium, and their distributions are proportional to their relative solubilities in the oil, interfacial, and aqueous regions. Our chemical kinetic method is grounded in thermodynamics and combines a pseudophase model with methods for monitoring the reactions of AOs with a hydrophobic arenediazonium ion probe in opaque emulsions. We introduce (a) the logic and basic assumptions of the pseudophase model used to define the distributions of AOs among the oil, interfacial, and aqueous regions in microemulsions and emulsions and (b) the dye derivatization and linear sweep voltammetry methods for monitoring the rates of reaction in opaque emulsions. Our results show that this approach provides a unique, versatile, and robust method for obtaining quantitative estimates of AO partition coefficients or partition constants and distributions and interfacial rate constants in emulsions. The examples provided illustrate the effects of various emulsion properties on AO distributions such as oil hydrophobicity, emulsifier structure and HLB, temperature, droplet size, surfactant charge, and acidity on reactant distributions. Finally, we show that the chemical kinetic method provides a natural explanation for the cut-off effect, a maximum followed by a sharp reduction in AO efficiency with increasing alkyl chain length of a particular AO. We conclude with perspectives and prospects.

Viscosity-dependent diffusion of fluorescent particles using fluorescence correlation spectroscopy.

PubMed

Jung, Chanbae; Lee, Jaeran; Kang, Manil; Kim, Sok Won

2014-11-01

Fluorescent particles show the variety characteristics by the interaction with other particles and solvent. In order to investigate the relationship between the dynamic properties of fluorescent particles and solvent viscosity, particle diffusion in various solvents was evaluated using a fluorescence correlation spectroscopy. Upon analyzing the correlation functions of AF-647, Q-dot, and beads with different viscosity values, the diffusion time of all particles was observed to increase with increasing solvent viscosity, and the ratio of diffusion time to solvent viscosity, τ D /η, showed a linear dependence on particle size. The particle diffusion coefficients calculated from the diffusion time decreased with increasing solvent viscosity. Further, the hydrodynamic radii of AF-647, Q-dot, and beads were 0.98 ± 0.1 nm, 64.8 ± 3.23 nm, and 89.8 ± 4.91 nm, respectively, revealing a linear dependence on τ D /η, which suggests that the hydrodynamic radius of a particle strongly depends on both the physical size of the particle and solvent viscosity.

Electric field-driven, magnetically-stabilized ferro-emulsion phase contactor

DOEpatents

Scott, T.C.

1990-07-17

Methods and systems are disclosed for interfacial surface area contact between a dispersed phase liquid and a continuous phase liquid in counter-current flow for purposes such as solvent extraction. Initial droplets of a dispersed phase liquid material containing ferromagnetic particles functioning as a packing'' are introduced to a counter-current flow of the continuous phase. A high intensity pulsed electric field is applied so as to shatter the initial droplets into a ferromagnetic emulsion comprising many smaller daughter droplets having a greater combined total surface area than that of the initial droplets in contact with the continuous phase material. A magnetic field is applied to control the position of the ferromagnetic emulsion for enhanced coalescence of the daughter droplets into larger reformed droplets. 2 figs.

Electric field-driven, magnetically-stabilized ferro-emulsion phase contactor

DOEpatents

Scott, Timothy C.

1990-01-01

Methods and systems for interfacial surface area contact between a dispersed phase liquid and a continuous phase liquid in counter-current flow for purposes such as solvent extraction. Initial droplets of a dispersed phase liquid material containing ferromagnetic particles functioning as a "packing" are introduced to a counter-current flow of the continuous phase. A high intensity pulsed electric field is applied so as to shatter the initial droplets into a ferromagnetic emulsion comprising many smaller daughter droplets having a greater combined total surface area than that of the initial droplets in contact with the continuous phase material. A magnetic field is applied to control the position of the ferromagnetic emulsion for enhanced coalescence of the daughter droplets into larger reformed droplets.

Fluorescence correlation spectroscopy directly monitors coalescence during nanoparticle preparation.

PubMed

Schaeffel, David; Staff, Roland Hinrich; Butt, Hans-Juergen; Landfester, Katharina; Crespy, Daniel; Koynov, Kaloian

2012-11-14

Dual color fluorescence cross-correlation spectroscopy (DC FCCS) experiments were conducted to study the coalescence and aggregation during the formation of nanoparticles. To assess the generality of the method, three completely different processes were selected to prepare the nanoparticles. Polymeric nanoparticles were formed either by solvent evaporation from emulsion nanodroplets of polymer solutions or by miniemulsion polymerization. Inorganic nanocapsules were formed by polycondensation of alkoxysilanes at the interface of nanodroplets. In all cases, DC FCCS provided fast and unambiguous information about the occurrence of coalescence and thus a deeper insight into the mechanism of nanoparticle formation. In particular, it was found that coalescence played a minor role for the emulsion-solvent evaporation process and the miniemulsion polymerization, whereas substantial coalescence was detected during the formation of the inorganic nanocapsules. These findings demonstrate that DC FCCS is a powerful tool for monitoring nanoparticles genesis.

Enzymatic Synthesis of Glyserol-Coconut Oil Fatty Acid and Glycerol-Decanoic Acis Ester as Emulsifier and Antimicrobial Agents Using Candida rugosa Lipase EC 3.1.1.3

NASA Astrophysics Data System (ADS)

Handayani, Sri; Putri, Ayu Tanissa Tamara; Setiasih, Siswati; Hudiyono, Sumi

2018-01-01

In this research, enzymatic esterification was carried out between glycerol and fatty acid from coconut oil and decanoic acid using n-hexane as solvent. In this reaction Candida rugosa lipase was used as biocatalyst. Optimization esterification reaction was carried out for parameter of the substrate ratio. The mmol ratio between fatty acid and glycerol were used are 1:1, 1:2, 1:3, and 1: 4. The highest conversion percentage obtained at the mole ratio of 1: 4 with the value of 78.5% for the glycerol-decanoic acid ester and 55.4% for the glycerol coconut oil fatty acid ester. Esterification products were characterized by FT-IR. The FT-IR spectrum showed that the ester bond was formed as indicated by the wave number 1750-1739 cm-1. The esterification products were then examined by simple emulsion test and was proved to be an emulsifier. The glycerol-coconut oil fatty acid ester produced higher stability emulsion compare with glycerol decanoic ester. The antimicrobial activity assay using disc diffusion method showed that both glycerol-coconut oil fatty acid ester and glycerol-decanoic ester had the ability inhibiting the growth of Propionibacterium acnes and Staphylococcus epidermidis. Glycerol-decanoic ester shows higher antimicrobial activity than glycerol-coconut oil fatty acid ester.

Development of soy lecithin based novel self-assembled emulsion hydrogels.

PubMed

Singh, Vinay K; Pandey, Preeti M; Agarwal, Tarun; Kumar, Dilip; Banerjee, Indranil; Anis, Arfat; Pal, Kunal

2015-03-01

The current study reports the development and characterization of soy lecithin based novel self-assembled emulsion hydrogels. Sesame oil was used as the representative oil phase. Emulsion gels were formed when the concentration of soy lecithin was >40% w/w. Metronidazole was used as the model drug for the drug release and the antimicrobial tests. Microscopic study showed the apolar dispersed phase in an aqueous continuum phase, suggesting the formation of emulsion hydrogels. FTIR study indicated the formation of intermolecular hydrogen bonding, whereas, the XRD study indicated predominantly amorphous nature of the emulsion gels. Composition dependent mechanical and drug release properties of the emulsion gels were observed. In-depth analyses of the mechanical studies were done using Ostwald-de Waele power-law, Kohlrausch and Weichert models, whereas, the drug release profiles were modeled using Korsmeyer-Peppas and Peppas-Sahlin models. The mechanical analyses indicated viscoelastic nature of the emulsion gels. The release of the drug from the emulsion gels was diffusion mediated. The drug loaded emulsion gels showed good antimicrobial activity. The biocompatibility test using HaCaT cells (human keratinocytes) suggested biocompatibility of the emulsion gels. Copyright © 2015 Elsevier Ltd. All rights reserved.

Solvent and solute ingress into hydrogels resolved by a combination of imaging techniques

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

Wagner, D.; Burbach, J.; Egelhaaf, S. U.

2016-05-28

Using simultaneous neutron, fluorescence, and optical brightfield transmission imaging, the diffusion of solvent, fluorescent dyes, and macromolecules into a crosslinked polyacrylamide hydrogel was investigated. This novel combination of different imaging techniques enables us to distinguish the movements of the solvent and fluorescent molecules. Additionally, the swelling or deswelling of the hydrogels can be monitored. From the sequence of images, dye and solvent concentrations were extracted spatially and temporally resolved. Diffusion equations and different boundary conditions, represented by different models, were used to quantitatively analyze the temporal evolution of these concentration profiles and to determine the diffusion coefficients of solvent andmore » solutes. Solute size and network properties were varied and their effect was investigated. Increasing the crosslinking ratio or partially drying the hydrogel was found to hinder solute diffusion due to the reduced pore size. By contrast, solvent diffusion seemed to be slightly faster if the hydrogel was only partially swollen and hence solvent uptake enhanced.« less

Integration of whole-cell reaction and product isolation: Highly hydrophobic solvents promote in situ substrate supply and simplify extractive product isolation.

PubMed

Leis, Dorothea; Lauß, Bernhard; Macher-Ambrosch, Robert; Pfennig, Andreas; Nidetzky, Bernd; Kratzer, Regina

2017-09-10

Product isolation from aqueous-organic reaction mixtures that contain high concentrations of whole cells constitutes a challenging task in bioprocessing. Stirring of the biphasic reaction media leads to the formation of solvent droplets coated by cells and other surface active components and an emulsion forms. We used an early focus on phase separation to simplify a whole-cell bioreduction. Octanol, heptanol, hexanol, hexane and dipropylether were tested as co-solvents in the E. coli catalyzed reduction of o-chloroacetophenone. All solvents showed very similar performance in bioreductions and highest yields were obtained with low organic-to-aqueous phase ratios. Reaction mixtures were directly investigated for organic-phase recovery. Phase separation was optimized in small-scale settling experiments and confirmed by the isolation of 20.4g (S)-1-(2-chlorophenyl)ethanol from a 0.5L batch reduction containing 40g CDW /L whole-cell catalyst. Solvent consumption during product isolation could be halved by the simple addition of sodium hydroxide prior to product extraction. Basification to pH 13.5 and three extraction steps with a total of 1.2v/v hexane led to an isolated yield of 87% (97% reduction yield). A general emulsion destabilizing effect under harsh conditions, as extreme pH values and presence of toxic reactants, was observed. Copyright © 2016 The Authors. Published by Elsevier B.V. All rights reserved.

Synthesis of soluble conducting polymers by acoustic mixing

DOEpatents

Kane, Marie C.

2016-09-13

A method including combining an aniline monomer, an oxidant, water and an organic solvent; subjecting the combination to acoustic mixing to form an emulsion; and recovering a polyaniliine from the combination. A method including combining a aniline monomer, an oxidant, water and an organic solvent; forming a polyaniline by acoustic mixing the combination; and recovering the polyaniliine from the combination. A method including forming a combination of an aniline monomer, an oxidant, water and an organic solvent in the absence of an emulsifier; acoustic mixing the combination for a time period to form a polyaniline; and recovering a polyaniliine from the combination.

How does oil type determine emulsion characteristics in concentrated Na-caseinate emulsions?

PubMed

Tan, Hui Lin; McGrath, Kathryn M

2013-08-01

Macroscopic properties and ensemble average diffusion of concentrated (dispersed phase 50-60 wt%) Na-caseinate-stabilised emulsions for three different oils (soybean oil, palm olein and tetradecane) were explored. On a volume fraction basis, pulsed gradient stimulated echo (PGSTE)-NMR data show that droplet dynamics for all three systems are similar within a region of the emulsion morphology diagram. The exact limits of the emulsion space depend however on which oil is considered. The reduced solubility of tetradecane in water, and Na-caseinate in tetradecane, result in the stabilisation of flocs during formulation. Floc formation is not observed when soybean oil or palm olein is used under identical emulsion formulation conditions. Linear rheology experiments provide indirect evidence that the local structure and the properties of the thin film interfacial domain of tetradecane emulsions vary from those of soybean oil and palm olein emulsions. Collectively these data indicate that protein/oil interactions within a system dominate over specific oil droplet structure and size distribution, which are similar in the three systems. Copyright © 2013 Elsevier Inc. All rights reserved.

Emulsion Liquid Membrane Removal of Arsenic and Strontium from Wastewater: AN Experimental and Theoretical Study.

NASA Astrophysics Data System (ADS)

Zhou, Ding-Wei

The emulsion liquid membrane (ELM) technique has been successfully applied on the removal of arsenic (As) from metallurgical wastewater and the removal of strontium (Sr) from radioactive wastewater. This study consisted of experimental work and mathematical modeling. Extraction of arsenic by an emulsion liquid membrane was firstly investigated. The liquid membrane used was composed of 2-ethylhexyl alcohol (2EHA) as the extractant, ECA4360J as the surfactant, and Exxsol D-80 solvent (or heptane) as the diluent. The sulfuric acid and sodium hydroxide solutions were used as the external and internal phases, respectively. The arsenic removal efficiency reached 92% within 15 minutes in one stage. Extraction and stripping chemistries were postulated and investigated. It was observed that extraction efficiency and rate increase with the increase of acidic strength and alkali strength in the external and internal phases, respectively. It was also observed that the removal selectivity of arsenic over copper is extremely high. Strontium-90 is one of the major radioactive metals appearing in nuclear wastewater. The emulsion liquid membrane process was investigated as a separation method by using the non-radioactive ^{87}Sr as its substitute. In our study, the membrane phase was composed of di-(2-ethylhexyl) phosphoric acid (D2EHPA) as the extractant, ECA4360J as the surfactant and Exxsol D-80 as the diluent. A sulfuric acid solution was used in the internal phase as the stripping agent. The pH range in the external phase was determined by the extraction isotherm. Under the most favorable operating condition, the strontium removal efficiency can reach 98% in two minutes. Mass transfer of the emulsion liquid membrane (ELM) system was modeled mathematically. Our model took into account the following: mass transfer of solute across the film between the external phase and the membrane phase, chemical equilibrium of the extraction reaction at the external phase-membrane interface, simultaneous diffusion of the solute-carrier complex inside the globule membrane phase and stripping of the complex at the membrane-internal phase interface, chemical equilibrium of the stripping reaction at the membrane-internal phase interface and leakage of the solute from the internal phase to the external phase. Resulting simultaneous partial differential equations were solved analytically by the Laplace transform method. Four dimensionless groups were found with special physical meanings to characterize the emulsion liquid membrane systems. It not only predicted the concentration of solute in the external phase versus time, but also gave the concentration profile inside the membrane globule and the interfacial concentration at the external-membrane phase interface at different time. The model predicted very well the experimental data obtained from the removal of arsenic and strontium by the emulsion liquid membranes.

Preparation and in vitro/in vivo evaluation of PLGA microspheres containing norquetiapine for long-acting injection.

PubMed

Park, Chun-Woong; Lee, Hyo-Jung; Oh, Dong-Won; Kang, Ji-Hyun; Han, Chang-Soo; Kim, Dong-Wook

2018-01-01

Norquetiapine ( N -desalkyl quetiapine, NQ) is an active metabolite of quetiapine with stable pharmacokinetic and pharmacological properties. However, its short half-life is a drawback for clinical applications, and long-acting formulations are required. The objectives of this study were to prepare improved entrapment efficiency NQ freebase microspheres by the solvent evaporation method with poly(d,l-lactic-co-glycolic acid) (PLGA) as a release modulator and to evaluate their physicochemical and in vitro/in vivo release properties. NQ freebase PLGA (1:5 w/w) formulations were prepared by the oil-in-water (o/w) emulsion-solvent evaporation method. A solution of the drug and PLGA in 9:1 v/v dichloromethane:ethanol was mixed with 0.2% polyvinyl alcohol and homogenized at 2,800 rpm. The emulsion was stirred for 3 h to dilute and evaporate the solvent. After that, the resulting product was freeze-dried. Drug-loading capacity was measured by the validated RP-HPLC method. The surface morphology of the microspheres was observed by scanning electron microscopy (SEM), and the physicochemical properties were evaluated by differential scanning calorimetry, powder X-ray diffraction, and Fourier-transform infrared spectroscopy particle size distribution. The in vitro dissolution test was performed using a rotary shaking bath at 37°C, with constant shaking at 50 rpm in sink condition. The NQ freebase microspheres prepared by o/w emulsion-solvent evaporation showed over 30% efficiency. NQ was confirmed to be amorphous in the microspheres by powder X-ray diffraction and differential scanning calorimetry. Special chemical interaction in the microspheres was not observed by FT-IR. The in vitro dissolution test demonstrated that the prepared microspheres' release properties were maintained for more than 20 days. The in vivo test also confirmed that the particles' long acting properties were maintained. Therefore, good in vitro-in vivo correlation was established. In this study, NQ freebase-PLGA microspheres showed potential for the treatment of schizophrenia for long-periods.

Organic Thin Films Deposited by Emulsion-Based, Resonant Infrared, Matrix-Assisted Pulsed Laser Evaporation: Fundamentals and Applications

NASA Astrophysics Data System (ADS)

Ge, Wangyao

Thin film deposition techniques are indispensable to the development of modern technologies as thin film based optical coatings, optoelectronic devices, sensors, and biological implants are the building blocks of many complicated technologies, and their performance heavily depends on the applied deposition technique. Particularly, the emergence of novel solution-processed materials, such as soft organic molecules, inorganic compounds and colloidal nanoparticles, facilitates the development of flexible and printed electronics that are inexpensive, light weight, green and smart, and these thin film devices represent future trends for new technologies. One appealing feature of solution-processed materials is that they can be deposited into thin films using solution-processed deposition techniques that are straightforward, inexpensive, high throughput and advantageous to industrialize thin film based devices. However, solution-processed techniques rely on wet deposition, which has limitations in certain applications, such as multi-layered film deposition of similar materials and blended film deposition of dissimilar materials. These limitations cannot be addressed by traditional, vacuum-based deposition techniques because these dry approaches are often too energetic and can degrade soft materials, such as polymers, such that the performance of resulting thin film based devices is compromised. The work presented in this dissertation explores a novel thin film deposition technique, namely emulsion-based, resonant infrared, matrix-assisted pulsed laser evaporation (RIR-MAPLE), which combines characteristics of wet and dry deposition techniques for solution-processed materials. Previous studies have demonstrated the feasibility of emulsion-based RIR-MAPLE to deposit uniform and continuous organic, nanoparticle and blended films, as well as hetero-structures that otherwise are difficult to achieve. However, fundamental understanding of the growth mechanisms that govern emulsion-based RIR-MAPLE is still missing, which increases the difficulty of using rational design to improve the performance of initial RIR-MAPLE devices that have been demonstrated. As a result, it is important to study the fundamentals of emulsion-based RIR-MAPLE in order to provide insight into the long-term prospects for this thin film deposition technique. This dissertation explores the fundamental deposition mechanisms of emulsion-based RIR-MAPLE by considering the effects of the emulsion target composition (namely, the primary solvent, secondary solvent, and surfactant) on the properties of deposited polymer films. The study of primary solvent effects on hydrophobic polymer deposition helps identify the unique method of film formation for emulsion-based RIR-MAPLE, which can be described as cluster-by-cluster deposition of emulsified particles that yields two levels of ordering (i.e., within the clusters and among the clusters). The generality of this film formation mechanism is tested by applying the lessons learned to hydrophilic polymer deposition. Based on these studies, the deposition design rules to achieve smooth polymer films, which are important for different device applications, are identified according to the properties of the polymer. After discussion of the fundamental deposition mechanisms, three applications of emulsion-based RIR-MAPLE, namely thin film deposition of organic solar cells, polymer/nanoparticle hybrid solar cells, and antimicrobial/fouling-release multifunctional films, are studied. The work on organic solar cells identifies the ideal deposition mode for blended films with nanoscale domain sizes, as well as demonstrates the relationships among emulsion target composition, film properties, and corresponding device performance. The studies of polymer/nanoparticle hybrid solar cells demonstrate precise control of colloidal nanoparticle deposition, in which the integrity of nanoparticles is maintained and a distinct film morphology is achieved when co-deposited with polymers. Finally, the application of antimicrobial and fouling-release multifunctional films demonstrates the importance of blended film deposition with nanoscale phase separation, a key feature to achieving reusable bio-films that can kill bacteria when illuminated with ultraviolet light. Thus, this dissertation provides great insight to the fundamentals of emulsion-based RIR-MAPLE, serves as a valuable reference for future development, and paves the pathway for wider adoption of this unique thin film deposition technique, especially for organic solar cells.

Variational Implicit Solvation with Solute Molecular Mechanics: From Diffuse-Interface to Sharp-Interface Models.

PubMed

Li, Bo; Zhao, Yanxiang

2013-01-01

Central in a variational implicit-solvent description of biomolecular solvation is an effective free-energy functional of the solute atomic positions and the solute-solvent interface (i.e., the dielectric boundary). The free-energy functional couples together the solute molecular mechanical interaction energy, the solute-solvent interfacial energy, the solute-solvent van der Waals interaction energy, and the electrostatic energy. In recent years, the sharp-interface version of the variational implicit-solvent model has been developed and used for numerical computations of molecular solvation. In this work, we propose a diffuse-interface version of the variational implicit-solvent model with solute molecular mechanics. We also analyze both the sharp-interface and diffuse-interface models. We prove the existence of free-energy minimizers and obtain their bounds. We also prove the convergence of the diffuse-interface model to the sharp-interface model in the sense of Γ-convergence. We further discuss properties of sharp-interface free-energy minimizers, the boundary conditions and the coupling of the Poisson-Boltzmann equation in the diffuse-interface model, and the convergence of forces from diffuse-interface to sharp-interface descriptions. Our analysis relies on the previous works on the problem of minimizing surface areas and on our observations on the coupling between solute molecular mechanical interactions with the continuum solvent. Our studies justify rigorously the self consistency of the proposed diffuse-interface variational models of implicit solvation.

Ultrasonication-assisted preparation and characterization of emulsions and emulsion gels for topical drug delivery.

PubMed

Singh, Vinay K; Behera, Baikuntha; Pramanik, Krishna; Pal, Kunal

2015-03-01

The current study describes the use of ultrasonication for the preparation of biphasic emulsions and emulsion gels for topical drug delivery. Sorbitan monostearate (SMS) was used as the surfactant for stabilizing the interface of sesame oil (apolar phase) and water (polar phase). Emulsions were formed at lower concentrations of SMS, whereas emulsion gels were formed at higher concentrations of SMS. The formulations were characterized by fluorescent microscopy, X-ray diffraction, viscosity, stress relaxation, spreadability, and differential scanning calorimetry studies. Fluorescence microscopy suggested formation of oil-in-water type of formulations. There was an increase in the viscosity, bulk resistance, and firmness of the formulations as the proportions of SMS was increased. The emulsion gels were viscoelastic in nature. Thermal studies suggested higher thermodynamic stability at higher proportions of either SMS or water. Metronidazole, a model antimicrobial drug, was incorporated within the formulations. The release of the drug from the formulations was found to be diffusion mediated. The drug-loaded formulations showed sufficient antimicrobial efficiency to be used as carriers for topical antimicrobial drug delivery. © 2014 Wiley Periodicals, Inc. and the American Pharmacists Association.

Oxidative Stability of Granola Bars Enriched with Multilayered Fish Oil Emulsion in the Presence of Novel Brown Seaweed Based Antioxidants.

PubMed

Hermund, Ditte B; Karadağ, Ayşe; Andersen, Ulf; Jónsdóttir, Rósa; Kristinsson, Hordur G; Alasalvar, Cesarettin; Jacobsen, Charlotte

2016-11-09

Fucus vesiculosus extracts that have both radical scavenging activity and metal chelating ability in vitro were used as natural antioxidant in granola bars enriched with fish oil emulsion by using primary and secondary emulsion systems stabilized by sodium caseinate alone and sodium caseinate-chitosan. The bars were stored at 20 °C and evaluated over a period of 10 weeks by measuring the development of primary and secondary oxidation products. The samples prepared with secondary emulsion system developed less oxidation products probably due to increased interfacial layer thickness that would act as a barrier to the penetration and diffusion of molecular species that promote oxidation. The positive charge of oil droplets in the secondary emulsion may also inhibit iron-lipid interaction through electrostatic repulsion. Additional protection against lipid oxidation was obtained when fish oil emulsions were added to the granola bars especially in combination with acetone and ethanol extracts of Fucus vesiculosus.

Impact of Protein Gel Porosity on the Digestion of Lipid Emulsions.

PubMed

Sarkar, Anwesha; Juan, Jean-Marc; Kolodziejczyk, Eric; Acquistapace, Simone; Donato-Capel, Laurence; Wooster, Tim J

2015-10-14

The present study sought to understand how the microstructure of protein gels impacts lipolysis of gelled emulsions. The selected system consisted of an oil-in-water (o/w) emulsion embedded within gelatin gels. The gelatin-gelled emulsions consisted of a discontinuous network of aggregated emulsion droplets (mesoscale), dispersed within a continuous network of gelatin (microscale). The viscoelastic properties of the gelled emulsions were dominated by the rheological behavior of the gelatin, suggesting a gelatin continuous microstructure rather than a bicontinuous gel. A direct relationship between the speed of fat digestion and gel average mesh size was found, indicating that the digestion of fat within gelatin-gelled emulsions is controlled by the ability of the gel's microstructure to slow lipase diffusion to the interface of fat droplets. Digestion of fat was facilitated by gradual breakdown of the gelatin network, which mainly occurred via surface erosion catalyzed by proteases. Overall, this work has demonstrated that the lipolysis kinetics of gelled emulsions is driven by the microstructure of protein gels; this knowledge is key for the future development of microstructures to control fat digestion and/or the delivery of nutrients to different parts of the gastrointestinal tract.

Osmosis-driven viscous fingering of oil-in-water emulsions

NASA Astrophysics Data System (ADS)

Liu, Ying; Rallabandi, Bhargav; Baskaran, Mrudhula; Stone, Howard

2017-11-01

Viscous fingering occurs when a low viscosity fluid invades a more viscous fluid. Fingering of two miscible fluids is more complicated than that of immiscible fluids in that there is no sharp fluid-fluid interface and diffusion occurs between the phases. We experimentally studied the fingering of two miscible fluids: an oil-in-water emulsion and a sodium chloride solution. When the concentration of sodium chloride in the water phase in the emulsion exceeds that in the sodium chloride solution, the consequent osmotic flow automatically facilitates the occurrence of the fingering. On the contrary, when the sodium chloride solution has higher concentration, the spreading of emulsion is more uniform than the case without the concentration difference. We provide a model to rationalize and quantify these observations.

Effects of Shapes of Solute Molecules on Diffusion: A Study of Dependences on Solute Size, Solvent, and Temperature.

PubMed

Chan, T C; Li, H T; Li, K Y

2015-12-24

Diffusivities of basically linear, planar, and spherical solutes at infinite dilution in various solvents are studied to unravel the effects of solute shapes on diffusion. On the basis of the relationship between the reciprocal of diffusivity and the molecular volume of solute molecules with similar shape in a given solvent at constant temperature, the diffusivities of solutes of equal molecular volume but different shapes are evaluated and the effects due to different shapes of two equal-sized solute molecules on diffusion are determined. It is found that the effects are dependent on the size of the solute pairs studied. Evidence of the dependence of the solute-shape effects on solvent properties is also demonstrated and discussed. Here, some new diffusion data of aromatic compounds in methanol at different temperatures are reported. The result for methanol in this study indicates that the effects of solute shape on diffusivity are only weakly dependent on temperature.

Impact of solvent granularity and layering on tracer hydrodynamics in confinement.

PubMed

Bollinger, Jonathan A; Carmer, James; Jain, Avni; Truskett, Thomas M

2016-11-28

Classic hydrodynamic arguments establish that when a spherical tracer particle is suspended between parallel walls, tracer-wall coupling mediated by the solvent will cause the tracer to exhibit position-dependent diffusivity. We investigate how the diffusivity profiles of confined tracers are impacted by the diameter size-ratio of the tracer to solvent: starting from the classic limit of infinite size-ratio (i.e., continuum solvent), we consider size-ratios of four or less to examine how hydrodynamic predictions are disrupted for systems where the tracer and solvent are of similar scale. We use computer simulations and techniques based on the Fokker-Planck formalism to calculate the diffusivity profiles of hard-sphere tracer particles in hard-sphere solvents, focusing on the dynamics perpendicular to the walls. Given wall separations of several tracer diameters, we first consider confinement between hard walls, where anisotropic structuring at the solvent lengthscale generates inhomogeneity in the tracer free-energy landscape and undermines hydrodynamic predictions locally. We then introduce confining planes that we term transparent walls, which restrict tracer and solvent center-accessibilities while completely eliminating static anisotropy, and reveal position-dependent signatures in tracer diffusivity solely attributable to confinement. With or without suppressing static heterogeneity, we find that tracer diffusivity increasingly deviates on a local basis from hydrodynamic predictions at smaller size-ratios. However, hydrodynamic theory still approximately captures spatially-averaged dynamics across the pores even for very small tracer-solvent size-ratios over a wide range of solvent densities and wall separations.

Application of edible paraffin oil for cationic dye removal from water using emulsion liquid membrane.

PubMed

Zereshki, Sina; Daraei, Parisa; Shokri, Amin

2018-05-18

Using an emulsion liquid membrane based on edible oils is investigated for removing cationic dyes from aqueous solutions. There is a great potential for using edible oils in food industry extraction processes. The parameters affecting the stability of the emulsion and the extraction rate were studied. These parameters were the emulsification time, the stirring speed, the surfactant concentration, the internal phase concentration, the feed phase concentration, the volume ratio of internal phase to organic phase and the treat ratio. In order to stabilize the emulsion without using a carrier, edible paraffin oil and heptane are used at an 80:20 ratio. The optimum conditions for the extraction of methylene blue (MB), crystal violet and methyl violet (CV and MV) cationic dyes using edible paraffin oil as an environment friendly solvent are represented. A removal percentage of 95% was achieved for a mixture of dyes. The optimum concentration of sodium hydroxide in the internal phase, which results a stabile emulsion with a high stripping efficiency of 96%, was 0.04 M. An excellent membrane recovery was observed and the extraction of dyes did not decrease up to seven run cycles. Copyright © 2018 Elsevier B.V. All rights reserved.

pH-sensitive Eudragit nanoparticles for mucosal drug delivery.

PubMed

Yoo, Jin-Wook; Giri, Namita; Lee, Chi H

2011-01-17

Drug delivery via vaginal epithelium has suffered from lack of stability due to acidic and enzymatic environments. The biocompatible pH-sensitive nanoparticles composed of Eudragit S-100 (ES) were developed to protect loaded compounds from being degraded under the rigorous vaginal conditions and achieve their therapeutically effective concentrations in the mucosal epithelium. ES nanoparticles containing a model compound (sodium fluorescein (FNa) or nile red (NR)) were prepared by the modified quasi-emulsion solvent diffusion method. Loading efficiencies were found to be 26% and 71% for a hydrophilic and a hydrophobic compound, respectively. Both hydrophilic and hydrophobic model drugs remained stable in nanoparticles at acidic pH, whereas they are quickly released from nanoparticles upon exposure at physiological pH. The confocal study revealed that ES nanoparticles were taken up by vaginal cells, followed by pH-responsive drug release, with no cytotoxic activities. The pH-sensitive nanoparticles would be a promising carrier for the vaginal-specific delivery of various therapeutic drugs including microbicides and peptides/proteins. Published by Elsevier B.V.

Synthesis of berberine loaded polymeric nanoparticles by central composite design

NASA Astrophysics Data System (ADS)

Mehra, Meenakshi; Sheorain, Jyoti; Kumari, Santosh

2016-04-01

Berberine is an isoquinoline alkaloid which is extracted from bark and roots of Berberis vulgaris plant. It has been used in ayurvedic medicine as it possess antimicrobial, antidiabetic, anticancer, antioxidant properties etc. But poor solubility of berberine leads to poor stability and bioavailability in medical formulations decreasing its efficacy. Hence nanoformulations of berberine can help in removing the limiting factors of alkaloid enhancing its utilization in pharmaceutical industry. Sodium alginate polymer was used to encapsulate berberine within nanoparticles by emulsion solvent evaporation method using tween 80 as a surfactant. Two factors and three level in central composite design was used to study the formulation. The optimized formulation (1% v/v of Tween 80 and 0.01% w/v of sodium alginate) of polymeric nanoparticles was taken for further evaluations. The size of synthesized nanoparticles was found to be 71.18 nm by particle size analysis (PSA). The berberine loaded polymeric nanoparticles showed better antibacterial activity compared to aqueous solution of berberine by well diffusion assay.

Analytical applications of emulsions and microemulsions.

PubMed

Burguera, José Luis; Burguera, Marcela

2012-07-15

Dispersion systems like emulsions and microemulsions are able to solubilize both polar and non-polar substances due to the special arrangement of the oil and aqueous phases. The main advantages of using emulsions or microemulsions in analytical chemistry are that they do not require the previous destruction of the sample matrix or the use of organic solvents as diluents, and behave similarly to aqueous solutions, frequently allowing the use of aqueous standard solutions for calibration. However, it appears that there are many contradictory concepts and misunderstandings often related to terms definition when referring to such systems. The main aim of this review is to outline the differences between these two aggregates and to give an overview of the most recent advances on their analytical applications with emphasis on the potentiality of the on-line emulsification processes. Copyright © 2012 Elsevier B.V. All rights reserved.

Eudragit RS PO nanoparticles for sustained release of pyridostigmine bromide

NASA Astrophysics Data System (ADS)

Hoobakht, Fatemeh; Ganji, Fariba; Vasheghani-Farahani, Ebrahim; Mousavi, Seyyed Mohammad

2013-09-01

Pyridostigmine bromide (PB) is an inhibitor of cholinesterase, which is used in the treatment of myasthenia gravis and administered for protection against exposure to toxic nerve agents. Tests were done to investigate prolonging the half-life of PB and improving its release behavior. PB was loaded in nanoparticles (NPs) of Eudragit RS PO (Eu-RS) prepared using the technique of quasi emulsion solvent diffusion. Variables of output power of the sonicator, bath temperature and mixing time, were chosen as the optimization factors to obtain the minimum sized NPs. In addition, emulsions were tested at different ratios of drug-to-polymer by dynamic light scattering to determine size and zeta potential of NPs. UV-spectroscopy was used to determine PB content of the NPs. Drug-loaded NPs were characterized by scanning electron microscopy, X-ray diffraction, and Fourier transform infrared spectra. Results determined that mixing time had a significant impact on the size of Eu-RS NPs, but power output of sonicator and bath temperature had no significant effect. The particle size obtained at the optimum condition (power output of 70 W, bath temperature of 33 °C, and mixing time of 7 min) was less than 200 nm (optimum sizes were 138.9 and 179.5 nm for Eu-RS and PB-loaded Eu-RS NPs, respectively). The optimum PB-loaded Eu-RS NPs at the PB to Eu-RS weight ratio of 1-4 and 20 % of loaded PB released from the nanocarriers within 100 h.

Increased rate of solvent diffusion in a prototypical supramolecular gel measured on the picosecond timescale.

PubMed

Seydel, Tilo; Edkins, Robert M; Jones, Christopher D; Foster, Jonathan A; Bewley, Robert; Aguilar, Juan A; Edkins, Katharina

2018-06-14

Solvent diffusion in a prototypical supramolecular gel probed by quasi-elastic neutron scattering on the picosecond timescale is faster than that in the respective bulk solvent. This phenomenon is hypothesized to be due to disruption of the hydrogen bonding of the solvent by the large hydrophobic surface of the gel network.

Synthesis of half-sphere/half-funnel-shaped silica structures by reagent localization and the role of water in shape control

DOE PAGES

Datskos, Panos; Polizos, Georgios; Cullen, David A.; ...

2016-11-11

Role of water and ammonium hydroxide is investigated in evolution of shape of silica structures in the polyvinylpyrrolidone-pentanol emulsion droplet system. Shape control of silica structures is demonstrated by localization of the reagents. A uniform dispersion of reagents provided straight silica rods, while localization of the reagents at the emulsion droplet periphery provided a new type of structures half sphere-half funnel. The absence of water in the initial stages prompted a different nucleation process for the structure growth compared to when water was present in the intial stages. Effect of effective water concentration appeared to be related to the easemore » of diffusion of silica percursor inside the emulsion droplet,i.e., the higher the water concentration, the lower the silica precursor diffusion. Additionally, mixing the reagents in different combinations before adding to the reaction mixture also affected the silica structure thickness, length, and shape.« less

Synthesis of half-sphere/half-funnel-shaped silica structures by reagent localization and the role of water in shape control

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

Datskos, Panos; Polizos, Georgios; Cullen, David A.

Role of water and ammonium hydroxide is investigated in evolution of shape of silica structures in the polyvinylpyrrolidone-pentanol emulsion droplet system. Shape control of silica structures is demonstrated by localization of the reagents. A uniform dispersion of reagents provided straight silica rods, while localization of the reagents at the emulsion droplet periphery provided a new type of structures half sphere-half funnel. The absence of water in the initial stages prompted a different nucleation process for the structure growth compared to when water was present in the intial stages. Effect of effective water concentration appeared to be related to the easemore » of diffusion of silica percursor inside the emulsion droplet,i.e., the higher the water concentration, the lower the silica precursor diffusion. Additionally, mixing the reagents in different combinations before adding to the reaction mixture also affected the silica structure thickness, length, and shape.« less

Determination of mean droplet sizes of water-in-oil emulsions using an Earth's field NMR instrument.

PubMed

Fridjonsson, Einar O; Flux, Louise S; Johns, Michael L

2012-08-01

The use of the Earth's magnetic field (EF) to conduct nuclear magnetic resonance (NMR) experiments has a long history with a growing list of applications (e.g. ground water detection, diffusion measurements of Antarctic sea ice). In this paper we explore whether EFNMR can be used to accurately and practically measure the mean droplet size () of water-in-oil emulsions (paraffin and crude oil). We use both pulsed field gradient (PFG) measurements of restricted self-diffusion and T₂ relaxometry, as appropriate. T₂ relaxometry allows the extension of droplet sizing ability below the limits set by the available magnetic field gradient strength of the EFNMR apparatus. A commercially available bench-top NMR spectrometer is used to verify the results obtained using the EFNMR instrument, with good agreement within experimental error, seen between the two instruments. These results open the potential for further investigation of the application of EFNMR for emulsion droplet sizing. Copyright © 2012 Elsevier Inc. All rights reserved.

Formulation and optimization by experimental design of eco-friendly emulsions based on d-limonene.

PubMed

Pérez-Mosqueda, Luis M; Trujillo-Cayado, Luis A; Carrillo, Francisco; Ramírez, Pablo; Muñoz, José

2015-04-01

d-Limonene is a natural occurring solvent that can replace more pollutant chemicals in agrochemical formulations. In the present work, a comprehensive study of the influence of dispersed phase mass fraction, ϕ, and of the surfactant/oil ratio, R, on the emulsion stability and droplet size distribution of d-limonene-in-water emulsions stabilized by a non-ionic triblock copolymer surfactant has been carried out. An experimental full factorial design 3(2) was conducted in order to optimize the emulsion formulation. The independent variables, ϕ and R were studied in the range 10-50 wt% and 0.02-0.1, respectively. The emulsions studied were mainly destabilized by both creaming and Ostwald ripening. Therefore, initial droplet size and an overall destabilization parameter, the so-called turbiscan stability index, were used as dependent variables. The optimal formulation, comprising minimum droplet size and maximum stability was achieved at ϕ=50 wt%; R=0.062. Furthermore, the surface response methodology allowed us to obtain the formulation yielding sub-micron emulsions by using a single step rotor/stator homogenizer process instead of most commonly used two-step emulsification methods. In addition, the optimal formulation was further improved against Ostwald ripening by adding silicone oil to the dispersed phase. The combination of these experimental findings allowed us to gain a deeper insight into the stability of these emulsions, which can be applied to the rational development of new formulations with potential application in agrochemical formulations. Copyright © 2015 Elsevier B.V. All rights reserved.

Emulsion Solvent Evaporation-Induced Self-Assembly of Block Copolymers Containing pH-Sensitive Block.

PubMed

Wu, Yuqing; Wang, Ke; Tan, Haiying; Xu, Jiangping; Zhu, Jintao

2017-09-26

A simple yet efficient method is developed to manipulate the self-assembly of pH-sensitive block copolymers (BCPs) confined in emulsion droplets. Addition of acid induces significant variation in morphological transition (e.g., structure and surface composition changes) of the polystyrene-block-poly(4-vinylpyridine) (PS-b-P4VP) assemblies, due to the hydrophobic-hydrophilic transition of the pH-sensitive P4VP block via protonation. In the case of pH > pKa (P4VP) (pKa (P4VP) = 4.8), the BCPs can self-assemble into pupa-like particles because of the nearly neutral wetting of PS and P4VP blocks at the oil/water interface. As expected, onion-like particles obtained when pH is slightly lower than pKa (P4VP) (e.g., pH = 3.00), due to the interfacial affinity to the weakly hydrophilic P4VP block. Interestingly, when pH was further decreased to ∼2.5, interfacial instability of the emulsion droplets was observed, and each emulsion droplet generated nanoscale assemblies including vesicles, worm-like and/or spherical micelles rather than a nanostructured microparticle. Furthermore, homopolymer with different molecular weights and addition ratio are employed to adjust the interactions among copolymer blocks. By this means, particles with hierarchical structures can be obtained. Moreover, owing to the kinetically controlled processing, we found that temperature and stirring speed, which can significantly affect the kinetics of the evaporation of organic solvent and the formation of particles, played a key role in the morphology of the assemblies. We believe that manipulation of the property for the aqueous phase is a promising strategy to rationally design and fabricate polymeric assemblies with desirable shapes and internal structures.

Preparation and Characterization of Polymeric Nanoparticles: An Interdisciplinary Experiment

ERIC Educational Resources Information Center

Ramalho, Maria J.; Pereira, M. Carmo

2016-01-01

In this work, a laboratory experiment to introduce graduate students to nanotechnology is described. Students prepared poly(lactic-"co"-glycolic acid) (PLGA) nanoparticles using two different synthesis procedures, a single and a double emulsion-solvent evaporation method. The students also performed a physicochemical characterization of…

The high water solubility of inclusion complex of taxifolin-γ-CD prepared and characterized by the emulsion solvent evaporation and the freeze drying combination method.

PubMed

Zu, Yuangang; Wu, Weiwei; Zhao, Xiuhua; Li, Yong; Zhong, Chen; Zhang, Yin

2014-12-30

This study selected γ-cyclodextrin (γ-CD) as the inclusion material and prepared inclusion complex of taxifolin-γ-CD by the emulsion solvent evaporation and the freeze drying combination method to achieve the improvement of the solubility and oral bioavailability of taxifolin. We selected ethyl acetate as the oil phase, deionized water as the water phase. The taxifolin emulsion was prepared using adjustable speed homogenate machine in the process of this experiment, whose particle size was related to the concentration of taxifolin solution, the volume ratio of water phase to oil phase, the speed and time of homogenate. We knew through the single-factor test that, the optimum conditions were: the concentration of taxifolin solution was 40 mg/ml, the volume ratio of water phase to oil phase was 1.5, the speed of homogenate was 5,000 rpm, the homogenate time was 11 min. Taxifolin emulsion with a MPS of 142.5 nm was obtained under the optimum conditions, then the high-concentration taxifolin solution (3mg/ml) was obtained by the rotary evaporation process. Finally, the inclusion complex of taxifolin-γ-CD was prepared by vacuum freeze-dry. The characteristics of the inclusion complex of taxifolin-γ-CD were analyzed using SEM, FTIR, XRD, DSC, and TG. The FTIR results analyzed the interaction of taxifolin and γ-CD and determined the molecular structure of the inclusion complex of taxifolin-γ-CD. The analysis results of XRD, DSC and TG indicated that the inclusion complex of taxifolin-γ-CD was obtained and showed significantly different characteristics with taxifolin. In addition, dissolving capability test, antioxidant capacity test, solvent residue test were also carried out. The experimental datas showed that the solubility of inclusion complex of taxifolin-γ-CD at 25°C and 37°C were about 18.5 times and 19.8 times of raw taxifolin, the dissolution rate of inclusion complex of taxifolin-γ-CD were about 2.84 times of raw taxifolin, the bioavailability of inclusion complex of taxifolin-γ-CD increased 3.72 times compared with raw taxifolin, and the antioxidant capacity of inclusion complex of taxifolin-γ-CD was also superior to raw taxifolin. Furthermore, the amounts of residual solvent of the inclusion complex of taxifolin-γ-CD were suitable for pharmaceutical use. These results suggested that inclusion complex of taxifolin-γ-CD may have potential value to become a new oral taxifolin formulation with high solubility. Copyright © 2014 Elsevier B.V. All rights reserved.

The effects of esterified solvents on the diffusion of a model compound across human skin: an ATR-FTIR spectroscopic study.

PubMed

McAuley, W J; Chavda-Sitaram, S; Mader, K T; Tetteh, J; Lane, M E; Hadgraft, J

2013-04-15

Attenuated total reflectance Fourier transform infrared (ATR-FTIR) spectroscopy has been used to investigate the effects of three fatty acid esters on skin permeation. Propylene glycol diperlargonate (DPPG), isopropyl myristate (IPM) and isostearyl isostearate (ISIS) were selected as pharmaceutically relevant solvents with a range of lipophilicities and cyanophenol (CNP) was used as a model drug. The resultant data were compared with that obtained when water was used as the solvent. The diffusion of CNP, DPPG and IPM across epidermis was successfully described by a Fickian model. When ISIS was used as a solvent Fickian behaviour was only obtained across isolated stratum corneum suggesting that the hydrophilic layers of the epidermis interfere with the permeation of the hydrophobic ISIS. The diffusion coefficients of CNP across epidermis in the different solvents were not significantly different. Using chemometric data analysis diffusion profiles for the solvents were deconvoluted from that of the skin and modelled. Each of these solvents was found to diffuse at a faster rate across the skin than CNP. DPPG considerably increased the concentration of CNP in the stratum corneum in comparison with the other solvents indicating strong penetration enhancer potential. In contrast IPM produced a similar CNP concentration in the stratum corneum to water with ISIS resulting in a lower CNP concentration suggesting negligible enhancement and penetration retardation effects for these two solvents respectively. Copyright © 2013 Elsevier B.V. All rights reserved.

Physicochemical properties of macrogol ointment and emulsion ointment blend developed for regulation of water absorption.

PubMed

Noda, Yasuhiro; Watanabe, Kazuya; Sanagawa, Akimasa; Sobajima, Yu; Fujii, Satoshi

2011-10-31

Pressure ulcers can form with excess pressure and shearing stress on skin tissue. Because pressure ulcer is often accompanies by exudates, selection of appropriate topical emulsion ointment is difficult. Blended ointments consisting of emulsion base and water-soluble base are clinically used for adjustment of wound moist environment. Because regulating the amount of wound exudates can enhance treatment efficacy, two new blended ointments were developed. LY-SL blended ointment consisted of lysozyme hydrochloride water-in-oil (w/o) emulsion (LY-cream) and sulfadiazine macrogol (polyethylene glycol) ointment (SL-pasta). TR-SL blended ointment consisted of tretinoin tocoferil oil-in-water (o/w) emulsion (TR-cream) and SL-pasta (TR-SL). LY-SL and TR-SL were applied to Franz diffusion cell with cellulose membranes for the evaluation of water absorption characteristics at 32 °C. Water absorption rate constants (mg/cm(2)/min(0.5)) were 12.5, 16.3 and 34.6 for LY-cream, TR-cream and SL-pasta, respectively. Water absorption rate constants for LY-SL and TR-SL (SL-pasta 70%) exhibited intermediate values of 21.2 and 27.2, as compared to each ointment alone, respectively. Because amount of water absorbed was linearly related to square root of time, it was suggested that water-absorbable macrogol was surrounded by oily ingredients forming matrix structure. This diffusion-limited structure may regulate water absorption capacity. This is the first report of physicochemical properties of macrogol ointment and emulsion ointment blend developed for regulation of water absorption. The blended ointment can properly regulate amount of exudates in wounds and may be useful for treatment of pressure ulcers. Copyright © 2011 Elsevier B.V. All rights reserved.

Biofoam

DOEpatents

Morrison, Robert L.

1995-01-01

Biofoam is a rigid, opaque microcellular organic foam made from organic materials derived from natural products and biological organisms. Typical organic materials are agar, agarose, gelatin, algin, alginates, gellan gum, and microcrystalline cellulose. The organic material is dissolved in a polar solvent, typically water, and the solution can be gelled immediately. The gel is frozen and freeze-dried to form the biofoam. Alternatively, a nonpolar solvent is added to the solution and emulsified. The resulting emulsion is then gelled, frozen, and freeze-dried. A variety of crystalline, fibrous, or metallic additives may be added to produce lightweight composite materials with enhanced strength and insulating properties. The amount of dilution of the organic material in the solvent(s) determines the density of the resulting biofoams, which ranges from about 1.0 mg/cm.sup.3 to about 500 mg/cm.sup.3.

Phase recording for formation of holographic optical elements on silver-halide photographic emulsions

NASA Astrophysics Data System (ADS)

Ganzherli, Nina M.; Gulyaev, Sergey N.; Maurer, Irina A.; Chernykh, Dmitrii F.

2009-05-01

Holographic fabrication methods of regular and nonregular relief-phase structures on silver-halide photographic emulsions are considered. Methods of gelatin photodestruction under short-wave ultra-violet radiation and chemical hardening with the help of dichromated solutions were used as a technique for surface relief formation. The developed techniques permitted us to study specimens of holographic diffusers and microlens rasters with small absorption and high light efficiency.

Non-destructive monitoring of creaming of oil-in-water emulsion-based formulations using magnetic resonance imaging.

PubMed

Onuki, Yoshinori; Horita, Akihiro; Kuribayashi, Hideto; Okuno, Yoshihide; Obata, Yasuko; Takayama, Kozo

2014-07-01

A non-destructive method for monitoring creaming of emulsion-based formulations is in great demand because it allows us to understand fully their instability mechanisms. This study was aimed at demonstrating the usefulness of magnetic resonance (MR) techniques, including MR imaging (MRI) and MR spectroscopy (MRS), for evaluating the physicochemical stability of emulsion-based formulations. Emulsions that are applicable as the base of practical skin creams were used as test samples. Substantial creaming was developed by centrifugation, which was then monitored by MRI. The creaming oil droplet layer and aqueous phase were clearly distinguished by quantitative MRI by measuring T1 and the apparent diffusion coefficient. Components in a selected volume in the emulsions could be analyzed using MRS. Then, model emulsions having different hydrophilic-lipophilic balance (HLB) values were tested, and the optimal HLB value for a stable dispersion was determined. In addition, the MRI examination enables the detection of creaming occurring in a polyethylene tube, which is commonly used for commercial products, without losing any image quality. These findings strongly indicate that MR techniques are powerful tools to evaluate the physicochemical stability of emulsion-based formulations. This study will make a great contribution to the development and quality control of emulsion-based formulations.

Characterization of starch Pickering emulsions for potential applications in topical formulations.

PubMed

Marku, Diana; Wahlgren, Marie; Rayner, Marilyn; Sjöö, Malin; Timgren, Anna

2012-05-30

The aim of this work has been to characterize starch based Pickering emulsions as a first step to evaluate their possible use as vehicles for topical drug delivery. A minor phase study of emulsions with high oil content has been performed. Emulsion stability against coalescence over eight weeks and after mild centrifugation treatment has been studied. The particle size, rheological properties and in vitro skin penetration of emulsions containing three different oils (Miglyol, paraffin and sheanut oil) was investigated. It was shown that it is possible to produce oil in water starched stabilised Pickering emulsions with oil content as high as 56%. Furthermore, this emulsions show good stability during storage over eight weeks and towards mild centrifugation. The particle size of the systems are only dependent on the ratio between oil and starch and for liquid oils the type of oil do not affect the particle size. The type of oil also affects the cosmetic and rheological properties of the creams but did not affect the transdermal diffusion in in vitro tests. However, it seems as if the Pickering emulsions affected the transport over the skin, as the flux was twice that of what has been previously reported for solutions. Copyright © 2012 Elsevier B.V. All rights reserved.

DELIVERY OF WATER-SOLUBLE DRUGS USING ACOUSTICALLY-TRIGGERED, PERFLUOROCARBON DOUBLE EMULSIONS

PubMed Central

Fabiilli, Mario L.; Lee, James A.; Kripfgans, Oliver D.; Carson, Paul L.; Fowlkes, J. Brian

2010-01-01

Purpose Ultrasound can be used to release a therapeutic payload encapsulated within a perfluorocarbon (PFC) emulsion via acoustic droplet vaporization (ADV), a process whereby the PFC phase is vaporized and the agent is released. ADV-generated microbubbles have been previously used to selectively occlude blood vessels in vivo. The coupling of ADV-generated drug delivery and occlusion has therapeutically, synergistic potentials. Methods Micron-sized, water-in-PFC-in-water (W1/PFC/W2) emulsions were prepared in a two-step process using perfluoropentane (PFP) or perfluorohexane (PFH) as the PFC phase. Fluorescein or thrombin was contained in the W1 phase. Results Double emulsions containing fluorescein in the W1 phase displayed a 5.7±1.4 fold and 8.2±1.3 fold increase in fluorescein mass flux, as measured using a Franz diffusion cell, after ADV for the PFP and PFH emulsions, respectively. Thrombin was stably retained in four out of five double emulsions. For three out of five formulations tested, the clotting time of whole blood decreased, in a statistically significant manner (p < 0.01), when incubated with thrombin-loaded emulsions exposed to ultrasound compared to emulsions not exposed to ultrasound. Conclusions ADV can be used to spatially and temporally control the delivery of water-soluble compounds formulated in PFC double emulsions. Thrombin release could extend the duration of ADV-generated, microbubble occlusions. PMID:20872050

Hollow microspheres of diclofenac sodium - a gastroretentive controlled delivery system.

PubMed

Bv, Basavaraj; R, Deveswaran; S, Bharath; Abraham, Sindhu; Furtado, Sharon; V, Madhavan

2008-10-01

Most of the floating systems have an inherent drawback of high variability in the GI transit time, invariably affecting the bioavailability of drug. To overcome it, a multiple unit floating system with extended GI transit time, capable of distributing widely throughout the GIT for effective enteric release of the drug has been sought. Microballoons loaded with drug in their outer polymer shells were prepared by novel emulsion solvent diffusion method. The ethanol: dicloromethane solution of drug and Eudragit-S were poured into an aqueous solution of PVA that was thermally controlled at 40 degrees C. The gas phase generated in the dispersed polymer droplet by the evaporation of solvent formed an internal cavity in the microsphere of the polymer with the drug. The flowability of the resulting microballoons improved when compared to pure drug. The microballoons on floatation along with the surfactant, floated continuously for more than 12 hours in the acidic medium in-vitro conditions. The in-vitro drug release profile of the formulation in the simulated gastric buffer showed no drug release, which emphasizes the enteric release property and in simulated intestinal buffer, a slow and controlled drug release of 60 to 84% was obtained over a period of 8 hours. Drug release was significantly affected by increased drug to polymer concentration at pH 6.8. The formulation was found to be physically and chemically stable as per the ICH guidelines.

RIR-MAPLE deposition of conjugated polymers and hybrid nanocomposites for application to optoelectronic devices

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

Stiff-Roberts, Adrienne D.; Pate, Ryan; McCormick, Ryan

2012-07-30

Resonant infrared matrix-assisted pulsed laser evaporation (RIR-MAPLE) is a variation of pulsed laser deposition that is useful for organic-based thin films because it reduces material degradation by selective absorption of infrared radiation in the host matrix. A unique emulsion-based RIR-MAPLE approach has been developed that reduces substrate exposure to solvents and provides controlled and repeatable organic thin film deposition. In order to establish emulsion-based RIR-MAPLE as a preferred deposition technique for conjugated polymer or hybrid nanocomposite optoelectronic devices, studies have been conducted to demonstrate the value added by the approach in comparison to traditional solution-based deposition techniques, and this workmore » will be reviewed. The control of hybrid nanocomposite thin film deposition, and the photoconductivity in such materials deposited using emulsion-based RIR-MAPLE, will also be reviewed. The overall result of these studies is the demonstration of emulsion-based RIR-MAPLE as a viable option for the fabrication of conjugated polymer and hybrid nanocomposite optoelectronic devices that could yield improved device performance.« less

Electrospun composite matrices of poly(ε-caprolactone)-montmorillonite made using tenside free Pickering emulsions.

PubMed

Samanta, Archana; Takkar, Sonam; Kulshreshtha, Ritu; Nandan, Bhanu; Srivastava, Rajiv K

2016-12-01

The production of composite electrospun matrices of poly(ε-caprolactone) (PCL) using an emulsifier-free emulsion, made with minimal organic solvent, as precursor is reported. Pickering emulsions of PCL were prepared using modified montmorillonite (MMT) clay as the stabilizer. Hydrophobic tallow group of the modified MMT clay resulted in analogous interaction of clay with oil and aqueous phase and its adsorption at the interface to provide stability to the resultant emulsion. Composite fibrous matrices of PCL and MMT were produced using electrospinning under controlled conditions. The fiber fineness was found to alter with PCL concentration and volume fraction of the aqueous and oil phases. A higher tensile strength and modulus was obtained with inclusion of MMT in PCL electrospun matrix in comparison to a matrix made using neat PCL. The presence of clay in the fibrous matrix did not change the cell proliferation efficiency in comparison to neat PCL matrix. Composite fibrous matrices of PCL/MMT bearing enhanced tensile properties may find applications in areas other than tissue engineering for example food packaging and filtration. Copyright © 2016 Elsevier B.V. All rights reserved.

Drug delivery monitoring by photoacoustic tomography with an ICG encapsulated double emulsion

NASA Astrophysics Data System (ADS)

Rajian, Justin Rajesh; Fabiilli, Mario L.; Fowlkes, J. Brian; Carson, Paul L.; Wang, Xueding

2011-07-01

The absorption spectrum of indocyanine green (ICG), a nontoxic dye used for medical diagnostics, depends upon its concentration as well as the nature of its environment, i.e., the solvent medium into which it is dissolved. In blood, ICG binds with plasma proteins, thus causing changes in its photoacoustic spectrum. We successfully encapsulated ICG in an ultrasound-triggerable perfluorocarbon double emulsion that prevents ICG from binding with plasma proteins. Photoacoustic spectral measurements on point target as well as 2-D photoacoustic images of blood vessels revealed that the photoacoustic spectrum changes significantly in blood when the ICG-loaded emulsion undergoes acoustic droplet vaporization (ADV), which is the conversion of liquid droplets into gas bubbles using ultrasound. We propose that these changes in the photoacoustic spectrum of the ICG emulsion in blood, coupled with photoacoustic tomography, could be used to spatially and quantitatively monitor ultrasound initiated drug delivery. In addition, we suggest that the photoacoustic spectral change induced by ultrasound exposure could also be used as contrast in photoacoustic imaging to obtain a background free image.

Hydroxyapatite-armored poly(ε-caprolactone) microspheres and hydroxyapatite microcapsules fabricated via a Pickering emulsion route.

PubMed

Fujii, Syuji; Okada, Masahiro; Nishimura, Taiki; Maeda, Hayata; Sugimoto, Tatsuya; Hamasaki, Hiroyuki; Furuzono, Tsutomu; Nakamura, Yoshinobu

2012-05-15

Hydroxyapatite (HAp) nanoparticle-armored poly(ε-caprolactone) (PCL) microspheres were fabricated via a "Pickering-type" emulsion solvent evaporation method in the absence of any molecular surfactants. It was clarified that the interaction between carbonyl/carboxylic acid groups of PCL and the HAp nanoparticles at an oil-water interface played a crucial role in the preparation of the stable Pickering-type emulsions and the HAp nanoparticle-armored microspheres. The HAp nanoparticle-armored PCL microspheres were characterized in terms of size, size distribution, morphology, and chemical compositions using scanning electron microscopy, laser diffraction, energy dispersive X-ray microanalysis, and thermogravimetric analysis. The presence of HAp nanoparticles at the surface of the microspheres was confirmed by scanning electron microscopy and energy dispersive X-ray microanalysis. Pyrolysis of the PCL cores led to the formation of the corresponding HAp hollow microcapsules. Copyright © 2012 Elsevier Inc. All rights reserved.

Friction and Wear Modifiers Using Solvent Partitioning of Hydrophilic Surface-interactive Chemicals Contained in Boundary Layer-targeted Emulsions

NASA Technical Reports Server (NTRS)

Richmond, Robert Chafee (Inventor); Schramm, Jr., Harry F. (Inventor); Defalco, Francis G. (Inventor)

2013-01-01

A wear and/or friction reducing additive for a lubricating fluid in which the additive is a combination of a moderately hydrophilic single-phase compound and an anti-wear and/or anti-friction aqueous salt solution. The aqueous salt solution produces a coating on boundary layer surfaces. The lubricating fluid can be an emulsion-free hydrophobic oil, hydraulic fluid, antifreeze, or water. Preferably, the moderately hydrophilic single-phase compound is sulfonated castor oil and the aqueous salt solution additionally contains boric acid and zinc oxide. The emulsions produced by the aqueous salt solutions, the moderately hydrophilic single-phase compounds, or the combination thereof provide targeted boundary layer organizers that significantly enhance the anti-wear and/or anti-friction properties of the base lubricant by decreasing wear and/or friction of sliding and/or rolling surfaces at boundary layers.

Safe, in situ methodologies for the destruction of triacetone triperoxide and other explosive peroxides

NASA Technical Reports Server (NTRS)

Geiger, Cherie L. (Inventor); Sigman, Michael (Inventor); Clausen, III, Christian (Inventor); Fidler, Rebecca (Inventor)

2011-01-01

Triacetone triperoxide (TATP) and other explosives of the peroxide family are safely degraded in situ. Nano and micron size metal particles in an elemental state include pure iron and magnesium or iron and magnesium particles that are mechanically alloyed with palladium and nickel. The metal particles are used in both the elemental state and in emulsions that are made from water, a hydrophobic solvent, such as corn oil, and a food-grade nonionic surfactant. The neat metals and emulsified zero valent metals (EZVM) safely degrade TATP with the major degradation product being acetone. The EZVM system absorbs and dissolves the TATP into the emulsion droplets where TATP degradation occurs. EZVM systems are ideal for degrading dry TATP crystals that may be present on a carpet or door entrance. Both the neat metal system and the emulsion system (EZVM) degrade TATP in an aqueous slurry.

Friction and Wear Modifiers Using Solvent Partitioning of Hydrophilic Surface-Interactive Chemicals Contained in Boundary Layer-Targeted Emulsions

NASA Technical Reports Server (NTRS)

Defalco, Francis G. (Inventor); Richmond, Robert Chaffee (Inventor); Schramm, Jr., Harry F. (Inventor)

2017-01-01

A wear and/or friction reducing additive for a lubricating fluid in which the additive is a combination of a moderately hydrophilic single-phase compound and an anti-wear and/or anti-friction aqueous salt solution. The aqueous salt solution produces a coating on boundary layer surfaces. The lubricating fluid can be an emulsion-free hydrophobic oil, hydraulic fluid, antifreeze, water, or a water-based lubricant. Preferably, the moderately hydrophilic single-phase compound is sulfonated castor oil and the aqueous salt solution additionally contains boric acid and zinc oxide. The emulsions produced by the aqueous salt solutions, the moderately hydrophilic single-phase compounds, or the combination thereof provide targeted boundary layer organizers that significantly enhance the anti-wear and/or anti-friction properties of the base lubricant by decreasing wear and/or friction of sliding and/or rolling surfaces at boundary layers.

Friction and Wear Modifiers Using Solvent Partitioning of Hydrophilic Surface-Interactive Chemicals Contained in Boundary Layer-Targeted Emulsions

NASA Technical Reports Server (NTRS)

Defalco, Francis G. (Inventor); Richmond, Robert Chaffee (Inventor); Schramm, Harry F., Jr. (Inventor)

2016-01-01

A wear and/or friction reducing additive for a lubricating fluid in which the additive is a combination of a moderately hydrophilic single-phase compound and an anti-wear and/or anti-friction aqueous salt solution. The aqueous salt solution produces a coating on boundary layer surfaces. The lubricating fluid can be an emulsion-free hydrophobic oil, hydraulic fluid, antifreeze, or water. Preferably, the moderately hydrophilic single-phase compound is sulfonated castor oil and the aqueous salt solution additionally contains boric acid and zinc oxide. The emulsions produced by the aqueous salt solutions, the moderately hydrophilic single-phase compounds, or the combination thereof provide targeted boundary layer organizers that significantly enhance the anti-wear and/or anti-friction properties of the base lubricant by decreasing wear and/or friction of sliding and/or rolling surfaces at boundary layers.

Influence of palmitoyl pentapeptide and Ceramide III B on the droplet size of nanoemulsion

NASA Astrophysics Data System (ADS)

Sondari, Dewi; Haryono, Agus; Harmami, Sri Budi; Randy, Ahmad

2010-05-01

The influence of the Palmitoyl Pentapeptide (PPp) and Ceramide IIIB (Cm III B) as active ingredients on the droplet size of nano-emulsion was studied using different kinds of oil (avocado oil, sweet almond oil, jojoba oil, mineral oil and squalene). The formation of nano-emulsions were prepared in water mixed non ionic surfactant/oils system using the spontaneous emulsification mechanism. The aqueous solution, which consist of water and Tween® 20 as a hydrophilic surfactant was mixed homogenously. The organic solution, which consist of oil and Span® 80 as a lipophilic surfactant was mixed homogenously in ethanol. Ethanol was used as a water miscible solvent, which can help the formation of nano-emulsion. The oil phase (containing the blend of surfactant Span® 80, ethanol, oil and active ingredient) and the aqueous phase (containing water and Tween® 20) were separately prepared at room temperatures. The oil phase was slowly added into aqueous phase under continuous mechanical agitation (18000 rpm). All samples were subsequently homogenized with Ultra-Turrax for 30 minutes. The characterizations of nano-emulsion were carried out using photo-microscope and particle size analyzer. Addition of active ingredients on the formation of nano-emulsion gave smallest droplet size compared without active ingredients addition on the formation of nano-emulsion. Squalene oil with Palmitoyl Pentapeptide (PPm) and Ceramide IIIB (Cm IIIB) gave smallest droplet size (184.0 nm) compared without Palmitoyl Pentapeptide and Ceramide IIIB (214.9 nm), however the droplets size of the emulsion prepared by the other oils still in the range of nano-emulsion (below 500 nm). The stability of nano-emulsion was observed using two methods. In one method, the stability of nano-emulsion was observed for three months at temperature of 5°C and 50°C, while in the other method, the stability nano-emulsion was observed by centrifuged at 12000 rpm for 30 minutes. Nanoemulsion with active ingredient was remained stable even when stored until three months. Coalescence process between the droplets was not occurred significantly and droplet size was still below 500 nm. Over all, the emulsion remained stable, even it was centrifuged at 12000 rpm for 30 minutes.

Reverse micelle-loaded lipid nano-emulsions: new technology for nano-encapsulation of hydrophilic materials.

PubMed

Anton, Nicolas; Mojzisova, Halina; Porcher, Emilien; Benoit, Jean-Pierre; Saulnier, Patrick

2010-10-15

This study presents novel, recently patented technology for encapsulating hydrophilic species in lipid nano-emulsions. The method is based on the phase-inversion temperature method (the so-called PIT method), which follows a low-energy and solvent-free process. The nano-emulsions formed are stable for months, and exhibit droplet sizes ranging from 10 to 200 nm. Hydrophilic model molecules of fluorescein sodium salt are encapsulated in the oily core of these nano-emulsion droplets through their solubilisation in the reverse micellar system. As a result, original, multi-scaled nano-objects are generated with a 'hydrophilic molecule in a reverse-micelles-in-oil-in-water' structure. Once fluorescein has been encapsulated it remains stable, for thermodynamic reasons, and the encapsulation yields can reach 90%. The reason why such complex objects can be formed is due to the soft method used (PIT method) which allows the conservation of the structure of the reverse micelles throughout the formulation process, up to their entrapment in the nano-emulsion droplets. In this study, we focus the investigation on the process itself, revealing its potential and limits. Since the formulation of nanocarriers for the encapsulation of hydrophilic substances still remains a challenge, this study may constitute a significant advance in this field. Copyright 2010 Elsevier B.V. All rights reserved.

Uniform discotic wax particles via electrospray emulsification.

PubMed

Mejia, Andres F; He, Peng; Luo, Dawei; Marquez, Manuel; Cheng, Zhengdong

2009-06-01

We present a novel colloidal discotic system: the formation and self-assembling of wax microdisks with a narrow size distribution. Uniform wax emulsions are first fabricated by electrospraying of melt alpha-eicosene. The size of the emulsions can be flexibly tailored by varying the flow rate of the discontinuous phase, its electric conductivity, and the applied voltage. The process of entrainment of wax droplets, vital for obtaining uniform emulsions, is facilitated by the reduction of air-water surface tension and the density of the continuous phase. Then uniform wax discotic particles are produced via phase transition, during which the formation of a layered structure of the rotator phase of wax converts the droplets, one by one, into oblate particles. The time span for the conversion from spherical emulsions to disk particles is linearly dependent on the size of droplets in the emulsion, indicating the growth of a rotator phase from surface to the center is the limiting step in the shape transition. Using polarized light microscopy, the self-assembling of wax disks is observed by increasing disk concentration and inducing depletion attraction among disks, where several phases, such as isotropic, condensed, columnar stacking, and self-assembly of columnar rods are present sequentially during solvent evaporation of a suspension drop.

Disposition of lipid-based formulation in the intestinal tract affects the absorption of poorly water-soluble drugs.

PubMed

Iwanaga, Kazunori; Kushibiki, Toshihiro; Miyazaki, Makoto; Kakemi, Masawo

2006-03-01

Solvent Green 3 (SG), a model poorly water-soluble compound, was orally administered to rats with soybean oil emulsion or the Self-microemulsifying drug delivery system (SMEDDS) composed of Gelucire44/14. The bioavailability of SG after oral administration with SMEDDS was 1.7-fold higher than that with soybean oil emulsion. The intestinal absorption of lipid-based formulations themselves was evaluated by the in situ closed loop method. The effect of lipase and bile salt on their absorption was also evaluated. SMEDDS itself was rapidly absorbed in the intestine even in the absence of lipase and bile salt, and the absorption was increased by the addition of lipase and bile salt. On the other hand, no soybean oil emulsion was absorbed in the absence of lipase and bile salt. However, mixed micelle prepared from emulsion by incubating soybean oil emulsion with lipase and bile salt was rapidly absorbed through the intestine. Without lipase and bile salt, SG was not absorbed after administration with soybean oil emulsion. Therefore, we concluded that the degradation of soybean oil emulsion was needed for SG to be absorbed through the intestine. Furthermore, we investigated the intestinal absorption of SG after oral administration to rats whose chylomicron synthesis were inhibited by pretreatment with colchicine. Colchicine completely inhibited the intestinal absorption of SG after administration with each lipid-based formulation, suggesting that SG was absorbed from the intestine via a lymphatic route. Absorption of the dosage formulation should be paid attention when poorly water-soluble drugs are orally administered with lipid-based formulation.

The secondary drying and the fate of organic solvents for spray dried dispersion drug product.

PubMed

Hsieh, Daniel S; Yue, Hongfei; Nicholson, Sarah J; Roberts, Daniel; Schild, Richard; Gamble, John F; Lindrud, Mark

2015-05-01

To understand the mechanisms of secondary drying of spray-dried dispersion (SDD) drug product and establish a model to describe the fate of organic solvents in such a product. The experimental approach includes characterization of the SDD particles, drying studies of SDD using an integrated weighing balance and mass spectrometer, and the subsequent generation of the drying curve. The theoretical approach includes the establishment of a Fickian diffusion model. The kinetics of solvent removal during secondary drying from the lab scale to a bench scale follows Fickian diffusion model. Excellent agreement is obtained between the experimental data and the prediction from the modeling. The diffusion process is dependent upon temperature. The key to a successful scale up of the secondary drying is to control the drying temperature. The fate of primary solvents including methanol and acetone, and their potential impurity such as benzene can be described by the Fickian diffusion model. A mathematical relationship based upon the ratio of diffusion coefficient was established to predict the benzene concentration from the fate of the primary solvent during the secondary drying process.

Air-assisted liquid-liquid microextraction using floating organic droplet solidification for simultaneous extraction and spectrophotometric determination of some drugs in biological samples through chemometrics methods

NASA Astrophysics Data System (ADS)

Farahmand, Farnaz; Ghasemzadeh, Bahar; Naseri, Abdolhossein

2018-01-01

An air assisted liquid-liquid microextraction by applying the solidification of a floating organic droplet method (AALLME-SFOD) coupled with a multivariate calibration method, namely partial least squares (PLS), was introduced for the fast and easy determination of Atenolol (ATE), Propanolol (PRO) and Carvedilol (CAR) in biological samples via a spectrophotometric approach. The analytes would be extracted from neutral aqueous solution into 1-dodecanol as an organic solvent, using AALLME. In this approach a low-density solvent with a melting point close to room temperature was applied as the extraction solvent. The emulsion was immediately formed by repeatedly pulling in and pushing out the aqueous sample solution and extraction solvent mixture via a 10-mL glass syringe for ten times. After centrifugation, the extractant droplet could be simply collected from the aqueous samples by solidifying the emulsion at a lower than the melting point temperature. In the next step, analytes were back extracted simultaneously into the acidic aqueous solution. Derringer and Suich multi-response optimization were utilized for simultaneous optimizing the parameters of three analytes. This method incorporates the benefits of AALLME and dispersive liquid-liquid microextraction considering the solidification of floating organic droplets (DLLME-SFOD). Calibration graphs under optimized conditions were linear in the range of 0.30-6.00, 0.32-2.00 and 0.30-1.40 μg mL- 1 for ATE, CAR and PRO, respectively. Other analytical parameters were obtained as follows: enrichment factors (EFs) were found to be 11.24, 16.55 and 14.90, and limits of detection (LODs) were determined to be 0.09, 0.10 and 0.08 μg mL- 1 for ATE, CAR and PRO, respectively. The proposed method will require neither a highly toxic chlorinated solvent for extraction nor an organic dispersive solvent in the application process; hence, it is more environmentally friendly.

Air-assisted liquid-liquid microextraction using floating organic droplet solidification for simultaneous extraction and spectrophotometric determination of some drugs in biological samples through chemometrics methods.

PubMed

Farahmand, Farnaz; Ghasemzadeh, Bahar; Naseri, Abdolhossein

2018-01-05

An air assisted liquid-liquid microextraction by applying the solidification of a floating organic droplet method (AALLME-SFOD) coupled with a multivariate calibration method, namely partial least squares (PLS), was introduced for the fast and easy determination of Atenolol (ATE), Propanolol (PRO) and Carvedilol (CAR) in biological samples via a spectrophotometric approach. The analytes would be extracted from neutral aqueous solution into 1-dodecanol as an organic solvent, using AALLME. In this approach a low-density solvent with a melting point close to room temperature was applied as the extraction solvent. The emulsion was immediately formed by repeatedly pulling in and pushing out the aqueous sample solution and extraction solvent mixture via a 10-mL glass syringe for ten times. After centrifugation, the extractant droplet could be simply collected from the aqueous samples by solidifying the emulsion at a lower than the melting point temperature. In the next step, analytes were back extracted simultaneously into the acidic aqueous solution. Derringer and Suich multi-response optimization were utilized for simultaneous optimizing the parameters of three analytes. This method incorporates the benefits of AALLME and dispersive liquid-liquid microextraction considering the solidification of floating organic droplets (DLLME-SFOD). Calibration graphs under optimized conditions were linear in the range of 0.30-6.00, 0.32-2.00 and 0.30-1.40μg mL -1 for ATE, CAR and PRO, respectively. Other analytical parameters were obtained as follows: enrichment factors (EFs) were found to be 11.24, 16.55 and 14.90, and limits of detection (LODs) were determined to be 0.09, 0.10 and 0.08μg mL -1 for ATE, CAR and PRO, respectively. The proposed method will require neither a highly toxic chlorinated solvent for extraction nor an organic dispersive solvent in the application process; hence, it is more environmentally friendly. Copyright © 2017 Elsevier B.V. All rights reserved.

Material research in microgravity

NASA Technical Reports Server (NTRS)

Langbein, D.

1984-01-01

A popular discussion is given of microgravity effects in engineering and medicine gained from Skylab experience. Areas covered include crystal growing, liquid surface properties, diffusion, ferromagnetism, and emulsions.

Biofoam

DOEpatents

Morrison, R.L.

1995-01-17

Biofoam is a rigid, opaque microcellular organic foam made from organic materials derived from natural products and biological organisms. Typical organic materials are agar, agarose, gelatin, algin, alginates, gellan gum, and microcrystalline cellulose. The organic material is dissolved in a polar solvent, typically water, and the solution can be gelled immediately. The gel is frozen and freeze-dried to form the biofoam. Alternatively, a nonpolar solvent is added to the solution and emulsified. The resulting emulsion is then gelled, frozen, and freeze-dried. A variety of crystalline, fibrous, or metallic additives may be added to produce lightweight composite materials with enhanced strength and insulating properties. The amount of dilution of the organic material in the solvent(s) determines the density of the resulting biofoams, which ranges from about 1.0 mg/cm[sup 3] to about 500 mg/cm[sup 3]. 4 figures.

Molecular dynamics simulation of solute diffusion in Lennard-Jones fluids

NASA Astrophysics Data System (ADS)

Yamaguchi, T.; Kimura, Y.; Hirota, N.

We performed a molecular dynamics (MD) simulation for a system of 5 solute molecules in 495 solvent molecules interacting through the Lennard-Jones (LJ) 12-6 potential, in order to study solvent density effects on the diffusion coefficients in supercritical fluids. The effects of the size of the solute and the strength of the solute-solvent attractive interaction on the diffusion coefficient of the solute were examined. The diffusion coefficients of the solute molecules were calculated at T = 1.5 (in the LJ reduced unit), slightly above the critical temperature, from rho = 0.1 to rho = 0.95, where rho is the number density in the LJ reduced unit. The memory function in the generalized Langevin equation was calculated, in order to know the molecular origin of the friction on a solute. The memory function is separated into fast and slow components. The former arises from the solute-solvent repulsive interaction, and is interpreted as collisional Enskog-like friction. The interaction strength dependence of the collisional friction is larger in the low- and medium-density regions, which is consistent with the 'clustering' picture, i.e., the local density enhancement due to the solute-solvent attractive interaction. However, the slow component of the memory function suppresses the effect of the local density on the diffusion coefficients, and as a result the effect of the attractive interaction is smaller on the diffusion coefficients than on the local density. Nonetheless, the solvent density dependence of the effect of the attraction on the diffusion coefficient varies with the local density, and it is concluded that the local density is the principal factor that determines the interaction strength dependence of the diffusion coefficient in the low- and medium-density regions (p < 0.6).

Comparison of non-toxic methods for creating beta-carotene encapsulated in PMMA nanoparticles

NASA Astrophysics Data System (ADS)

Dobrzanski, Christopher D.

Nano/microcapsules are becoming more prevalent in various industries such as drug delivery, cosmetics, etc. Current methods of particle formation often use toxic or carcinogenic/mutagenic/reprotoxic (CMR) chemicals. This study intends to improve upon existing methods of particle formation and compare their effectiveness in terms of entrapment efficiency, mean particle size, and yield utilizing only non-toxic chemicals. In this study, the solvent evaporation (SE), spontaneous emulsification, and spontaneous emulsion solvent diffusion (SESD) methods were compared in systems containing green solvents ethyl acetate, dimethyl carbonate or acetone. PMMA particles containing encapsulated beta carotene, an ultraviolet sensitive substance, were synthesized. It was desired to produce particles with minimum mean size and maximum yield and entrapment of beta carotene. The mass of the water phase, the mass of the polymer and the pumping or blending rate were varied for each synthesis method. The smallest particle sizes for SE and SESD both were obtained from the middle water phase sizes, 200 g and 100 g respectively. The particles obtained from the larger water phase in SESD were much bigger, about 5 microns in diameter, even larger than the ones obtained from SE. When varying the mass of PMMA used in each synthesis method, as expected, more PMMA led to larger particles. Increasing the blending rate in SE from 6,500 to 13,500 rpm had a minimal effect on average particle size, but the higher shear resulted in highly polydisperse particles (PDI = 0.87). By decreasing the pump rate in SESD, particles became smaller and had lower entrapment efficiency. The entrapment efficiencies of the particles were generally higher for the larger particles within a mode. Therefore, we found that minimizing the particle size while maximizing entrapment were somewhat contradictory goals. The solvent evaporation method was very consistent in terms of the values of mean particle size, yield, and entrapment efficiency. Comparing the synthesis methods, the smallest particles with the highest yield and entrapment efficiency were generated by the spontaneous emulsification method.

Novel one-pot facile technique for preparing nanoparticles modified with hydrophilic polymers on the surface via block polymer-assisted emulsification/evaporation process.

PubMed

Kanakubo, Yurie; Ito, Fuminori; Murakami, Yoshihiko

2010-06-15

In this paper, we describe the novel facile technique for preparing surface-modified nanoparticles via newly developed amphiphilic block polymer-assisted emulsification/evaporation process. The effects of both organic solvents (the dispersed phase) and stabilizer in the external continuous phase on the stability of o/w emulsion was firstly investigated to clarify the optimal conditions for stable emulsification/evaporation processes. We found that the organic solvent mixture having a density adjusted to be 1.00 g/cm(3) gave the highly stable o/w emulsion. Under the optimal conditions, the relatively monodisperse poly(ethylene glycol) (PEG)-modified poly(lactide-co-glycolide) (PLGA) nanoparticle was obtained and characterized. The introduction of PEG to the particle surface was suggested by the fact that the diameter and zeta potential of the particle increased as the amount of added block polymer increased. The facile method presented in this paper can be a universal tool for modifying the surface of nanoparticles, even though reactive groups are not present on the surface. Copyright 2010 Elsevier B.V. All rights reserved.

Whey protein/polysaccharide-stabilized emulsions: Effect of polymer type and pH on release and topical delivery of salicylic acid.

PubMed

Combrinck, Johann; Otto, Anja; du Plessis, Jeanetta

2014-06-01

Emulsions are widely used as topical formulations in the pharmaceutical and cosmetic industries. They are thermodynamically unstable and require emulsifiers for stabilization. Studies have indicated that emulsifiers could affect topical delivery of actives, and this study was therefore designed to investigate the effects of different polymers, applied as emulsifiers, as well as the effects of pH on the release and topical delivery of the active. O/w emulsions were prepared by the layer-by-layer technique, with whey protein forming the first layer around the oil droplets, while either chitosan or carrageenan was subsequently adsorbed to the protein at the interface. Additionally, the emulsions were prepared at three different pH values to introduce different charges to the polymers. The active ingredient, salicylic acid, was incorporated into the oil phase of the emulsions. Physical characterization of the resulting formulations, i.e., droplet size, zeta potential, stability, and turbidity in the water phase, was performed. Release studies were conducted, after which skin absorption studies were performed on the five most stable emulsions, by using Franz type diffusion cells and utilizing human, abdominal skin membranes. It was found that an increase in emulsion droplet charge could negatively affect the release of salicylic acid from these formulations. Contrary, positively charged emulsion droplets were found to enhance dermal and transdermal delivery of salicylic acid from emulsions. It was hypothesized that electrostatic complex formation between the emulsifier and salicylic acid could affect its release, whereas electrostatic interaction between the emulsion droplets and skin could influence dermal/transdermal delivery of the active.

Galantamine-loaded PLGA nanoparticles, from nano-emulsion templating, as novel advanced drug delivery systems to treat neurodegenerative diseases

NASA Astrophysics Data System (ADS)

Fornaguera, C.; Feiner-Gracia, N.; Calderó, G.; García-Celma, M. J.; Solans, C.

2015-07-01

Polymeric nanoparticles could be promising drug delivery systems to treat neurodegenerative diseases. Among the various methods of nanoparticle preparation, nano-emulsion templating was used in the present study to prepare galantamine-loaded nano-emulsions by a low-energy emulsification method followed by solvent evaporation to obtain galantamine-loaded polymeric nanoparticles. This approach was found to be suitable because biocompatible, biodegradable and safe nanoparticles with appropriate features (hydrodynamic radii around 20 nm, negative surface charge and stability higher than 3 months) for their intravenous administration were obtained. Encapsulation efficiencies higher than 90 wt% were obtained with a sustained drug release profile as compared to that from aqueous and micellar solutions. The enzymatic activity of the drug was maintained at 80% after its encapsulation into nanoparticles that were non-cytotoxic at the required therapeutic concentration. Therefore, novel galantamine-loaded polymeric nanoparticles have been designed for the first time using the nano-emulsification approach and showed the appropriate features to become advanced drug delivery systems to treat neurodegenerative diseases.Polymeric nanoparticles could be promising drug delivery systems to treat neurodegenerative diseases. Among the various methods of nanoparticle preparation, nano-emulsion templating was used in the present study to prepare galantamine-loaded nano-emulsions by a low-energy emulsification method followed by solvent evaporation to obtain galantamine-loaded polymeric nanoparticles. This approach was found to be suitable because biocompatible, biodegradable and safe nanoparticles with appropriate features (hydrodynamic radii around 20 nm, negative surface charge and stability higher than 3 months) for their intravenous administration were obtained. Encapsulation efficiencies higher than 90 wt% were obtained with a sustained drug release profile as compared to that from aqueous and micellar solutions. The enzymatic activity of the drug was maintained at 80% after its encapsulation into nanoparticles that were non-cytotoxic at the required therapeutic concentration. Therefore, novel galantamine-loaded polymeric nanoparticles have been designed for the first time using the nano-emulsification approach and showed the appropriate features to become advanced drug delivery systems to treat neurodegenerative diseases. Electronic supplementary information (ESI) available. See DOI: 10.1039/c5nr03474d

Diffusion coefficients of nitric oxide in water: A molecular dynamics study

NASA Astrophysics Data System (ADS)

Pokharel, Sunil; Pantha, Nurapati; Adhikari, N. P.

2016-09-01

Self-diffusion coefficients along with the mutual diffusion coefficients of nitric oxide (NO) and SPC/E water (H2O) as solute and solvent of the mixture, have been studied within the framework of classical molecular dynamics level of calculations using GROMACS package. The radial distribution function (RDF) of the constituent compounds are calculated to study solute-solute, solute-solvent and solvent-solvent molecular interactions as a function of temperature. A dilute solution of five NO molecules (mole fraction 0.018) and 280 H2O molecules (mole fraction 0.982) has been taken as the sample. The self-diffusion coefficient of the solvent is calculated by using mean square displacement (MSD) where as that for solute (NO) is calculated by using MSD and velocity auto-correlation function (VACF). The results are then compared with the available experimental values. The results from the present work for water come in good agreement, very precise at low temperatures, with the experimental values. The diffusion coefficients of NO, on the other hands, agree well with the available theoretical studies, and also with experiment at low temperatures (up to 310 K). The results at the higher temperatures (up to 333 K), however, deviate significantly with the experimental observations. Also, the mutual diffusion coefficients of NO in water have been calculated by using Darken’s relation. The temperature dependence of the calculated diffusion coefficients follow the Arrhenius behavior.

Suspended polyhydroxyalkanoate microspheres as 3D carriers for mammalian cell growth.

PubMed

Wei, Dai-Xu; Dao, Jin-Wei; Liu, Hua-Wei; Chen, Guo-Qiang

2018-04-13

Different forms of biopolyester PHBVHHx microspheres were prepared so as to compare the mammalian cell behaviors in suspension cultivation system. Based on a microbial terpolyester PHBVHHx consisting of 3-hydroxybutyrate (HB), 3-hydroxyvalerate (HV), and 3-hydroxyhexanoate (HHx), solid microspheres (SMSs), hollow microspheres (HMSs), and porous microspheres (PMS) were successfully prepared by a modified solvent evaporation method involving gas-in-oil-in-water (G1/O/W2) double emulsion, water-in-oil-in-water (W1/O/W2) double emulsion and oil-in-water (O/W) single emulsion, respectively. Generally, PMSs have diameters ranging from 330 to 400 μm with pore sizes of 10 to 60 μm. The pores inside the PMSs were found well interconnected compared with PHBVHHx prepared by the traditional solvent evaporation method, resulting in the highest water uptake ratio. When inoculated with human osteoblast-like cells lasting 6 days, PMS showed much better cell attachment and proliferation compared with other less porous microspheres due to its large inner space as a 3 D carrier. Cell migration towards surface and other interconnected inner pores was clearly observable. Dead or apoptotic cells were found more common among less porous SMSs or HMSs compared with highly porous PMSs. It is therefore concluded that porous PHBVHHx microspheres with larger surface open pores and interconnected inner pores can serve as a carrier or scaffold supporting more and better cell growth for either injectable purposes or simply supporting cell growth.

An algorithm for emulsion stability simulations: account of flocculation, coalescence, surfactant adsorption and the process of Ostwald ripening.

PubMed

Urbina-Villalba, German

2009-03-01

The first algorithm for Emulsion Stability Simulations (ESS) was presented at the V Conferencia Iberoamericana sobre Equilibrio de Fases y Diseño de Procesos [Luis, J.; García-Sucre, M.; Urbina-Villalba, G. Brownian Dynamics Simulation of Emulsion Stability In: Equifase 99. Libro de Actas, 1(st) Ed., Tojo J., Arce, A., Eds.; Solucion's: Vigo, Spain, 1999; Volume 2, pp. 364-369]. The former version of the program consisted on a minor modification of the Brownian Dynamics algorithm to account for the coalescence of drops. The present version of the program contains elaborate routines for time-dependent surfactant adsorption, average diffusion constants, and Ostwald ripening.

Protein instability toward organic solvent/water emulsification: implications for protein microencapsulation into microspheres.

PubMed

Sah, H

1999-01-01

The objective of this study was to investigate the behavior of three proteins at an organic solvent/water interface. To simulate the first microencapsulation step of a water-in-oil-in-water emulsion technique, a water-in-oil emulsion was prepared by emulsifying an aqueous protein solution in either methylene chloride or ethyl acetate. Phase separation was then followed to collect protein samples from the aqueous phase and the organic solvent/water interface. Their properties were assessed by sodium dodecyl sulfate-polyacrylamide gel electrophoresis and size exclusion-HPLC. Bovine serum albumin was relatively unharmed during emulsification, compared to other proteins such as ovalbumin and lysozyme. In particular, the methylene chloride treatment on ovalbumin led to the formation of a large quantity of water-insoluble, solid-like aggregates and changes in the composition of monomeric and dimeric ovalbumin species. With regard to the question of ovalbumin recovery, only 9.74 approximately 37.72% of the used ovalbumin was present in the aqueous phases after emulsification. Similar penchant was noted with lysozyme. Water-insoluble aggregates brought with by emulsification were found to be covalently bound. Interestingly, less emulsification-induced denaturing effects were observed with ethyl acetate. Our study clearly demonstrated the emulsification-induced adverse events that were detrimental to the integrity of proteins and the importance of preserving protein stability toward microencapsulation.

Evaluation of percutaneous permeation of repellent DEET and sunscreen oxybenzone from emulsion-based formulations in artificial membrane and human skin.

PubMed

Wang, Tao; Miller, Donald; Burczynski, Frank; Gu, Xiaochen

2014-02-01

Insect repellent DEET and sunscreen ingredient oxybenzone play an essential role in minimizing vector-borne diseases and skin cancers. The purpose of this study was to investigate the effects of emulsion type, addition of thickening agent and droplet size in three emulsion-based lotions on percutaneous permeation of DEET and oxybenzone using in vitro diffusion experiments, in order to minimize overall systemic permeation of the substances. Formulation C (water-in-oil emulsion) significantly increased overall permeation of DEET through human skin (56%) compared to Formulation A (oil-in-water emulsion). Formulation B (oil-in-water emulsion with thickening agent xanthan gum) significantly decreased the size of oil droplet containing DEET (16%), but no effect on oil droplets containing oxybenzone. Adding xanthan gum also increased overall permeation of DEET and oxybenzone (21% and 150%) when compared to Formulation A; presence of both ingredients in Formulation B further increased their permeation (36% and 23%) in comparison to its single counterparts. Overall permeation of oxybenzone through LDPE was significantly higher by 26%-628% than that through human skin; overall permeation of DEET through human skin was significantly higher by 64%-338% than that through LDPE.

Gelatin-hydroxypropyl methylcellulose water-in-water emulsions as a new bio-based packaging material.

PubMed

Esteghlal, Sara; Niakosari, Mehrdad; Hosseini, Seyed Mohammad Hashem; Mesbahi, Gholam Reza; Yousefi, Gholam Hossein

2016-05-01

Gelatin and hydroxypropyl methylcellulose (HPMC) are two incompatible and immiscible biopolymers which cannot form homogeneous composite films using usual methods. In this study, to prevent phase separation, gelatin-HPMC water-in-water (W/W) emulsion was utilized to from transparent composite films by entrapment the HPMC dispersed droplets in gelatin continuous network. The physicochemical and mechanical properties of emulsion-based films containing different amounts (5-30%) of dispersed phase were determined and compared with those of individual polymer-based films. Incorporating HPMC into W/W emulsion-based films had no significant effect on the tensile strength. The flexibility of composite films decreased at HPMC concentrations below 20%. The depletion layer at the droplets interface reduced the diffusion of water vapor molecules because of its hydrophobic nature, so the water vapor permeability remained constant. Increasing the HPMC content in the emulsion films increased the swelling and decreased the transparency. The entrapment of HPMC in continuous gelatin phase decreased its solubility. Therefore, W/W emulsions are capable of holding two incompatible polymers alongside each other within a homogeneous film network without weakening the physical properties. Copyright © 2016 Elsevier B.V. All rights reserved.

Antimicrobial property and microstructure of micro-emulsion edible composite films against Listeria.

PubMed

Guo, Mingming; Jin, Tony Z; Yadav, Madhav P; Yang, Ruijin

2015-09-02

Edible antimicrobial composite films from micro-emulsions containing all natural compounds were developed and their antimicrobial properties and microstructures were investigated. Chitosan, allyl isothiocyanate (AIT), barley straw arabinoxylan (BSAX), and organic acids (acetic, lactic and levulinic acids) were used as film-forming agent, antimicrobial agent, emulsifier, and solvent, respectively. Micro-emulsions were obtained using high pressure homogenization (HPH) processing at 138MPa for 3cycles. The composite films made from the micro-emulsions significantly (p<0.05) inactivated Listeria innocua in tryptic soy broth (TSB) and on the surface of ready-to-eat (RTE) meat samples, achieving microbial reductions of over 4logCFU/ml in TSB after 2days at 22°C and on meat samples after 35days at 10°C. AIT was a major contributor to the antimicrobial property of the films and HPH processing further enhanced its antimicrobial efficacy, while the increase of chitosan from 1.5% to 3%, or addition of acetic acid to the formulations didn't result in additional antimicrobial effects. This study demonstrated an effective approach to developing new edible antimicrobial films and coatings used for food applications. Published by Elsevier B.V.

Microsponges based novel drug delivery system for augmented arthritis therapy

PubMed Central

Osmani, Riyaz Ali M.; Aloorkar, Nagesh H.; Ingale, Dipti J.; Kulkarni, Parthasarathi K.; Hani, Umme; Bhosale, Rohit R.; Jayachandra Dev, Dandasi

2015-01-01

The motive behind present work was to formulate and evaluate gel containing microsponges of diclofenac diethylamine to provide prolonged release for proficient arthritis therapy. Quasi-emulsion solvent diffusion method was implied using Eudragit RS-100 and microsponges with varied drug–polymer ratios were prepared. For the sake of optimization, diverse factors affecting microparticles physical properties were too investigated. Microsponges were characterized by SEM, DSC, FT-IR, XRPD and particle size analysis, and evaluated for morphology, drug loading, in vitro drug release and ex vivo diffusion as well. There were no chemical interactions between drug and polymers used as revealed by compatibility studies outcomes. The drug polymer ratio reflected notable effect on drug content, encapsulation efficiency and particle size. SEM results revealed spherical microsponges with porous surface, and had 7.21 μm mean particle size. The microsponges were then incorporated in gel; which exhibited viscous modulus along with pseudoplastic behavior. In vitro drug release results depicted that microsponges with 1:2 drug–polymer ratio were more efficient to give extended drug release of 75.88% at the end of 8 h; while conventional formulation get exhausted incredibly earlier by releasing 81.11% drug at the end of 4 h only. Thus the formulated microsponge-based gel of diclofenac diethylamine would be a promising alternative to conventional therapy for safer and efficient treatment of arthritis and musculoskeletal disorders. PMID:26594124

Microsponges based novel drug delivery system for augmented arthritis therapy.

PubMed

Osmani, Riyaz Ali M; Aloorkar, Nagesh H; Ingale, Dipti J; Kulkarni, Parthasarathi K; Hani, Umme; Bhosale, Rohit R; Jayachandra Dev, Dandasi

2015-10-01

The motive behind present work was to formulate and evaluate gel containing microsponges of diclofenac diethylamine to provide prolonged release for proficient arthritis therapy. Quasi-emulsion solvent diffusion method was implied using Eudragit RS-100 and microsponges with varied drug-polymer ratios were prepared. For the sake of optimization, diverse factors affecting microparticles physical properties were too investigated. Microsponges were characterized by SEM, DSC, FT-IR, XRPD and particle size analysis, and evaluated for morphology, drug loading, in vitro drug release and ex vivo diffusion as well. There were no chemical interactions between drug and polymers used as revealed by compatibility studies outcomes. The drug polymer ratio reflected notable effect on drug content, encapsulation efficiency and particle size. SEM results revealed spherical microsponges with porous surface, and had 7.21 μm mean particle size. The microsponges were then incorporated in gel; which exhibited viscous modulus along with pseudoplastic behavior. In vitro drug release results depicted that microsponges with 1:2 drug-polymer ratio were more efficient to give extended drug release of 75.88% at the end of 8 h; while conventional formulation get exhausted incredibly earlier by releasing 81.11% drug at the end of 4 h only. Thus the formulated microsponge-based gel of diclofenac diethylamine would be a promising alternative to conventional therapy for safer and efficient treatment of arthritis and musculoskeletal disorders.

Double emulsions for the compatibilization of hydrophilic nanocellulose with non-polar polymers and validation in the synthesis of composite fibers.

PubMed

Carrillo, Carlos A; Nypelö, Tiina; Rojas, Orlando J

2016-03-14

A route for the compatibilization of aqueous dispersions of cellulose nanofibrils (CNFs) with a non-polar polymer matrix is proposed to overcome a major challenge in CNF-based material synthesis. Non-ionic surfactants were used in CNF aqueous dispersions equilibrated with an organic phase (for demonstration, a polystyrene solution, PS, was used). Stable water-in-oil-in-water (W/O/W) double emulsions were produced as a result of the compromise between composition and formulation variables. Most remarkably, the proposed route for CNF integration with hydrophobic polymers removed the need for drying or solvent-exchange of the CNF aqueous dispersion prior to processing. The rheological behavior of the double emulsions showed strong shear thinning behavior and facilitated CNF-PS co-mixing in solid nanofibers upon electrospinning. The morphology and thermal properties of the resultant nanofibers revealed that CNFs were efficiently integrated in the hydrophobic matrix which was consistent with the high interfacial area of the precursor double emulsion. In addition, the morphology and quality of the composite nanofibers can be controlled by the conductivity (ionic strength) of the CNF dispersion. Overall, double emulsion systems are proposed as a novel, efficient and scalable platform for CNF co-processing with non-polar systems and they open up the possibility for the redispersion of CNFs after removal of the organic phase.

Mesoscale Polymer Dissolution Probed by Raman Spectroscopy and Molecular Simulations

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

Chang, Tsun-Mei; Xantheas, Sotiris S.; Vasdekis, Andreas E.

2016-10-13

The diffusion of various solvents into a polystyrene (PS) matrix was probed experimentally by monitoring the temporal profiles of the Raman spectra and theoretically from molecular dynamics (MD) simulations of the binary system. The simulation results assist in providing a fundamental, molecular level connection between the mixing/dissolution processes and the difference = solvent – PS in the values of the Hildebrand parameter () between the two components of the binary systems: solvents having similar values of with PS (small ) exhibit fast diffusion into the polymer matrix, whereas the diffusion slows down considerably when the ’s are different (large ).more » To this end, the Hildebrand parameter was identified as a useful descriptor that governs the process of mixing in polymer – solvent binary systems. The experiments also provide insight into further refinements of the models specific to non-Fickian diffusion phenomena that need to be used in the simulations.« less

Release and in vitro skin permeation of polyphenols from cosmetic emulsions.

PubMed

Zillich, O V; Schweiggert-Weisz, U; Hasenkopf, K; Eisner, P; Kerscher, M

2013-10-01

Polyphenols are natural antioxidants, which can inhibit oxidative chain reactions in human skin and prevent therefore some skin diseases and premature ageing. A prerequisite of this behaviour is their permeation through the skin barrier, in particular the stratum corneum (SC). In this study, we investigated the skin permeation kinetic of polyphenols, incorporated to semisolid emulsions, and the release of polyphenols from the emulsions. Mixtures of model substances, consisting of catechin, epigallocatechin gallate (EGCG), resveratrol, quercetin, rutin and protocatechuic acid (PCA), were formulated into o/w emulsions with different oil phase content. The in vitro experiments were carried out in Franz-type diffusion cells by means of ex vivo pig skin and a cellulose membrane. The increased oil content in the emulsion led to a significant decrease in initial release coefficients (K(r)), diffusion coefficients within the formulation (D(v)) and skin permeation coefficients (K(p)), respectively. The study considered the dependence of K(r) on molecular weight and lipophilicity of polyphenolics. For both more hydrophilic and more lipophilic substance groups, the values for K(r) were inverse proportional to molecular weight. For catechin, quercetin, rutin, resveratrol and PCA, a good correlation between K(p) and K(r) parameters was obtained. The most permeable substance was PCA (K(p) = 1.2·10(-3) cm h(-1)), and the least permeable was quercetin (K(p) = 1.5·10(-5) cm h(-1)). All substances could pass the SC barrier and were found mostly in the epidermis and dermis, confirming the potential of polyphenols as anti-ageing active cosmetic ingredients. © 2013 Society of Cosmetic Scientists and the Société Française de Cosmétologie.

Cross-linked gelatin/nanoparticles composite coating on micro-arc oxidation film for corrosion and drug release

NASA Astrophysics Data System (ADS)

Xu, Xinhua; Lu, Ping; Guo, Meiqing; Fang, Mingzhong

2010-02-01

A composite coating which could control drug release and biocorrosion of magnesium alloy stent materials WE42 was prepared. This composite coating was fabricated on the surface of the micro-arc oxidation (MAO) film of the magnesium alloy, WE42, by mixing different degrees of cross-linked gelatin with well-dispersed poly( DL-lactide-co-glycolide) (PLGA) nanoparticles. The PLGA nanoparticles were prepared by emulsion solvent evaporation/extraction technique. Nano ZS laser diffraction particle size analyzer detected that the size of the nanoparticles to be 150-300 nm. Scanning electron microscopy (SEM) and atomic force microscopy (AFM) was used to analyze the morphology of the nanoparticles and the composite coating. Potentiodynamic polarization and electrochemical impedance spectroscopy (EIS) were used to evaluate the corrosion behavior of the composite coating. Drug release was determined by ultraviolet-visible (UV-vis) spectrophotometer. The corrosion resistance of the composite coating was improved by preventing the corrosive ions from diffusing to the MAO films. The drug release rate of paclitaxel (PTX) exhibited a nearly linear sustained-release profile with no significant burst releases.

Influence of hydrophilic surfactants on the properties of multiple W/O/W emulsions.

PubMed

Schmidts, T; Dobler, D; Nissing, C; Runkel, F

2009-10-01

Multiple W/O/W emulsions for topical application using Span 80 as a lipophilic emulsifier were prepared. Several hydrophilic emulsifiers were tested in respect of their suitability for the preparation of multiple emulsions. In addition, the effect of different oil-phase compositions on emulsion stability was investigated. The physicochemical parameters of the formulations were characterized and their long-term stability was evaluated by means of rheological measurements, droplet size observations and conductivity analysis. As discovered, the modification of an oil-phase composition results in a decrease in the diffusion coefficient of water and water-soluble substances and, consequently, in enhanced stability. The influence of the release of electrolytes from the inner to the outer water phase on the emulsion stability behaviour was investigated. It was found, that the effect of the hydrophilic emulsifiers on the formulation properties is related not only to its HLB value, but rather to its chemical composition. As a result, polyethoxylated ethers of fatty alcohols (C=16-18) with HLBs between 15.3 and 16.2 appear to be the most suitable ones for creating stable formulations.

Vapor-phase interactions and diffusion of organic solvents in the unsaturated zone

USGS Publications Warehouse

Roy, W.R.; Griffin, R.A.

1990-01-01

This article presents an analysis of the interactions and static movement of 37 organic solvents as vapors through the unsaturated soil zone. The physicochemical interactions of the organic vapors with unsaturated soil materials were emphasized with focus on diffusive, and adsorptive interactions. Fick's Law and porous media diffusion coefficients for most of the solvent vapors were either compiled or estimated; coefficients were not available for some of the fluorinated solvents. The adsorption of some of the solvent vapors by silica was concluded to be due to hydrogen bond formation with surface silanol groups. Heats of adsorption data for different adsorbents were also compiled. There were very few data on the adsorption of these solvent vapors by soils, but it appears that the magnitude of adsorption of nonpolar solvents is reduced as the relative humidity of the vapor-solid system is increased. Consequently, the interaction of the vapors may then separated into two processes; (1) gas-water partitioning described by Henry's Law constants, and (2) solid-water adsorption coefficients which may be estimated from liquid-solid partition coefficients (Kd values). ?? 1990 Springer-Verlag New York Inc.

Nano-emulsions as vehicles for topical delivery of forskolin.

PubMed

Miastkowska, Małgorzata; Sikora, Elżbieta; Lasoń, Elwira; Garcia-Celma, Maria Jose; Escribano-Ferrer, Elvira; Solans, Conxita; Llinas, Meritxell

2017-01-01

Two O/W forskolin-loaded nano-emulsions (0.075% wt.) based on medium chain triglycerides (MCT) and stabilized by a nonionic surfactant (Polysorbate 80 or Polysorbate 40) were studied as forskolin delivery systems. The nano-emulsions were prepared by the PIC method. The mean droplet size of the nano-emulsions with Polysorbate 80 and Polysorbate 40 with oil/surfactant (O/S) ratios of 20/80 and 80% water concentration, measured by Dynamic Light Scattering (DLS), was of 118 nm and 111 nm, respectively. Stability of the formulations, as assessed by light backscattering for 24 h, showed that both nano-emulsions were stable at 25°C. Studies of forskolin in vitro skin permeation from the nano-emulsions and from a triglyceride solution were carried out at 32°C, using Franz-type diffusion cells. A mixture of PBS/ethanol (60/40 v/v) was used as a receptor solution. The highest flux and permeability coefficient was obtained for the system stabilized with Polysorbate 80 (6.91±0.75 µg · cm -2 ·h -1 and 9.21 · 10 -3 ±1.00 · 10 -3 cm · h -1 , respectively) but no significant differences were observed with the flux and permeability coefficient value of forskolin dissolved in oil. The obtained results showed that the nano-emulsions developed in this study could be used as effective carriers for topical administration of forskolin.

Structure and diffusion of furans and other cellulose-derived compounds in solvents via MD simulation

NASA Astrophysics Data System (ADS)

Rabideau, Brooks; Ismail, Ahmed

2011-03-01

There is now a large push towards the development of energy sources that are both environmentally friendly and sustainable; with the conversion of cellulose derived from biomass into biofuels being one promising route. In this conversion, a variety of intermediary compounds have been identified, which appear critical to successful expansion of the process to an industrial scale. Here we examine the structure and diffusion of these furans and acids derived from cellulose within ionic liquids via molecular dynamic simulation. Ionic liquids have shown the ability to dissolve cellulose with certain `green' benefits over existing, conventional solvents. Specifically, we study the solvation properties of these chemicals by examining the pair correlation functions of solute with solvent, and by exploring the agglomeration and separation of these chemicals from the solvent as well as the hydrogen bonding between species. Additionally, we determine the diffusion constant of these compounds in ionic liquid and aqueous solvents.

Surface area generation and droplet size control in solvent extraction systems utilizing high intensity electric fields

DOEpatents

Scott, Timothy C.; Wham, Robert M.

1988-01-01

A method and system for solvent extraction where droplets are shattered by a high intensity electric field. These shattered droplets form a plurality of smaller droplets which have a greater combined surface area than the original droplet. Dispersion, coalescence and phase separation are accomplished in one vessel through the use of the single pulsing high intensity electric field. Electric field conditions are chosen so that simultaneous dispersion and coalescence are taking place in the emulsion formed in the electric field. The electric field creates a large amount of interfacial surface area for solvent extraction when the droplet is disintegrated and is capable of controlling droplet size and thus droplet stability. These operations take place in the presence of a counter current flow of the continuous phase.

Face-Dependent Solvent Adsorption: A Comparative Study on the Interfaces of HMX Crystal with Three Solvents.

PubMed

Liu, Yingzhe; Lai, Weipeng; Ma, Yiding; Yu, Tao; Kang, Ying; Ge, Zhongxue

2017-07-27

To understand the crystal-solvent interfacial interactions on the molecular scale, the interfaces between three solvents, that is, acetone, γ-butyrolactone, and cyclohexanone, and three growth faces of 1,3,5,7-tetranitro-1,3,5,7-tetrazocane (HMX) crystal have been investigated with the aid of theoretical chemistry. The results show that the structural features of crystal faces play a critical role in the energetic, structural, and dynamic properties at the interfaces. For each solvent, the same change trend of some properties among the three faces of HMX crystal is observed, including adsorption affinity, local mass density, and solvent diffusion. For example, the rate of solvent diffusion at the three faces ranks as (011) > (110) > (020) regardless of solvent species. This can be attributed to the similar adsorption sites for solvent incorporation at the same face, which are concentrated at the cavities formed by surficial HMX molecules.

Differential Microscopic Mobility of Components within a Deep Eutectic Solvent

DOE PAGES

Wagle, Durgesh V.; Baker, Gary A.; Mamontov, Eugene

2015-07-13

From macroscopic measurements of deep eutectic solvents such as glyceline (1:2 molar ratio of choline chloride to glycerol), the long-range translational diffusion of the larger cation (choline) is known to be slower compared to that of the smaller hydrogen bond donor (glycerol). However, when the diffusion dynamics are analyzed on the subnanometer length scale, we discover that the displacements associated with the localized diffusive motions are actually larger for choline. This counterintuitive diffusive behavior can be understood as follows. The localized diffusive motions confined in the transient cage of neighbor particles, which precede the cage-breaking long-range diffusion jumps, are moremore » spatially constrained for glycerol than for choline because of the stronger hydrogen bonds the former makes with chloride anions. The implications of differential localized mobility of the constituents should be especially important for applications where deep eutectic solvents are confined on the nanometer length scale and their long-range translational diffusion is strongly inhibited (e.g., within microporous media).« less

Lithium ion solvation and diffusion in bulk organic electrolytes from first-principles and classical reactive molecular dynamics.

PubMed

Ong, Mitchell T; Verners, Osvalds; Draeger, Erik W; van Duin, Adri C T; Lordi, Vincenzo; Pask, John E

2015-01-29

Lithium-ion battery performance is strongly influenced by the ionic conductivity of the electrolyte, which depends on the speed at which Li ions migrate across the cell and relates to their solvation structure. The choice of solvent can greatly impact both the solvation and diffusivity of Li ions. In this work, we used first-principles molecular dynamics to examine the solvation and diffusion of Li ions in the bulk organic solvents ethylene carbonate (EC), ethyl methyl carbonate (EMC), and a mixture of EC and EMC. We found that Li ions are solvated by either carbonyl or ether oxygen atoms of the solvents and sometimes by the PF6(-) anion. Li(+) prefers a tetrahedrally coordinated first solvation shell regardless of which species are involved, with the specific preferred solvation structure dependent on the organic solvent. In addition, we calculated Li diffusion coefficients in each electrolyte, finding slightly larger diffusivities in the linear carbonate EMC compared to the cyclic carbonate EC. The magnitude of the diffusion coefficient correlates with the strength of Li(+) solvation. Corresponding analysis for the PF6(-) anion shows greater diffusivity associated with a weakly bound, poorly defined first solvation shell. These results can be used to aid in the design of new electrolytes to improve Li-ion battery performance.

Evaluation of percutaneous permeation of repellent DEET and sunscreen oxybenzone from emulsion-based formulations in artificial membrane and human skin

PubMed Central

Wang, Tao; Miller, Donald; Burczynski, Frank; Gu, Xiaochen

2014-01-01

Insect repellent DEET and sunscreen ingredient oxybenzone play an essential role in minimizing vector-borne diseases and skin cancers. The purpose of this study was to investigate the effects of emulsion type, addition of thickening agent and droplet size in three emulsion-based lotions on percutaneous permeation of DEET and oxybenzone using in vitro diffusion experiments, in order to minimize overall systemic permeation of the substances. Formulation C (water-in-oil emulsion) significantly increased overall permeation of DEET through human skin (56%) compared to Formulation A (oil-in-water emulsion). Formulation B (oil-in-water emulsion with thickening agent xanthan gum) significantly decreased the size of oil droplet containing DEET (16%), but no effect on oil droplets containing oxybenzone. Adding xanthan gum also increased overall permeation of DEET and oxybenzone (21% and 150%) when compared to Formulation A; presence of both ingredients in Formulation B further increased their permeation (36% and 23%) in comparison to its single counterparts. Overall permeation of oxybenzone through LDPE was significantly higher by 26%–628% than that through human skin; overall permeation of DEET through human skin was significantly higher by 64%–338% than that through LDPE. PMID:26579363

[Effects of sub-micro emulsion composition on cellular disposition of incorporated lipophilic drug].

PubMed

Sun, Xiao-Yi; Xiang, Zhi-Qiang; Wu, Shuo; Lv, Yuan-Yuan; Liang, Wen-Quan

2013-09-01

To investigate the effects of sub-micro emulsion composition on cellular uptake and disposition of incorporated lipophilic drug. Sub-micro emulsions containing 10 % oil, 1.2 % lecithin and 2.25 % glycerol were prepared, and the fluorescent agent coumarin 6 was used as a model drug. The effects of oil types, co-surfactants and cationic lipid on uptake and elimination kinetics of 6-coumarin in HeLa cells were studied. The uptake mechanism of sub-micro emulsions was further investigated. Oil type and Tweens had no influence on the cellular uptake. Modifications of surfactants with Span series increased the cellular influx, among which Span 20 with hydrophilic-lipophilic balance (HLB) value of 8.6 was the best enhancer. The intracellular drug level reached up to (46.09 ± 1.98)ng/μg protein which had significant difference with control group [(38.54 ± 0.34)ng/μg protein]. The positively charged emulsions significantly increased the uptake rate constant and elimination rate constant which were 4 times and 1.5 times of those in anionic groups, respectively. The uptake enhancement was also observed in cationic emulsions, cellular concentrations at plateau were (42.73 ± 0.84)ng/μg protein, which was about 3 times of that in anionic emulsions [(15.71 ± 0.74)ng/μg protein], when extracellular drug concentration kept at 100 ng/ml. Cationic emulsions delivered the payload mainly by direct drug transfer to contacted cells, while the negative ones depended on both drug passive diffusion and clathrin-mediated endocytosis of drug containing oil droplets which accounted for 20% of the intracellular drug. Interfacial characteristic of sub-micro emulsions such as co-surfactants HLB as well as zeta potentials can influence lipophilic drug both in cellular uptake and elimination.

METAL EXTRACTION PROCESS

DOEpatents

Lewis, G.W. Jr.; Rhodes, D.E.

1957-11-01

An improved method for extracting uranium from aqueous solutions by solvent extraction is presented. A difficulty encountered in solvent extraction operations using an organic extractant (e.g., tributyl phosphate dissolved in kerosene or carbon tetrachloride) is that emulsions sometimes form, and phase separation is difficult or impossible. This difficulty is overcome by dissolving the organic extractant in a molten wax which is a solid at operating temperatures. After cooling, the wax which now contains the extractant, is broken into small particles (preferably flakes) and this wax complex'' is used to contact the uranium bearing solutions and extract the metal therefrom. Microcrystalline petroleum wax and certain ethylene polymers have been found suitable for this purpose.

Evaluation of the separation performance of polyvinylpyrrolidone as a virtual stationary phase for chromatographic NMR.

PubMed

Huang, Shaohua; Wu, Rui; Bai, Zhengwu; Yang, Ying; Li, Suying; Dou, Xiaowei

2014-09-01

Polyvinylpyrrolidone (PVP) was used as a virtual stationary phase to separate p-xylene, benzyl alcohol, and p-methylphenol by the chromatographic NMR technique. The effects of concentration and weight-average molecular weight (Mw) of PVP, solvent viscosity, solvent polarity, and sample temperature on the resolution of these components were investigated. It was found that both higher PVP concentration and higher PVP Mw caused the increase of diffusion resolution for the three components. Moreover, the diffusion resolution did not change at viscosity-higher solvents. Moreover, the three components showed different resolution at different solvents. As temperature increased, the diffusion resolution between p-xylene and benzyl alcohol gradually increased, and the one between p-xylene and p-methylphenol slightly increased from 278 to 298 K and then decreased above 298 K. It was also found that the polarity of the analytes played an important role for the separation by affecting the diffusion coefficient. Copyright © 2014 John Wiley & Sons, Ltd.

Diffusion and solubility coefficients determined by permeation and immersion experiments for organic solvents in HDPE geomembrane.

PubMed

Chao, Keh-Ping; Wang, Ping; Wang, Ya-Ting

2007-04-02

The chemical resistance of eight organic solvents in high density polyethylene (HDPE) geomembrane has been investigated using the ASTM F739 permeation method and the immersion test at different temperatures. The diffusion of the experimental organic solvents in HDPE geomembrane was non-Fickian kinetic, and the solubility coefficients can be consistent with the solubility parameter theory. The diffusion coefficients and solubility coefficients determined by the ASTM F739 method were significantly correlated to the immersion tests (p<0.001). The steady state permeation rates also showed a good agreement between ASTM F739 and immersion experiments (r(2)=0.973, p<0.001). Using a one-dimensional diffusion equation based on Fick's second law, the diffusion and solubility coefficients obtained by immersion test resulted in over estimates of the ASTM F739 permeation results. The modeling results indicated that the diffusion and solubility coefficients should be obtained using ASTM F739 method which closely simulates the practical application of HDPE as barriers in the field.

Preparation of uniform-sized PELA microspheres with high encapsulation efficiency of antigen by premix membrane emulsification.

PubMed

Wei, Qiang; Wei, Wei; Tian, Rui; Wang, Lian-Yan; Su, Zhi-Guo; Ma, Guang-Hui

2008-07-15

Relatively uniform-sized poly(lactide-co-ethylene glycol) (PELA) microspheres with high encapsulation efficiency were prepared rapidly by a novel method combining emulsion-solvent extraction and premix membrane emulsification. Briefly, preparation of coarse double emulsions was followed by additional premix membrane emulsification, and antigen-loaded microspheres were obtained by further solidification. Under the optimum condition, the particle size was about 1 mum and the coefficient of variation (CV) value was 18.9%. Confocal laser scanning microscope and flow cytometer analysis showed that the inner droplets were small and evenly dispersed and the antigen was loaded uniformly in each microsphere when sonication technique was occupied to prepare primary emulsion. Distribution pattern of PEG segment played important role on the properties of microspheres. Compared with triblock copolymer PLA-PEG-PLA, the diblock copolymer PLA-mPEG yielded a more stable interfacial layer at the interface of oil and water phase, and thus was more suitable to stabilize primary emulsion and protect coalescence of inner droplets and external water phase, resulting in high encapsulation efficiency (90.4%). On the other hand, solidification rate determined the time for coalescence during microspheres fabrication, and thus affected encapsulation efficiency. Taken together, improving the polymer properties and solidification rate are considered as two effective strategies to yield high encapsulation.

In-pore exchange and diffusion of carbonate solvent mixtures in nanoporous carbon

DOE PAGES

Alam, Todd M.; Osborn Popp, Thomas M.

2016-06-04

High resolution magic angle spinning (HRMAS) 1H NMR spectroscopy has been used to resolve different surface and in-pore solvent environments of ethylene carbonate (EC) and dimethyl carbonate (DMC) mixtures absorbed within nanoporous carbon (NPC). Two dimensional (2D) 1H HRMAS NMR exchange measurements revealed that the inhomogeneous broadened in-pore resonances have pore-to-pore exchange rates on the millisecond timescale. Pulsed-field gradient (PFG) NMR diffusometry revealed the in-pore self-diffusion constants for both EC and DMC were reduced by up to a factor of five with respect to the diffusion in the non-absorbed solvent mixtures.

Micellar emulsions composed of mPEG-PCL/MCT as novel nanocarriers for systemic delivery of genistein: a comparative study with micelles

PubMed Central

Zhang, Tianpeng; Wang, Huan; Ye, Yanghuan; Zhang, Xingwang; Wu, Baojian

2015-01-01

Polymeric micelles receive considerable attention as drug delivery vehicles, depending on the versatility in drug solubilization and targeting therapy. However, their use invariably suffers with poor stability both in in vitro and in vivo conditions. Here, we aimed to develop a novel nanocarrier (micellar emulsions, MEs) for a systemic delivery of genistein (Gen), a poorly soluble anticancer agent. Gen-loaded MEs (Gen-MEs) were prepared from methoxy poly(ethylene glycol)-block-(ε-caprolactone) and medium-chain triglycerides (MCT) by solvent-diffusion technique. Nanocarriers were characterized by dynamic light scattering, transmission electron microscopy, and in vitro release. The resulting Gen-MEs were approximately 46 nm in particle size with a narrow distribution. Gen-MEs produced a different in vitro release profile from the counterpart of Gen-ME. The incorporation of MCT significantly enhanced the stability of nanoparticles against dilution with simulated body fluid. Pharmacokinetic study revealed that MEs could notably extend the mean retention time of Gen, 1.57- and 7.38-fold as long as that of micelles and solution formulation, respectively, following intravenous injection. Furthermore, MEs markedly increased the elimination half-life (t1/2β) of Gen, which was 2.63-fold larger than that of Gen solution. Interestingly, Gen distribution in the liver and kidney for MEs group was significantly low relative to the micelle group in the first 2 hours, indicating less perfusion in such two tissues, which well accorded with the elongated mean retention time. Our findings suggested that MEs may be promising carriers as an alternative of micelles to systemically deliver poorly soluble drugs. PMID:26491290

Insulin-loaded biodegradable PLGA microcapsules: initial burst release controlled by hydrophilic additives.

PubMed

Yamaguchi, Y; Takenaga, M; Kitagawa, A; Ogawa, Y; Mizushima, Y; Igarashi, R

2002-06-17

We investigated the controlled release of human insulin at an initial stage from poly(DL-lactic-co-glycolic acid) (PLGA, M(w) 6600) spherical matrices. PLGA microcapsules were prepared by the novel solvent evaporation multiple emulsion process. When the crystalline insulin was dispersed in dichloromethane as solid-in-oil (S/O) dispersion, it was found that most of insulin molecules were inlaid on the surface of PLGA microcapsules. Consequently, insulin-loaded PLGA microcapsules exhibited marked rapid release of insulin within several hours in both in vivo and in vitro experiments. On the other hand, the addition of glycerol or water in the primary dichloromethane dispersion results in drastically suppressed initial release. It was found by SEM observation that water- or glycerol-in-oil (W/O or G/O) type mini-emulsion droplets with a mean diameter of 300-500 nm were formed in this primary solution. This phenomenon can be theoretically presumed to occur because insulin and PLGA molecules, having amphiphilic properties, converge on the interface between the hydrophilic additive and dichloromethane. Hence, insulin molecules heterogeneously located in the inside of PLGA microcapsules, not on the surface, would be gradually released with PLGA hydrolytic decomposition. As an additional effect of glycerol, the initial burst was further suppressed due to the decrease of the glass transition temperature of PLGA from 42.5 to 36.7 degrees C. Since the annealing of PLGA molecules took place at around 37 degrees C, the porous structure of microspheres immediately disappeared after immersion in PBS or subcutaneous administration. The insulin diffusion through the water-filled pores would be effectively prevented. The strict controlled initial release of insulin from the PLGA microsphere suggested the possibility of utilization in insulin therapy for type I diabetic patients who need construction of a basal insulin profile.

Lithium Ion Solvation and Diffusion in Bulk Organic Electrolytes from First-Principles and Classical Reactive Molecular Dynamics

DOE PAGES

Ong, Mitchell T.; Verners, Osvalds; Draeger, Erik W.; ...

2014-12-19

We report that lithium-ion battery performance is strongly influenced by the ionic conductivity of the electrolyte, which depends on the speed at which Li ions migrate across the cell and relates to their solvation structure. The choice of solvent can greatly impact both the solvation and diffusivity of Li ions. In this work, we used first-principles molecular dynamics to examine the solvation and diffusion of Li ions in the bulk organic solvents ethylene carbonate (EC), ethyl methyl carbonate (EMC), and a mixture of EC and EMC. We found that Li ions are solvated by either carbonyl or ether oxygen atoms of the solvents and sometimes by the PF more » $$\\bar{6}$$ anion. Li + prefers a tetrahedrally coordinated first solvation shell regardless of which species are involved, with the specific preferred solvation structure dependent on the organic solvent. In addition, we calculated Li diffusion coefficients in each electrolyte, finding slightly larger diffusivities in the linear carbonate EMC compared to the cyclic carbonate EC. The magnitude of the diffusion coefficient correlates with the strength of Li + solvation. Corresponding analysis for the PF $$\\bar{6}$$ anion shows greater diffusivity associated with a weakly bound, poorly defined first solvation shell. In conclusion, these results can be used to aid in the design of new electrolytes to improve Li-ion battery performance.« less

Double emulsions based on silicone-fluorocarbon-water and their skin penetration.

PubMed

Mahrhauser, Denise-Silvia; Fischer, Claudia; Valenta, Claudia

2016-02-10

Double emulsions have significant potential in pharmacy and cosmetics due to the feasibility of combining incompatible substances in one product and the protection of sensitive compounds by incorporating them into their innermost phase. However, a major drawback of double emulsions is their thermodynamic instability and their strong tendency to coalesce. In the present study, the physicochemical stability, the skin permeation and the skin penetration potential of modified semi-solid double emulsions was investigated. The double emulsions were prepared of the cosmetically applied perfluoropolyethers Fomblin HC/04 or Fomblin HC-OH, silicone, carbomer and water. Measurement of the droplet size and examination of the microscopic images confirmed their physicochemical stability over the observation period of eight weeks. Franz-type diffusion cell experiments revealed no increase in curcumin permeation due to the employed perfluoropolyethers compared to the respective control formulations. The formulations used as control were O/W macroemulsions with or without a Polysorbate 80/Sorbitane monooleate 80 surfactant combination. Likewise, tape stripping studies showed no penetration enhancing effect of the employed perfluoropolyethers which is desirable as both perfluoropolyethers are commonly applied components in human personal-care products. Copyright © 2015 Elsevier B.V. All rights reserved.

PLGA nanoparticles from nano-emulsion templating as imaging agents: Versatile technology to obtain nanoparticles loaded with fluorescent dyes.

PubMed

Fornaguera, C; Feiner-Gracia, N; Calderó, G; García-Celma, M J; Solans, C

2016-11-01

The interest in polymeric nanoparticles as imaging systems for biomedical applications has increased notably in the last decades. In this work, PLGA nanoparticles, prepared from nano-emulsion templating, have been used to prepare novel fluorescent imaging agents. Two model fluorescent dyes were chosen and dissolved in the oil phase of the nano-emulsions together with PLGA. Nano-emulsions were prepared by the phase inversion composition (PIC) low-energy method. Fluorescent dye-loaded nanoparticles were obtained by solvent evaporation of nano-emulsion templates. PLGA nanoparticles loaded with the fluorescent dyes showed hydrodynamic radii lower than 40nm; markedly lower than those reported in previous studies. The small nanoparticle size was attributed to the nano-emulsification strategy used. PLGA nanoparticles showed negative surface charge and enough stability to be used for biomedical imaging purposes. Encapsulation efficiencies were higher than 99%, which was also attributed to the nano-emulsification approach as well as to the low solubility of the dyes in the aqueous component. Release kinetics of both fluorescent dyes from the nanoparticle dispersions was pH-independent and sustained. These results indicate that the dyes could remain encapsulated enough time to reach any organ and that the decrease of the pH produced during cell internalization by the endocytic route would not affect their release. Therefore, it can be assumed that these nanoparticles are appropriate as systemic imaging agents. In addition, in vitro toxicity tests showed that nanoparticles are non-cytotoxic. Consequently, it can be concluded that the preparation of PLGA nanoparticles from nano-emulsion templating represents a very versatile technology that enables obtaining biocompatible, biodegradable and safe imaging agents suitable for biomedical purposes. Copyright © 2016 Elsevier B.V. All rights reserved.

α-Tocopherol/chitosan-based nanoparticles: characterization and preliminary investigations for emulsion systems application

NASA Astrophysics Data System (ADS)

Aresta, Antonella; Calvano, Cosima Damiana; Trapani, Adriana; Zambonin, Carlo Giorgio; De Giglio, Elvira

2014-02-01

The processes of lipids oxidation represent a great concern for the consumer health because they are one of the major causes of quality deterioration in fat-containing products. One of the most effective methods of delaying lipid oxidation consists in incorporating antioxidants. The present investigation describes the formulation of chitosan and novel glycol chitosan nanoparticles (NPs) loaded with α-Tocopherol (αToc-NPs). The obtained NPs were characterized by various techniques, such as particle size (showing mean diameters in the range 335-503 nm) and zeta potential measurements, X-ray photoelectron spectroscopy and Fourier transform infrared spectroscopy. The NPs were, then, added in the preparation of oil-in-water simple emulsion both to make the lipophilic αToc available in an aqueous medium and to prevent emulsion oxidation. For this purpose, a new highly sensitive, simple and solvent-free method based on a solid phase microextraction (SPME) coupled to gas chromatography mass spectrometry was developed for the determination of αToc in aqueous medium. All the parameters influencing SPME, including fiber coating, time and temperature extraction, pH, ionic strength and desorption conditions, have been carefully screened. The method was successfully applied to the determination of vitamin in the αToc-NPs and its release from NPs-enriched simple emulsion formulations. SPME provided high recovery yields and the limits of detection and of quantification in emulsion were 0.1 and 0.5 μg/mg, respectively. The precision of the method has been also estimated. The delay of the lipid oxidation by the proposed formulations has been evaluated exploiting the Kreis test on αToc-NPs-enriched emulsions.

Influence of ionic complexation on release rate profiles from multiple water-in-oil-in-water (W/O/W) emulsions.

PubMed

Bonnet, Marie; Cansell, Maud; Placin, Frédéric; David-Briand, Elisabeth; Anton, Marc; Leal-Calderon, Fernando

2010-07-14

Water-in-oil-in-water (W/O/W) double emulsions were prepared, and the kinetics of release of magnesium ions from the internal to the external water phase was followed. Different chelating agents (phosvitin and gluconate) were used to bind magnesium within the prospect of improving the ion retention in the internal aqueous droplets. Magnesium release was monitored for 1 month of storage, for each formulation, with and without chelation, at two storage temperatures (4 and 25 degrees C). Leakage occurred without film rupturing (coalescence) and was mainly due to entropically driven diffusion/permeation phenomena. The experimental results revealed a clear correlation between the effectiveness of chelating agents to delay the delivery and their binding capacity characterized by the equilibrium affinity constant. The kinetic data (percent released versus time curves) were interpreted within the framework of a kinetic model based on diffusion and taking into account magnesium chelation.

Oral and topical sodium cromoglicate in the treatment of diffuse cutaneous mastocytosis in an infant

PubMed Central

Edwards, Alan Martin; Čapková, Štěpánka

2011-01-01

Diffuse cutaneous mastocytosis (DCM) is a rare, severe, variant of cutaneous mastocytosis. The authors report the case of a male infant who developed maculae and maculopapulae on his legs and abdomen when aged 3.5 months, which spread to all body surfaces within weeks. Diagnosis of DCM was made at the age of 6 months when he had developed extensive bullous eruptions, generalised pruritus, flushing and abdominal pain. Treatment was started with oral dimethindine maleate. At the age of 18 months, oral sodium cromoglicate (SCG) was introduced. At the age of 23 months, additional treatment was started with a cutaneous emulsion containing 4% SCG. Continued treatment with oral dimethindine maleate, oral SCG with the dose maintained at 25 mg/kg/day, and SCG 4% cutaneous emulsion applied two to four times daily has resulted in a steady improvement of symptoms and skin appearance. PMID:22693187

Multicomponent membranes

DOEpatents

Kulprathipanja, Santi; Kulkarni, Sudhir S.; Funk, Edward W.

1988-01-01

A multicomponent membrane which may be used for separating various components which are present in a fluid feed mixture comprises a mixture of a plasticizer such as a glycol and an organic polymer cast upon a porous organic polymer support. The membrane may be prepared by casting an emulsion or a solution of the plasticizer and polymer on the porous support, evaporating the solvent and recovering the membrane after curing.

Fabrication of an open Au/nanoporous film by water-in-oil emulsion-induced block copolymer micelles.

PubMed

Koh, Haeng-Deog; Kang, Nam-Goo; Lee, Jae-Suk

2007-12-18

Water-in-oil (W/O) emulsion-induced micelles with narrow size distributions of approximately 140 nm were prepared by sonicating the polystyrene-b-poly(2-vinylpyridine) (PS-b-P2VP) block copolymer in the toluene/water (50:1 vol %). The ordered nanoporous block copolymer films with the hydrophilic P2VP interior and the PS matrix were distinctly fabricated by casting the resultant solution on substrates, followed by evaporating the organic solvent and water. The porous diameter was estimated to be about 70 nm. Here, we successfully prepared the open nanoporous nanocomposites, the P2VP domain decorated by Au (5+/-0.4 nm) nanoparticles based on the methodology mentioned. We anticipate that this novelty enhances the specific function of nanoporous films.

Performance and Selectivity of Ceramic Membranes in the Ultrafiltration of Model Emulsion in Saline

NASA Astrophysics Data System (ADS)

Ćwirko, Konrad; Kalbarczyk-Jedynak, Agnieszka

2017-06-01

Oily wastewaters from different onshore and offshore installations and from maritime transport pose a serious threat to the environment so they must be treated by multistage separation also including membrane processes. The main advantages of such membranes are high performance and selectivity, high resistance for temperature and pressure, resistance for acids, bases and solvents, long service life and for application - significant reduction of industries and transport environmental impact. This work presents the results of the process of separation of oil from the emulsion with NaCl addition. Research was performed with a use of laboratory installation with ceramic 300 kDa membrane. The analysis concerned performance and selectivity of a membrane in the function of time and test results have been subsequently compared with the requirements of the IMO.

Capreomycin oleate microparticles for intramuscular administration: Preparation, in vitro release and preliminary in vivo evaluation.

PubMed

Cambronero-Rojas, Adrián; Torres-Vergara, Pablo; Godoy, Ricardo; von Plessing, Carlos; Sepúlveda, Jacqueline; Gómez-Gaete, Carolina

2015-07-10

Capreomycin sulfate (CS) is a second-line drug used for the treatment of multidrug-resistant tuberculosis (MDR-TB). The adverse effects profile and uncomfortable administration scheme of CS has led to the development of formulations based on liposomes and polymeric microparticles. However, as CS is a water-soluble peptide that does not encapsulate properly into hydrophobic particulate matrices, it was necessary to reduce its aqueous solubility by forming the pharmacologically active capreomycin oleate (CO) ion pair. The aim of this research was to develop a new formulation of CO for intramuscular injection, based on biodegradable microparticles that encapsulate CO in order to provide a controlled release of the drug with reduced local and systemic adverse effects. The CO-loaded microparticles prepared by spray drying or solvent emulsion-evaporation were characterized in their morphology, encapsulation efficiency, in vitro/in vivo kinetics and tissue tolerance. Through scanning electron microscopy it was confirmed that the microparticles were monodisperse and spherical, with an optimal size for intramuscular administration. The interaction between CO and the components of the microparticle matrix was confirmed on both formulations by X-ray powder diffraction and differential scanning calorimetry analyses. The encapsulation efficiencies for the spray-dried and emulsion-evaporation microparticles were 92% and 56%, respectively. The in vitro kinetics performed on both formulations demonstrated a controlled and continuous release of CO from the microparticles, which was successfully reproduced on an in vivo rodent model. The results of the histological analysis demonstrated that none of the formulations produced significant tissue damage on the site of injection. Therefore, the results suggest that injectable CO microparticles obtained by spray drying and solvent emulsion-evaporation could represent an interesting therapeutic alternative for the treatment of MDR-TB. Copyright © 2015 Elsevier B.V. All rights reserved.

Complementary methods for the determination of dissolved oxygen content in perfluorocarbon emulsions and other solutions.

PubMed

Fraker, Christopher A; Mendez, Armando J; Stabler, Cherie L

2011-09-08

Perfluorocarbons (PFCs) are compounds with increased oxygen solubility and effective diffusivity, making them ideal candidates for improving oxygen mass transfer in numerous biological applications. Historically, quantification of the mass transfer characteristics of these liquids has relied on the use of elaborate laboratory equipment and complicated methodologies, such as in-line gas chromatography coupled with temperature-controlled glass fritted diffusion cells. In this work, we present an alternative method for the determination of dissolved oxygen content in PFC emulsions and, by extrapolation, pure PFCs. We implemented a simple stirred oxygen consumption microchamber coupled with an enzymatic reaction for the quantitative determination of oxygen by optical density measurements. Chambers were also custom fitted with lifetime oxygen sensors to permit simultaneous measurement of internal chamber oxygen levels. Analyzing the consumption of oxygen during the enzymatic reaction via recorded oxygen depletion traces, we found a strong degree of correlation between the zero-order reaction rate and the total measured oxygen concentrations, relative to control solutions. The values obtained were in close agreement with published values in the literature, establishing the accuracy of this method. Overall, this method allows for easy, reliable, and reproducible measurements of oxygen content in aqueous solutions, including, but not limited to PFC emulsions.

Fractionation of Poly(butyl methacrylate) by Molecular Topology Using Multidetector Thermal Field-Flow Fractionation.

PubMed

Greyling, Guilaume; Pasch, Harald

2015-12-01

Thermal field-flow fractionation (ThFFF) is an interesting alternative to column-based fractionation being able to address different molecular parameters including size and composition. Until today it has not been shown to be able to fractionate polymers of similar molar masses and chemical compositions by molecular topology. The present study demonstrates that poly(butyl methacrylates) with identical molar masses can be fractionated by ThFFF according to the topology of the butyl group. The influence of the solvent polarity on the thermal diffusion behavior of these polymers is presented and it is shown to have a significant influence on the fractionation of poly(n-butyl methacrylate) and poly(t-butyl methacrylate). Fractionation improves with increasing solvent polarity and solvent polarity may have a greater influence on fractionation than solvent viscosity. It is found that the thermal diffusion coefficient, D(T), as well as the hydrodynamic diameter, D(h), exhibit increasing trends with increasing solvent polarity. The solvent quality has a significant influence on the fractionation. It is found that cyclohexane, being a theta solvent for poly(t-butyl methacrylate) but not for poly(n-butyl methacrylate), significantly improves the fractionation of the samples by decreasing the diffusion rate of the former but not the latter. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Application of mass spectrometer-inverse gas chromatography to study polymer-solvent diffusivity and solubility.

PubMed

Galdámez, J Román; Danner, Ronald P; Duda, J Larry

2007-07-20

The application of a mass spectrometer detector in capillary column inverse gas chromatography is shown to be a valuable tool in the measurement of diffusion and solubility in polymer-solvent systems. The component specific detector provides excellent results for binary polymer-solvent systems, but it is particularly valuable because it can be readily applied to multicomponent systems. Results for a number of infinitely dilute solvents in poly(vinyl acetate) (PVAc) are reported over a range of temperature from 60 to 150 degrees C. Results are also reported for finite concentrations of toluene and methanol in PVAc from 60 to 110 degrees C. Finally, the technique was applied to study the effect of finite concentrations of toluene on the diffusion coefficients of THF and cyclohexane in PVAc. The experimental data compare well with literature values for both infinite and finite concentrations, indicating that the experimental protocol described in this work is sound.

Experimental and Modeling Study of Solvent Diffusion in PDMS for Nanoparticle-Polymer Cosuspension Imprint Lithography.

PubMed

Gervasio, Michelle; Lu, Kathy; Davis, Richey

2015-09-15

This study is the first that focuses on solvent migration in a polydimethylsiloxane (PDMS) stamp during the imprint lithography of ZnO-poly(methyl methacrylate) (PMMA) hybrid suspensions. Using suspensions with varying solids loading levels and ZnO/PMMA ratios, the uptake of the anisole solvent in the stamp is evaluated as a function of time. Laser confocal microscopy is employed as a unique technique to measure the penetration depth of the solvent into the stamp. The suspension solids loading affects the anisole saturation depth in the PDMS stamp. For the suspensions with low solids loading, the experimental data agree with the model for non-Fickian diffusion through a rubbery-elastic polymer. For the suspensions with high solids loading, the data agree more with a sigmoidal diffusion curve, reflecting the rubbery-viscous behavior of a swelling polymer. This difference is due to the degree of swelling in the PDMS. Higher solids loadings induce more swelling because the rate of anisole diffusing into the stamp is increased, likely due to the less dense buildup of the solids as the suspension dries.

Firing of pulverized solvent refined coal

DOEpatents

Lennon, Dennis R.; Snedden, Richard B.; Foster, Edward P.; Bellas, George T.

1990-05-15

A burner for the firing of pulverized solvent refined coal is constructed and operated such that the solvent refined coal can be fired successfully without any performance limitations and without the coking of the solvent refined coal on the burner components. The burner is provided with a tangential inlet of primary air and pulverized fuel, a vaned diffusion swirler for the mixture of primary air and fuel, a center water-cooled conical diffuser shielding the incoming fuel from the heat radiation from the flame and deflecting the primary air and fuel steam into the secondary air, and a watercooled annulus located between the primary air and secondary air flows.

Optimization of two different dispersive liquid-liquid microextraction methods followed by gas chromatography-mass spectrometry determination for polycyclic aromatic hydrocarbons (PAHs) analysis in water.

PubMed

Tseng, Wan-Chi; Chen, Pai-Shan; Huang, Shang-Da

2014-03-01

Novel sample preparation methods termed "up-and-down shaker-assisted dispersive liquid-liquid microextraction (UDSA-DLLME)" and "water with low concentration of surfactant in dispersed solvent-assisted emulsion dispersive liquid-liquid microextraction (WLSEME)" coupled with gas chromatography-mass spectrometry (GC-MS) have been developed for the analysis of 11 polycyclic aromatic hydrocarbons (PAHs) in aqueous samples. For UDSA-DLLME, an up-and-down shaker-assisted emulsification was employed. Extraction was complete in 3min. Only 14 μL of 1-heptanol was required, without a dispersive solvent. Under the optimum conditions, the linear range was 0.08-100 µg L(-1), and the LODs were in the range 0.022-0.060 µg L(-1). The enrichment factors (EFs) ranged from 392 to 766. Relative recoveries were between 84% and 113% for river, lake, and field water. In WLSEME, 9 μL of 1-nonanol as extraction solvent and 240 μL of 1 mg L(-1) Triton X-100 as surfactant were mixed in a microsyringe to form a cloudy emulsified solution, which was then injected into the samples. Compared with other surfactant-assisted emulsion methods, WLSEME uses much less surfactant. The linear range was 0.08-100 µg L(-1), and the LODs were 0.022-0.13 µg L(-1). The EFs ranged from 388 to 649. The relative recoveries were 86-114% for all three water specimens. Copyright © 2013 Elsevier B.V. All rights reserved.

Comparative evaluation of antibacterial activity of caffeic acid phenethyl ester and PLGA nanoparticle formulation by different methods

NASA Astrophysics Data System (ADS)

Arasoglu, Tülin; Derman, Serap; Mansuroglu, Banu

2016-01-01

The aim of the present study was to evaluate the antimicrobial activity of nanoparticle and free formulations of the CAPE compound using different methods and comparing the results in the literature for the first time. In parallel with this purpose, encapsulation of CAPE with the PLGA nanoparticle system (CAPE-PLGA-NPs) and characterization of nanoparticles were carried out. Afterwards, antimicrobial activity of free CAPE and CAPE-PLGA-NPs was determined using agar well diffusion, disk diffusion, broth microdilution and reduction percentage methods. P. aeroginosa, E. coli, S. aureus and methicillin-resistant S. aureus (MRSA) were chosen as model bacteria since they have different cell wall structures. CAPE-PLGA-NPs within the range of 214.0 ± 8.80 nm particle size and with an encapsulation efficiency of 91.59 ± 4.97% were prepared using the oil-in-water (o-w) single-emulsion solvent evaporation method. The microbiological results indicated that free CAPE did not have any antimicrobial activity in any of the applied methods whereas CAPE-PLGA-NPs had significant antimicrobial activity in both broth dilution and reduction percentage methods. CAPE-PLGA-NPs showed moderate antimicrobial activity against S. aureus and MRSA strains particularly in hourly measurements at 30.63 and 61.25 μg ml-1 concentrations (both p < 0.05), whereas they failed to show antimicrobial activity against Gram-negative bacteria (P. aeroginosa and E. coli, p > 0.05). In the reduction percentage method, in which the highest results of antimicrobial activity were obtained, it was observed that the antimicrobial effect on S. aureus was more long-standing (3 days) and higher in reduction percentage (over 90%). The appearance of antibacterial activity of CAPE-PLGA-NPs may be related to higher penetration into cells due to low solubility of free CAPE in the aqueous medium. Additionally, the biocompatible and biodegradable PLGA nanoparticles could be an alternative to solvents such as ethanol, methanol or DMSO. Consequently, obtained results show that the method of selection is extremely important and will influence the results. Thus, broth microdilution and reduction percentage methods can be recommended as reliable and useful screening methods for determination of antimicrobial activity of PLGA nanoparticle formulations used particularly in drug delivery systems compared to both agar well and disk diffusion methods.

GFP as potential cellular viscosimeter.

PubMed

Visser, Antonie J W G; Westphal, Adrie H; Skakun, Victor V; Borst, Jan Willem

2016-08-18

The molecular dimensions of proteins such as green fluorescent protein (GFP) are large as compared to the ones of solvents like water or glycerol. The microscopic viscosity, which determines the resistance to diffusion of, e.g. GFP, is then the same as that determined from the resistance of the solvent to flow, which is known as macroscopic viscosity. GFP in water/glycerol mixtures senses this macroscopic viscosity, because the translational and rotational diffusion coefficients are proportional to the reciprocal value of the viscosity as predicted by the Stokes-Einstein equations. To test this hypothesis, we have performed time-resolved fluorescence anisotropy (reporting on rotational diffusion) and fluorescence correlation spectroscopy (reporting on translational diffusion) experiments of GFP in water/glycerol mixtures. When the solvent also contains macromolecules of similar or larger dimensions as GFP, the microscopic and macroscopic viscosities can be markedly different and the Stokes-Einstein relations must be adapted. It was established from previous dynamic fluorescence spectroscopy observations of diffusing proteins with dextran polysaccharides as co-solvents (Lavalette et al 2006 Eur. Biophys. J. 35 517-22), that rotation and translation sense a different microscopic viscosity, in which the one arising from rotation is always less than that from translation. A microscopic viscosity parameter is defined that depends on scaling factors between GFP and its immediate environment. The direct consequence is discussed for two reported diffusion coefficients of GFP in living cells.

GFP as potential cellular viscosimeter

NASA Astrophysics Data System (ADS)

Visser, Antonie J. W. G.; Westphal, Adrie H.; Skakun, Victor V.; Borst, Jan Willem

2016-09-01

The molecular dimensions of proteins such as green fluorescent protein (GFP) are large as compared to the ones of solvents like water or glycerol. The microscopic viscosity, which determines the resistance to diffusion of, e.g. GFP, is then the same as that determined from the resistance of the solvent to flow, which is known as macroscopic viscosity. GFP in water/glycerol mixtures senses this macroscopic viscosity, because the translational and rotational diffusion coefficients are proportional to the reciprocal value of the viscosity as predicted by the Stokes-Einstein equations. To test this hypothesis, we have performed time-resolved fluorescence anisotropy (reporting on rotational diffusion) and fluorescence correlation spectroscopy (reporting on translational diffusion) experiments of GFP in water/glycerol mixtures. When the solvent also contains macromolecules of similar or larger dimensions as GFP, the microscopic and macroscopic viscosities can be markedly different and the Stokes-Einstein relations must be adapted. It was established from previous dynamic fluorescence spectroscopy observations of diffusing proteins with dextran polysaccharides as co-solvents (Lavalette et al 2006 Eur. Biophys. J. 35 517-22), that rotation and translation sense a different microscopic viscosity, in which the one arising from rotation is always less than that from translation. A microscopic viscosity parameter is defined that depends on scaling factors between GFP and its immediate environment. The direct consequence is discussed for two reported diffusion coefficients of GFP in living cells.

Process for recovering uranium from waste hydrocarbon oils containing the same. [Uranium contaminated lubricating oils from gaseous diffusion compressors

DOEpatents

Conrad, M.C.; Getz, P.A.; Hickman, J.E.; Payne, L.D.

1982-06-29

The invention is a process for the recovery of uranium from uranium-bearing hydrocarbon oils containing carboxylic acid as a degradation product. In one aspect, the invention comprises providing an emulsion of water and the oil, heating the same to a temperature effecting conversion of the emulsion to an organic phase and to an acidic aqueous phase containing uranium carboxylate, and recovering the uranium from the aqueous phase. The process is effective, simple and comparatively inexpensive. It avoids the use of toxic reagents and the formation of undesirable intermediates.

Emulsion of Chloramphenicol: an Overwhelming Approach for Ocular Delivery.

PubMed

Ashara, Kalpesh C; Shah, Ketan V

2017-03-01

Ophthalmic formulations of chloramphenicol have poor bioavailability of chloramphenicol in the ocular cavity. The present study aimed at exploring the impact of different oil mixtures in the form of emulsion on the permeability of chloramphenicol after ocular application. Selection of oil mixture and ratio of the components was made by an equilibrium solubility method. An emulsifier was chosen according to its emulsification properties. A constrained simplex centroid design was used for the assessment of the emulsion development. Emulsions were evaluated for physicochemical properties; zone of inhibition, in-vitro diffusion and ex-vivo local accumulation of chloramphenicol. Validation of the design using check-point batch and reduced polynomial equations were also developed. Optimization of the emulsion was developed by software Design® expert 6.0.8. Assessment of the osmolarity, ocular irritation, sterility testing and isotonicity of optimized batch were also made. Parker Neem®, olive and peppermint oils were selected as an oil phase in the ratio 63.64:20.2:16.16. PEG-400 was selected as an emulsifier according to a pseudo-ternary phase diagram. Constrained simplex-centroid design was applied in the range of 25-39% water, 55-69% PEG-400, 5-19% optimized oil mixture, and 1% chloramphenicol. Unpaired Student's t-test showed for in-vitro and ex-vivo studies that there was a significant difference between the optimized batch of emulsion and Chloramphenicol eye caps (a commercial product) according to both were equally safe. The optimized batch of an emulsion of chloramphenicol was found to be as safe as and more effective than Chloramphenicol eye caps.

Monitoring equilibrium reaction dynamics of a nearly barrierless molecular rotor using ultrafast vibrational echoes

NASA Astrophysics Data System (ADS)

Nilsen, Ian A.; Osborne, Derek G.; White, Aaron M.; Anna, Jessica M.; Kubarych, Kevin J.

2014-10-01

Using rapidly acquired spectral diffusion, a recently developed variation of heterodyne detected infrared photon echo spectroscopy, we observe ˜3 ps solvent independent spectral diffusion of benzene chromium tricarbonyl (C6H6Cr(CO)3, BCT) in a series of nonpolar linear alkane solvents. The spectral dynamics is attributed to low-barrier internal torsional motion. This tripod complex has two stable minima corresponding to staggered and eclipsed conformations, which differ in energy by roughly half of kBT. The solvent independence is due to the relative size of the rotor compared with the solvent molecules, which create a solvent cage in which torsional motion occurs largely free from solvent damping. Since the one-dimensional transition state is computed to be only 0.03 kBT above the higher energy eclipsed conformation, this model system offers an unusual, nearly barrierless reaction, which nevertheless is characterized by torsional coordinate dependent vibrational frequencies. Hence, by studying the spectral diffusion of the tripod carbonyls, it is possible to gain insight into the fundamental dynamics of internal rotational motion, and we find some evidence for the importance of non-diffusive ballistic motion even in the room-temperature liquid environment. Using several different approaches to describe equilibrium kinetics, as well as the influence of reactive dynamics on spectroscopic observables, we provide evidence that the low-barrier torsional motion of BCT provides an excellent test case for detailed studies of the links between chemical exchange and linear and nonlinear vibrational spectroscopy.

N-Succinyl-chitosan nanoparticles coupled with low-density lipoprotein for targeted osthole-loaded delivery to low-density lipoprotein receptor-rich tumors

PubMed Central

Zhang, Chun-ge; Zhu, Qiao-ling; Zhou, Yi; Liu, Yang; Chen, Wei-liang; Yuan, Zhi-Qiang; Yang, Shu-di; Zhou, Xiao-feng; Zhu, Ai-jun; Zhang, Xue-nong; Jin, Yong

2014-01-01

N-Succinyl-chitosan (NSC) was synthesized and NSC nanoparticles (NPs) with loaded osthole (Ost) (Ost/NSC-NPs) were prepared by emulsion solvent diffusion. Subsequently, low-density lipoprotein (LDL)-mediated NSC-NPs with loaded Ost (Ost/LDL-NSC-NPs) were obtained by coupling LDL with Ost/NSC-NPs through amide linkage. The average particle size of Ost/NSC-NPs was approximately 145 nm, the entrapment efficiency was 78.28%±2.06%, and the drug-loading amount was 18.09%±0.17%. The release of Ost from Ost/NSC-NPs in vitro showed a more evident sustained effect than the native material. The half maximal inhibitory concentration of Ost/LDL-NSC-NPs was only 16.23% that of the free Ost at 24 hours in HepG2 cells. Ost inhibited HepG2 cell proliferation by arresting cells in the synthesis phase of the cell cycle and by triggering apoptosis. Cellular uptake and subcellular localization in vitro and near-infrared fluorescence real-time imaging in vivo showed that Ost/LDL-NSC-NPs had high targeting efficacy. Therefore, LDL-NSC-NPs are a promising system for targeted Ost delivery to liver tumor. PMID:24966673

Methotrexate loaded gellan gum microparticles for drug delivery.

PubMed

Dhanka, Mukesh; Shetty, Chaitra; Srivastava, Rohit

2018-04-15

Recently, polysaccharides based microparticles have been found to offer an attractive potential as a carrier in drug delivery field. In this study, bare gellan gum microparticles (GG MPs) and methotrexate (MTX) loaded gellan gum microparticles (MTX-GG MPs) prepared by using simple water-in-oil (W/O) emulsion solvent diffusion method. The developed microparticles (MPs) were found discretely distributed in a spherical shape. MTX has been encapsulated in microparticles with 84.8 ± 1.68% encapsulation efficiency (%EE) and 6.45 ± 0.07% loading capacity (%LC). The Fourier Transform Infrared Spectroscopy (FTIR) characterization of the MPs clearly indicated the physical encapsulation of MTX into polymeric matrix of MPs. Thermogravimetric analysis (TGA) characterization showed slightly higher thermal stability of MTX-GG MPs in comparison to the GG MPs. In vitro release study of MTX-GG MPs showed 84% drug release within 24 h. The hemolysis study of GG MPs and MTX-GG MPs on human red blood cells (RBCs) showed <1.0% hemolysis. The cell viability studies on L929 showed GG MPs, and MTX-GG MPs are biocompatible. Copyright © 2017 Elsevier B.V. All rights reserved.

Pantoprazole Sodium Loaded Microballoons for the Systemic Approach: In Vitro and In Vivo Evaluation.

PubMed

Gupta, Pravin; Kumar, Manish; Kaushik, Darpan

2017-09-01

Purpose: Various floating and pulsatile drug delivery systems suffer from variations in the gastric transit time affecting the bioavailability of drugs. The objective of the study was to develop Pantoprazole Sodium (PAN) microballoons that may prolong the gastric residence time and could enhance the drug bioavailability. Methods: Microballoons were prepared using Eudragit ® L100 by adopting emulsion solvent diffusion method with non-effervescent approach, in vitro studies were performed and the in vivo evaluation was carried out employing ethanol induced ulceration method. Optimization and validation were carried out through Design Expert ® software. Results: The results demonstrate an increase in percentage yield, buoyancy, encapsulation efficacy and swelling. Particles were in the size range 80-100 µm following zero order release pattern. SEM study revealed their rough surface with spherical shape, internal cavity and porous walls. DSC thermo gram confirms the encapsulation of drug in amorphous form. Significant anti ulcer activity was observed for the prepared microballoons. The calculated ulcer index and protection were 0.20±0.05 and 97.43 % respectively for LRS-O (optimized formulation). Conclusion: This kind of pH dependent drug delivery may provide an efficient dosage regimen with enhanced patient compliance.

Effect of O/W process parameters on Crataegus azarolus L nanocapsule properties.

PubMed

Esmaeili, Akbar; Rahnamoun, Soraya; Sharifnia, Fariba

2013-05-29

Nanocapsules have many applications in the drug, cosmetic, fragrance, and food industries. In this study, Crataegus azarolus L. nanocapsules were prepared by a modified emulsion diffusion technique. In this technique a shell was first made from the polyester triblock copolymer poly(ethylene glycol)-poly(butylene adipate)-poly(ethylene glycol) (PEG-PBA-PEG) and then olive oil was set as the core of the nanocapsule by a method known as the polymer deposition solvent evaporation method. Varying amounts of C. azarolus extract, polymer, and olive oil were mixed in acetone and then added to water on a shaker. Finally, the acetone was removed by vacuuming. The size of the prepared nanocapsules were measured with a particle size analysis report (PSAR) and identified by scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), and nuclear magnetic resonance (NMR). Our experiments showed that the size of the nanocapsules depends on the preparation conditions, i.e., the ratio of polymer to oil and concentrations of polymer and plant extract. A ratio of 1:0.25 polymer to oil was shown to be more suitable for the formation of smaller nanocapsules of C. azarolus.

Effect of O/W process parameters on Crataegus azarolus L nanocapsule properties

PubMed Central

2013-01-01

Background Nanocapsules have many applications in the drug, cosmetic, fragrance, and food industries. In this study, Crataegus azarolus L. nanocapsules were prepared by a modified emulsion diffusion technique. Methods In this technique a shell was first made from the polyester triblock copolymer poly(ethylene glycol)-poly(butylene adipate)-poly(ethylene glycol) (PEG-PBA-PEG) and then olive oil was set as the core of the nanocapsule by a method known as the polymer deposition solvent evaporation method. Varying amounts of C. azarolus extract, polymer, and olive oil were mixed in acetone and then added to water on a shaker. Finally, the acetone was removed by vacuuming. Results The size of the prepared nanocapsules were measured with a particle size analysis report (PSAR) and identified by scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), and nuclear magnetic resonance (NMR). Conclusions Our experiments showed that the size of the nanocapsules depends on the preparation conditions, i.e., the ratio of polymer to oil and concentrations of polymer and plant extract. A ratio of 1:0.25 polymer to oil was shown to be more suitable for the formation of smaller nanocapsules of C. azarolus. PMID:23718829

Boiling of an emulsion in a yield stress fluid.

PubMed

Guéna, Geoffroy; Wang, Ji; d'Espinose, Jean-Baptiste; Lequeux, François; Talini, Laurence

2010-11-01

We report the boiling behavior of pentane emulsified in a yield stress fluid, a colloidal clay (Laponite) suspension. We have observed that a superheated state is easily reached: the emulsion, heated more than 50 °C above the alkane boiling point, does not boil. Superheating is made possible by the suppression of heterogeneous nucleation in pentane, resulting from the emulsification process, a phenomenon evidenced decades ago in studies of the superheating of two phase fluids. We have furthermore studied the growth of isolated bubbles nucleated in the emulsion. The rate of increase of the bubble radius with time depends on both the temperature and emulsion volume fraction but, rather unexpectedly, does not depend on the fluid rheology. We show that the bubbles grow by diffusion of the alkane through the aqueous phase between liquid droplets and bubbles, analogously to an Ostwald ripening process. The peculiarity of the process reported here is that a layer depleted in oil droplets forms around the bubble, layer to which the alkane concentration gradient is confined. We successfully describe our experimental results with a simple transfer model.

Viscoelasticity of Depletion-Induced Emulsion Gels

NASA Astrophysics Data System (ADS)

Meller, Amit; Stavans, Joel; Gisler, Thomas; Weitz, David A.

1997-03-01

The presence of non-adsorbing polymer in an oil-in-water emulsion results in a depletion attraction between the emulsion droplets, causing a phase separation into an droplet-rich phase and a polymer-rich phase largely devoid of emulsion droplets. At high enough droplet concentration, however, this phase separation is kinetically arrested to a gel-like state where large (diameter>50 μm) clusters of droplets are weakly connected via ramifications, leading to a measurable elastic modulus. We measure the mean-square displacement <Δ r ^2 (t)> of a droplet of size a inside a cluster using diffusing wave spectroscopy (DWS); by means of a generalized Stokes-Einstein relation we obtain frequency dependent storage and loss moduli G'(ω) and G''(ω), respectively. G'(ω) reaches a plateau at frequencies between 1 rad/s and 100 rad/s; this plateau modulus is found to scale with the hard-sphere energy density k_BT/a^3; within the clusters the droplets are densely packed, yet remain undeformed, the droplet volume fraction being determined by the osmotic pressure exerted by the polymer.

Microstructural aspects in steel fiber reinforced acrylic emulsion polymer modified concrete

NASA Astrophysics Data System (ADS)

Hazimmah, Dayang; Ayob, Afizah; Sie Yee, Lau; Chee Cung, Wong

2018-03-01

Scanning electron microscope observations of polymer-free and polymer-modified cements have shown that the polymer particles are partitioned between the inside of hydrates and the surface of anhydrous cement grains. For optimum dosage of acrylic emulsion polymer with 2.5%, the C-S-H gel in this structure is finer and more acicular. Some polymer adheres or deposit on the surface of the C-S-H gel. The presence of acrylic emulsion polymer confines the ionic diffusion so that the Ca(OH)2 crystallized locally to form fine crystals. The void in the structures seems to be smaller but no polymer films appears to be bridging the walls of pores although many polymer bonds or C-S-H spread into the pore spaces. In addition to porosity reduction, acrylic emulsion polymer modified the hydration products in the steel fiber -matrix ITZ. The hydration product C-S-H appeared as a needle like shape. The needle-shaped C-S-H increases and gradually formed the gel, with needles growing into the pore space. The phenomenon is more obvious as curing age increased.

Physical and material properties of an emulsion-based lipstick produced via a continuous process.

PubMed

Beri, A; Pichot, R; Norton, I T

2014-04-01

Water-in-oil emulsions in lipsticks could have the potential to improve moisturizing properties and deliver hydrophilic molecules to the lips. The aim of this work was to investigate the effect of a continuous process (scraped surface heat exchanger (SSHE) and pin stirrer (PS)) on the physical and material properties of an emulsion-based lipstick by altering the processing conditions of both the SSHE and PS. Emulsion formation was achieved using a SSHE and PS. Emulsions were analysed using nuclear magnetic resonance restricted diffusion (droplet size), texture analysis and rheology (mechanical properties). Results showed that a higher impeller rotational velocity (IRV) (1500 r.p.m.) and a lower exit temperature (52°C) produce the smallest droplets (~ 4 μm), due to greater disruptive forces and a higher viscosity of the continuous phase. The addition of a PS reduces the droplet size (14-6 μm) if the SSHE has a low IRV (500 r.p.m.), due to greater droplet disruption as the emulsion passes through the PS unit. Results also show that if the jacket temperature of a SSHE is 65°C, so that crystallization occurs in both process and post-production, droplets can be integrated into the network resulting in a stiffer wax network (G' - 0.12, in comparison to 0.02 MPa). This is due to small crystals creating a shell around water droplets which can form connections with the continuous network forming a structured network. The addition of a pin stirrer can disrupt a formed network reducing the stiffness of the emulsion (0.3-0.05 MPa). This work suggests the potential use of a continuous process in producing an emulsion-based lipstick, particularly when wax crystals are produced in the process. Future work should consider the moisturizing or lubricating properties of wax continuous emulsions and the release of hydrophilic compounds from the aqueous phase.

Elementary kinematical model of thermal diffusion in liquids and gases.

PubMed

Brenner, Howard

2006-09-01

An elementary hydrodynamic and Brownian motion model of the thermal diffusivity D(T) of a restricted class of binary liquid mixtures, previously proposed by the author, is given a more transparent derivation than originally, exposing thereby the strictly kinematic-hydrodynamic nature of an important class of thermodiffusion separation phenomena. Moreover, it is argued that the solvent's thermometric diffusivity alpha appearing in that theory as one of the two fundamental parameters governing D(T) should be replaced by the solvent's (isothermal) self-diffusivity D(S). In addition, a corrective multiplier of O(1) is inserted to reflect the general physicochemical noninertness of the solute relative to the solvent, thus enhancing the applicability of the resulting formula D(T)=lambdaD(S)beta to "nonideal" solutions. Here, beta is the solvent's thermal expansivity and lambda is a term of O(1), insensitive to the physicochemical nature of the solute (thus rendering D(T) primarily dependent upon only the properties of the solvent). This formula is, on the basis of its derivation, presumably valid only under certain idealized, albeit well-defined, circumstances. This occurs when the solute molecules are: (i) large compared with those of the solvent; and (ii) present only in small proportions relative to those of the solvent. When the solute is physicochemically inert, it is expected that lambda=1. When these conditions are met, the resulting thermal diffusivity of the mixture is, in theory, independent of any and all properties of the solute. Moreover, because beta is algebraically signed, the thermal diffusivity can either by positive or negative, according as the solvent expands or contracts upon being heated. This formula for D(T) is compared with available experimental data for selected binary liquid mixtures. Reasonable agreement is found in almost all circumstances with lambda near unity, the more so the higher the temperature, especially when the solute-solvent mixture properties closely approximate those where agreement would be expected and conversely. Finally, it is pointed out that for the restricted circumstances described, the formula D(T)=lambdaD(S)beta is equally credible for gases. Here, based on gas-kinetic theory, it is possible to furnish the theoretical value of lambda. Overall, while spanning a range of about five orders of magnitude, the D(T) values given by this elementary formula are shown to apply with reasonable accuracy to: (i) liquids (including circumstances for which D(T) is negative) as well as gases; (ii) all combinations of solvents and solutes tested (the latter including, for example, polymer molecules and metallic colloidal particles); and (iii) all sizes of solute molecules, from angstroms to submicron.

In-syringe demulsified dispersive liquid-liquid microextraction and high performance liquid chromatography-mass spectrometry for the determination of trace fungicides in environmental water samples.

PubMed

Xia, Yating; Cheng, Min; Guo, Feng; Wang, Xiangfang; Cheng, Jing

2012-04-29

An in-syringe demulsified dispersive liquid-liquid microextraction (ISD-DLLME) technique was developed using low-density extraction solvents for the highly sensitive determination of the three trace fungicides (azoxystrobin, diethofencarb and pyrimethanil) in water samples by high performance liquid chromatography-mass spectrometry chromatography-diode array detector/electrospray ionisation mass spectrometry. In the proposed technique, a 5-mL syringe was used as an extraction, separation and preconcentration container. The emulsion was obtained after the mixture of toluene (extraction solvent) and methanol (dispersive solvent) was injected into the aqueous bulk of the syringe. The obtained emulsion cleared into two phases without centrifugation, when an aliquot of methanol was introduced as a demulsifier. The separated floating organic extraction solvent was impelled and collected into a pipette tip fitted to the tip of the syringe. Under the optimal conditions, the enrichment factors for azoxystrobin, diethofencarb and pyrimethanil were 239, 200, 195, respectively. The limits of detection, calculated as three times the signal-to-noise ratio (SN(-1)), were 0.026 μg L(-1) for azoxystrobin, 0.071 μg L(-1) for diethofencarb and 0.040 μg L(-1) for pyrimethanil. The repeatability study was carried out by extracting the spiked water samples at concentration levels of 0.02 μg mL(-1) for all the three fungicides. The relative standard deviations varied between 4.9 and 8.2% (n=5). The recoveries of all the three fungicides from tap, lake and rain water samples at spiking levels of 0.2, 1, 5 μg L(-1) were in the range of 90.0-105.0%, 86.0-114.0% and 88.6-110.0%, respectively. The proposed ISD-DLLME technique was demonstrated to be simple, practical and efficient for the determination of different kinds of fungicide residues in real water samples. Copyright © 2012. Published by Elsevier B.V.

The solvent-gelator interaction as the origin of different diffusivity behavior of diols in gels formed with sugar-based low-molecular-mass gelator.

PubMed

Kowalczuk, Joanna; Bielejewski, Michał; Lapiński, Andrzej; Luboradzki, Roman; Tritt-Goc, Jadwiga

2014-04-10

Organogels are soft materials consisting of low-molecular-mass gelators (LMOGs) self-assembled through noncovalent interactions into 3D structures, in which free spaces are filled by organic solvents. 4,6,4',6'-O-terephthylidene-bis(methyl-α-d-glucopyranoside) (1) is found to be a new LMOG. It gelatinizes only a limited number of solvents. Here, the gels of 1 with ethylene glycol (EG) and 1,3-propanediol (PG) are investigated with FT-IR, Raman, and UV-vis spectroscopies, the NMR relaxometry and diffusometry methods, and microscopic observation. The chemical structures of both solvents are closely related, but the variety of physical characteristics of the gels is large. The 1/PG gels are thermally more stable compared to 1/EG gels. The types of aggregates are most likely the H- and J-type in 1/EG gels and the J-type in 1/PG gels. Different microstructures are observed: bundles of crossing fibers for 1/EG and a honeycomb-like matrix for 1/PG gels. The diffusivity of the EG solvent in gels with 1 behaves as expected, decreasing with increasing gelator concentration, whereas the opposite behavior is observed for the PG solvent. This is a most fascinating result. To explain the diffusion enhancement, we suggest that a dynamic hydrogen bonding network of PG solvent in gel matrixes is disrupted due to solvent-gelator interaction. The direct proof of this interaction is given by the observed low frequency dispersion of the spin-lattice relaxation time of solvents in the gel matrixes.

Characterization and mosquito repellent activity of citronella oil nanoemulsion.

PubMed

Sakulku, Usawadee; Nuchuchua, Onanong; Uawongyart, Napaporn; Puttipipatkhachorn, Satit; Soottitantawat, Apinan; Ruktanonchai, Uracha

2009-05-08

Encapsulated citronella oil nanoemulsion prepared by high pressure homogenization at varying amounts of surfactant and glycerol, was studied in terms of the droplet size, stability, release characteristics and in vivo mosquito protection. Transparent nanoemulsion can be obtained at optimal concentration of 2.5% surfactant and 100% glycerol. Physical appearance and the stability of the emulsion were greatly improved through an addition of glycerol, owing to its co-solvent and highly viscous property. The increasing emulsion droplet increased the oil retention. The release behavior could be attributed to the effect of droplet size and concentrations of surfactant and glycerol. By fitting to Higuchi's equation, an increase in glycerol and surfactant concentrations resulted in slow release of the oil. The release rate related well to the protection time where a decrease in release rate can prolong mosquito protection time.

Liquid crystal Janus emulsion droplets: preparation, tumbling, and swimming.

PubMed

Jeong, Joonwoo; Gross, Adam; Wei, Wei-Shao; Tu, Fuquan; Lee, Daeyeon; Collings, Peter J; Yodh, A G

2015-09-14

This study introduces liquid crystal (LC) Janus droplets. We describe a process for the preparation of these droplets, which consist of nematic LC and polymer compartments. The process employs solvent-induced phase separation in emulsion droplets generated by microfluidics. The droplet morphology was systematically investigated and demonstrated to be sensitive to the surfactant concentration in the background phase, the compartment volume ratio, and the possible coalescence of multiple Janus droplets. Interestingly, the combination of a polymer and an anisotropic LC introduces new functionalities into Janus droplets, and these properties lead to unusual dynamical behaviors. The different densities and solubilities of the two compartments produce gravity-induced alignment, tumbling, and directional self-propelled motion of Janus droplets. LC Janus droplets with remarkable optical properties and dynamical behaviors thus offer new avenues for applications of Janus colloids and active soft matter.

Relating the variation of secondary structure of gelatin at fish oil-water interface to adsorption kinetics, dynamic interfacial tension and emulsion stability.

PubMed

Liu, Huihua; Wang, Bo; Barrow, Colin J; Adhikari, Benu

2014-01-15

The objectives of this study were to quantify the relationship between secondary structure of gelatin and its adsorption at the fish-oil/water interface and to quantify the implication of the adsorption on the dynamic interfacial tension (DST) and emulsion stability. The surface hydrophobicity of the gelatin solutions decreased when the pH increased from 4.0 to 6.0, while opposite tend was observed in the viscosity of the solution. The DST values decreased as the pH increased from 4.0 to 6.0, indicating that higher positive charges (measured trough zeta potential) in the gelatin solution tended to result in higher DST values. The adsorption kinetics of the gelatin solution was examined through the calculated diffusion coefficients (Deff). The addition of acid promoted the random coil and β-turn structures at the expense of α-helical structure. The addition of NaOH decreased the β-turn and increased the α-helix and random coil. The decrease in the random coil and triple helix structures in the gelatin solution resulted into increased Deff values. The highest diffusion coefficients, the highest emulsion stability and the lowest amount of random coil and triple helix structures were observed at pH=4.8. The lowest amount of random coil and triple helix structures in the interfacial protein layer correlated with the highest stability of the emulsion (highest ESI value). The lower amount of random coil and triple helix structures allowed higher coverage of the oil-water interface by relatively highly ordered secondary structure of gelatin. Copyright © 2013 Elsevier Ltd. All rights reserved.

Bioreactor droplets from liposome-stabilized all-aqueous emulsions

NASA Astrophysics Data System (ADS)

Dewey, Daniel C.; Strulson, Christopher A.; Cacace, David N.; Bevilacqua, Philip C.; Keating, Christine D.

2014-08-01

Artificial bioreactors are desirable for in vitro biochemical studies and as protocells. A key challenge is maintaining a favourable internal environment while allowing substrate entry and product departure. We show that semipermeable, size-controlled bioreactors with aqueous, macromolecularly crowded interiors can be assembled by liposome stabilization of an all-aqueous emulsion. Dextran-rich aqueous droplets are dispersed in a continuous polyethylene glycol (PEG)-rich aqueous phase, with coalescence inhibited by adsorbed ~130-nm diameter liposomes. Fluorescence recovery after photobleaching and dynamic light scattering data indicate that the liposomes, which are PEGylated and negatively charged, remain intact at the interface for extended time. Inter-droplet repulsion provides electrostatic stabilization of the emulsion, with droplet coalescence prevented even for submonolayer interfacial coatings. RNA and DNA can enter and exit aqueous droplets by diffusion, with final concentrations dictated by partitioning. The capacity to serve as microscale bioreactors is established by demonstrating a ribozyme cleavage reaction within the liposome-coated droplets.

Bioreactor droplets from liposome-stabilized all-aqueous emulsions.

PubMed

Dewey, Daniel C; Strulson, Christopher A; Cacace, David N; Bevilacqua, Philip C; Keating, Christine D

2014-08-20

Artificial bioreactors are desirable for in vitro biochemical studies and as protocells. A key challenge is maintaining a favourable internal environment while allowing substrate entry and product departure. We show that semipermeable, size-controlled bioreactors with aqueous, macromolecularly crowded interiors can be assembled by liposome stabilization of an all-aqueous emulsion. Dextran-rich aqueous droplets are dispersed in a continuous polyethylene glycol (PEG)-rich aqueous phase, with coalescence inhibited by adsorbed ~130-nm diameter liposomes. Fluorescence recovery after photobleaching and dynamic light scattering data indicate that the liposomes, which are PEGylated and negatively charged, remain intact at the interface for extended time. Inter-droplet repulsion provides electrostatic stabilization of the emulsion, with droplet coalescence prevented even for submonolayer interfacial coatings. RNA and DNA can enter and exit aqueous droplets by diffusion, with final concentrations dictated by partitioning. The capacity to serve as microscale bioreactors is established by demonstrating a ribozyme cleavage reaction within the liposome-coated droplets.

Evaporation of Particle-Stabilized Emulsion Sunscreen Films.

PubMed

Binks, Bernard P; Fletcher, Paul D I; Johnson, Andrew J; Marinopoulos, Ioannis; Crowther, Jonathan M; Thompson, Michael A

2016-08-24

We recently showed (Binks et al., ACS Appl. Mater. Interfaces, 2016, DOI: 10.1021/acsami.6b02696) how evaporation of sunscreen films consisting of solutions of molecular UV filters leads to loss of UV light absorption and derived sun protection factor (SPF). In the present work, we investigate evaporation-induced effects for sunscreen films consisting of particle-stabilized emulsions containing a dissolved UV filter. The emulsions contained either droplets of propylene glycol (PG) in squalane (SQ), droplets of SQ in PG or droplets of decane in PG. In these different emulsion types, the SQ is involatile and shows no evaporation, the PG is volatile and evaporates relatively slowly, whereas the decane is relatively very volatile and evaporates quickly. We have measured the film mass and area, optical micrographs of the film structure, and the UV absorbance spectra during evaporation. For emulsion films containing the involatile SQ, evaporation of the PG causes collapse of the emulsion structure with some loss of specular UV absorbance due to light scattering. However, for these emulsions with droplets much larger than the wavelength of light, the light is scattered only at small forward angles so does not contribute to the diffuse absorbance and the film SPF. The UV filter remains soluble throughout the evaporation and thus the UV absorption by the filter and the SPF remain approximately constant. Both PG-in-SQ and SQ-in-PG films behave similarly and do not show area shrinkage by dewetting. In contrast, the decane-in-PG film shows rapid evaporative loss of the decane, followed by slower loss of the PG resulting in precipitation of the UV filter and film area shrinkage by dewetting which cause the UV absorbance and derived SPF to decrease. Measured UV spectra during evaporation are in reasonable agreement with spectra calculated using models discussed here.

Ionic liquid-based air-assisted liquid-liquid microextraction followed by high performance liquid chromatography for the determination of five fungicides in juice samples.

PubMed

You, Xiangwei; Chen, Xiaochu; Liu, Fengmao; Hou, Fan; Li, Yiqiang

2018-01-15

A novel and simple ionic liquid-based air-assisted liquid-liquid microextraction technique combined with high performance liquid chromatography was developed to analyze five fungicides in juice samples. In this method, ionic liquid was used instead of a volatile organic solvent as the extraction solvent. The emulsion was formed by pulling in and pushing out the mixture of aqueous sample solution and extraction solvent repeatedly using a 10mL glass syringe. No organic dispersive solvent was required. Under the optimized conditions, the limits of detection (LODs) were 0.4-1.8μgL -1 at a signal-to-noise ratio of 3. The limits of quantification (LOQs) set as the lowest spiking levels with acceptable recovery in juices were 10μgL -1 , except for fludioxonil whose LOQ was 20μgL -1 . The proposed method was applied to determine the target fungicides in juice samples, and acceptable recoveries ranging from 74.9% to 115.4% were achieved. Copyright © 2017. Published by Elsevier Ltd.

Effect of spray-drying with organic solvents on the encapsulation, release and stability of fish oil.

PubMed

Encina, Cristian; Márquez-Ruiz, Gloria; Holgado, Francisca; Giménez, Begoña; Vergara, Cristina; Robert, Paz

2018-10-15

Fish-oil (FO) was encapsulated with hydroxypropylcelullose (HPC) by conventional spray-drying with water (FO-water) and solvent spray-drying with ethanol (FO-EtOH), methanol (FO-MeOH) and acetone (FO-Acet) in order to study the effect of the solvent on the encapsulation efficiency (EE), microparticle properties and stability of FO during storage at 40 °C. Results showed that FO-Acet presented the highest EE of FO (92.0%), followed by FO-EtOH (80.4%), FO-MeOH (75.0%) and FO-water (71.1%). A decrease of the dielectric constant increased the EE of FO, promoting triglyceride-polymer interactions instead of oil-in-water emulsion retention. FO release profile in aqueous model was similar for all FO-microparticles, releasing only the surface FO, according to Higuchi model. Oxidative stability of FO significantly improved by spray-drying with MeOH, both in surface and encapsulated oil fractions. In conclusion, encapsulation of FO by solvent spray-drying can be proposed as an alternative technology for encapsulation of hydrophobic molecules. Copyright © 2018 Elsevier Ltd. All rights reserved.

Physico-chemical separation process of nanoparticles in cosmetic formulations

NASA Astrophysics Data System (ADS)

Retamal Marín, R. R.; Babick, F.; Stintz, M.

2017-06-01

Understanding the world of nanoparticles, especially their interactions with the environment, begins with their correct detection and successive quantification. To achieve this purpose, one needs to perform correctly developed standard operating procedures (SOPs). Furthermore, the study of nanoparticles frequently requires their characterisation in complex media (e.g. in cosmetic formulations). In this study, a set of sample preparation procedures for the detection and extraction of NMs in emulsion-based formulations is proposed and their performance for model and real-life products is discussed. A separation or extraction of lipid phases is achieved by means of organic solvents. The polarity of the lipid phases is decisive for selecting an optimum solvent. The use of the Hansen Solubility Parameters (HSP) may clearly support this decision.

In vitro evaluation of suspoemulsions for in situ-forming polymeric microspheres and controlled release of progesterone.

PubMed

Turino, Ludmila N; Mariano, Rodolfo N; Mengatto, Luciano N; Luna, Julio A

2015-01-01

One possibility to obtain a higher dose of drug in a lower formulation volume can be by using of saturated quantity of drug in one of the phases of an emulsion. These formulations are called suspoemulsions (S/O/W). When a hydrophobic polymer is added to the organic phase of suspoemulsions, these formulations can be used to entrap the drug inside microspheres after in situ precipitation of the polymer-drug-excipients mix. In this work, performance and stability of progesterone suspensions in triacetin as organic phase of suspoemulsions were evaluated. These formulations were compared with O/W emulsions. Mathematical models were used to study in vitro release profiles. The results confirmed that S/O/W systems could be an attractive alternative to O/W formulations for the entrapment of progesterone inside poly(d,l-lactide-co-glycolide) microspheres. Diffusive-based models fit the in vitro release of progesterone from in situ-formed microspheres. For longer release periods, a time-dependent diffusion coefficient was successfully estimated.

An elasto-visco-plastic model for immortal foams or emulsions

NASA Astrophysics Data System (ADS)

Bénito, S.; Bruneau, C.-H.; Colin, T.; Gay, C.; Molino, F.

2008-03-01

A variety of complex fluids consists in soft, round objects (foams, emulsions, assemblies of copolymer micelles or of multilamellar vesicles--also known as onions). Their dense packing induces a slight deviation from their prefered circular or spherical shape. As a frustrated assembly of interacting bodies, such a material evolves from one conformation to another through a succession of discrete, topological events driven by finite external forces. As a result, the material exhibits a finite yield threshold. The individual objects usually evolve spontaneously (colloidal diffusion, object coalescence, molecular diffusion), and the material properties under low or vanishing stress may alter with time, a phenomenon known as aging. We neglect such effects to address the simpler behaviour of (uncommon) immortal fluids: we construct a minimal, fully tensorial, rheological model, equivalent to the (scalar) Bingham model. Importantly, the model consistently describes the ability of such soft materials to deform substantially in the elastic regime (be it compressible or not) before they undergo (incompressible) plastic creep--or viscous flow under even higher stresses.

Dynamics of Polydisperse Foam-like Emulsion

NASA Astrophysics Data System (ADS)

Hicock, Harry; Feitosa, Klebert

2011-10-01

Foam is a complex fluid whose relaxation properties are associated with the continuous diffusion of gas from small to large bubbles driven by differences in Laplace pressures. We study the dynamics of bubble rearrangements by tracking droplets of a clear, buoyantly neutral emulsion that coarsens like a foam. The droplets are imaged in three dimensions using confocal microscopy. Analysis of the images allows us to measure their positions and radii, and track their evolution in time. We find that the droplet size distribution fits a Weibull distribution characteristics of foam systems. Additionally, we observe that droplets undergo continuous evolution interspersed by occasional large rearrangements in par with local relaxation behavior typical of foams.

Effect of emulsion size and shelf life of azadirachtin A on the bioefficacy of neem (Azadirachta indica A. Juss) emulsifiable concentrates.

PubMed

Kumar, L; Parmar, B S

2000-08-01

In a study of 33 recipes of neem oil based emulsifiable concentrates, the specific surface area of the emulsions and cream plus oil layer separation in emulsions at 24 h revealed a correlation of -0.6874 between them and correlations of -0.8940 and 0.6972, respectively, with bioefficacy (LC(50)) against the 3-day-old second-instar larvae of the Bihar hairy caterpillar, Spilosoma obliqua Walker. Nearly 96-99% of azadirachtin A in emulsifiable concentrates (aza-A content = 617.93-1149.65 ppm) degraded during the heat stability test at 54 +/- 1 degrees C for 14 days with half-lives ranging between 1.84 and 4.53 days. The LC(50) values against S. obliqua were, however, statistically at par in both the pre- and the post-heat-treated samples, suggesting a similar effect of azadirachtin A and its degradation products on the bioactivity. The half-life of azadirachtin A could be enhanced by storing the concentrates at lower temperatures. A low pH of the formulation solvent did not check the degradation of azadirachtin A, as reported with aqueous solutions in the literature.

Effects of poly(lactic-co-glycolic acid) on preparation and characteristics of plasmid DNA-loaded solid lipid nanoparticles.

PubMed

Zhu, L; Xie, S; Dong, Z; Wang, X; Wang, Y; Zhou, W

2011-09-01

Poly(lactic-co-glycolic acid) (PLGA) was used as a polymeric emulsifier to encapsulate plasmid DNA into hydrogenated castor oil (HCO)-solid lipid nanoparticles (SLN) by w/o/w double emulsion and solvent evaporation techniques. The effects of PLGA on the preparation, characteristics and transfection efficiency of DNA-loaded SLN were studied. The results showed that PLGA was essential to form the primary w/o emulsion and the stability of the emulsion was enhanced with the increase of PLGA content. DNA-loaded SLN were spherical with smooth surfaces. The SLN had a negative charge in weak acid and alkaline environment but acquired a positive charge in acidic pH and the cationisation capacity of the SLN increased with the increase of PLGA/HCO ratio. Agarose gel electrophoresis demonstrated that the majority of the DNA maintained its structural integrity after preparation and being extracted or released from DNA-loaded SLN. When PLGA/HCO ratio increased from 5 to 15%, the encapsulation efficiency, loading capacity and transfection efficiency of the nanoparticles increased significantly, whereas the changes of particle size and polydispersity index were insignificant. Cytotoxicity study in cell culture demonstrated that the SLN was not toxic.

Low-density solvent based ultrasound-assisted emulsification microextraction and on-column derivatization combined with gas chromatography-mass spectrometry for the determination of carbamate pesticides in environmental water samples.

PubMed

Guo, Liang; Lee, Hian Kee

2012-04-27

A fast and efficient method for the determination of trace level of carbamate pesticides using a lower-density-than-water solvent for ultrasound-assisted emulsification microextraction coupled to on-column derivatization and analysis by GC-MS has been developed and studied. In this approach, a soft plastic Pasteur pipette was employed as a convenient extraction device. Fifty microliters of extraction solvent, of lower density than water, was injected into the sample solution held in the pipette. The latter was immediately immersed in an ultrasound water bath to form an emulsion. After 2 min extraction, the emulsion was fractionated into two layers by centrifugation. The upper layer (organic extract) could be collected conveniently by squeezing the bulb of the pipette, now held upside down, to move it into the narrow stem of the device, facilitating its retrieval for analysis. The extract was then combined with trimethylphenylammonium hydroxide and directly injected into a gas chromatography-mass spectrometry (GC-MS) system for on-column derivatization and analysis. The on-column derivatization provided an added convenience (since a separate step was not necessary). Parameters affecting the derivatization and extraction were investigated. Under the most favorable conditions, the method demonstrated high extraction efficiency with low limits of detection of between 0.01 and 0.1 μg/L, good linearity in the range of 0.05-50 μg/L, to 0.5-100 μg/L, and good repeatability (RSD below 9.2%, n=5). The proposed method was evaluated by determining carbamate pesticides in river water samples. Copyright © 2012 Elsevier B.V. All rights reserved.

High drug loading self-microemulsifying/micelle formulation: design by high-throughput formulation screening system and in vivo evaluation.

PubMed

Sakai, Kenichi; Obata, Kouki; Yoshikawa, Mayumi; Takano, Ryusuke; Shibata, Masaki; Maeda, Hiroyuki; Mizutani, Akihiko; Terada, Katsuhide

2012-10-01

To design a high drug loading formulation of self-microemulsifying/micelle system. A poorly-soluble model drug (CH5137291), 8 hydrophilic surfactants (HS), 10 lipophilic surfactants (LS), 5 oils, and PEG400 were used. A high loading formulation was designed by a following stepwise approach using a high-throughput formulation screening (HTFS) system: (1) an oil/solvent was selected by solubility of the drug; (2) a suitable HS for highly loading was selected by the screenings of emulsion/micelle size and phase stability in binary systems (HS, oil/solvent) with increasing loading levels; (3) a LS that formed a broad SMEDDS/micelle area on a phase diagram containing the HS and oil/solvent was selected by the same screenings; (4) an optimized formulation was selected by evaluating the loading capacity of the crystalline drug. Aqueous solubility behavior and oral absorption (Beagle dog) of the optimized formulation were compared with conventional formulations (jet-milled, PEG400). As an optimized formulation, d-α-tocopheryl polyoxyethylene 1000 succinic ester: PEG400 = 8:2 was selected, and achieved the target loading level (200 mg/mL). The formulation formed fine emulsion/micelle (49.1 nm), and generated and maintained a supersaturated state at a higher level compared with the conventional formulations. In the oral absorption test, the area under the plasma concentration-time curve of the optimized formulation was 16.5-fold higher than that of the jet-milled formulation. The high loading formulation designed by the stepwise approach using the HTFS system improved the oral absorption of the poorly-soluble model drug.

Comparation of Hypolipidemic and Antioxidant Effects of Aqueous and Ethanol Extracts of Crataegus pinnatifida Fruit in High-Fat Emulsion-Induced Hyperlipidemia Rats

PubMed Central

Shao, Feng; Gu, Lifei; Chen, Huijuan; Liu, Ronghua; Huang, Huilian; Ren, Gang

2016-01-01

Background: Hawthorn (Crataegus pinnatifida) is a Chinese medicinal plant traditionally used in the treatment of hyperlipidemia. Recently, studies indicated free radical scavenging was one of the major pathways to alleviate hyperlipidemia. Moreover, hawthorn fruit is a rich source of phenols, which quench free radical and attenuate hyperlipidemia. However, the phenols vary with processing methods, especially solvent type. Objective: Our aim was to compare hypolipidemic and antioxidant effects of aqueous and ethanol extracts of hawthorn fruit in hyperlipidemia rats. Materials and Methods: After a 4-week treatment of high-fat emulsion, lipid profile levels and antioxidant levels of two extracts were determined using commercial analysis. Total phenols content in the extract of hawthorn fruit was determined colorimetrically by the Folin–Ciocalteu method. Results: Both ethanol and aqueous extracts of hawthorn fruit possessed hypolipidemic and antioxidant activities. Simultaneously, stronger activities were observed in ethanol extract. Besides, total phenols content in ethanol extract from the same quality of hawthorn fruit was 3.9 times more than that in aqueous extract. Conclusion: The obvious difference of hypolipidemic and antioxidant effects between ethanol extract and aqueous extract of hawthorn fruit was probably due to the presence of total phenols content, under the influence of extraction solvent. SUMMARY Ethanol extract of hawthorn fruit exhibited more favorable hypolipidemic and antioxidant effects than aqueous extract. The higher effects could be due to the higher content of total phenols that varies with extraction solvent. Abbreviations used: TC: Total cholesterol, TG: Triglyceride, LDL-C: Low-density lipoprotein cholesterol, HDL-C: High-density lipoprotein cholesterol, GSH-Px: Glutathione peroxidase, SOD: Superoxide dismutase, MDA: Malondialdehyde, CAT: Catalase, NO: Nitric oxide, NOS: Nitric oxide synthase, SR-BI: Scavenger receptor Class B Type I PMID:27019563

Comparation of Hypolipidemic and Antioxidant Effects of Aqueous and Ethanol Extracts of Crataegus pinnatifida Fruit in High-Fat Emulsion-Induced Hyperlipidemia Rats.

PubMed

Shao, Feng; Gu, Lifei; Chen, Huijuan; Liu, Ronghua; Huang, Huilian; Ren, Gang

2016-01-01

Hawthorn (Crataegus pinnatifida) is a Chinese medicinal plant traditionally used in the treatment of hyperlipidemia. Recently, studies indicated free radical scavenging was one of the major pathways to alleviate hyperlipidemia. Moreover, hawthorn fruit is a rich source of phenols, which quench free radical and attenuate hyperlipidemia. However, the phenols vary with processing methods, especially solvent type. Our aim was to compare hypolipidemic and antioxidant effects of aqueous and ethanol extracts of hawthorn fruit in hyperlipidemia rats. After a 4-week treatment of high-fat emulsion, lipid profile levels and antioxidant levels of two extracts were determined using commercial analysis. Total phenols content in the extract of hawthorn fruit was determined colorimetrically by the Folin-Ciocalteu method. Both ethanol and aqueous extracts of hawthorn fruit possessed hypolipidemic and antioxidant activities. Simultaneously, stronger activities were observed in ethanol extract. Besides, total phenols content in ethanol extract from the same quality of hawthorn fruit was 3.9 times more than that in aqueous extract. The obvious difference of hypolipidemic and antioxidant effects between ethanol extract and aqueous extract of hawthorn fruit was probably due to the presence of total phenols content, under the influence of extraction solvent. Ethanol extract of hawthorn fruit exhibited more favorable hypolipidemic and antioxidant effects than aqueous extract. The higher effects could be due to the higher content of total phenols that varies with extraction solvent. Abbreviations used: TC: Total cholesterol, TG: Triglyceride, LDL-C: Low-density lipoprotein cholesterol, HDL-C: High-density lipoprotein cholesterol, GSH-Px: Glutathione peroxidase, SOD: Superoxide dismutase, MDA: Malondialdehyde, CAT: Catalase, NO: Nitric oxide, NOS: Nitric oxide synthase, SR-BI: Scavenger receptor Class B Type I.

Preparation and evaluation of sustained release microballoons of propranolol.

PubMed

Porwal, A; Swami, G; Saraf, Sa

2011-01-01

The purpose of the present investigation was to characterize, optimize and evaluate microballoons of Propranolol hydrochloride and to increase its boioavailability by increasing the retention time of the drug in the gastrointestinal tract. Propranolol hydrochloride-loaded microballoons were prepared by the non-aqueous O/O emulsion solvent diffusion evaporation method using Eudragit RSPO as polymer. It was found that preparation temperature determined the formation of cavity inside the microballoon and this in turn determined the buoyancy. Microballoons were subjected to particle size determination, micromeritic properties, buoyancy, entrapment efficiency, drug loading, in vitro drug release and IR study. The correlation between the buoyancy, bulk density and porosity of microballoons were elucidated. The release rate was determined in simulated gastric fluid (SGF) of pH 1.2 at 37±0.5°C. The microballoons presented spherical and smooth morphologies (SEM) and were porous due to presence of hollow cavity. Microballoons remained buoyant for >12 hrs for the optimized formulation. The formulation demonstrated favorable in vitro floating and release characteristics. The encapsulation efficiency was high. In vitro dissolution kinetics followed the Higuchi model. The drug release from microballoons was mainly controlled by diffusion and showed a biphasic pattern with an initial burst release, followed by sustained release for 12 hrs. The amount of the drug which released up to 12 hrs was 82.05±0.64%. Statistical analysis (ANOVA) showed significant difference (p<0.05) in the cumulative amount of drug released after 30 min, and up to 12 hrs from optimized formulations. The designed system for propanolol would possibly be advantageous in terms of increased bioavailability and patient compliance.

Ion Pairing and Diffusion in Magnesium Electrolytes Based on Magnesium Borohydride.

PubMed

Samuel, Devon; Steinhauser, Carl; Smith, Jeffrey G; Kaufman, Aaron; Radin, Maxwell D; Naruse, Junichi; Hiramatsu, Hidehiko; Siegel, Donald J

2017-12-20

One obstacle to realizing a practical, rechargeable magnesium-ion battery is the development of efficient Mg electrolytes. Electrolytes based on simple Mg(BH 4 ) 2 salts suffer from poor salt solubility and/or low conductivity, presumably due to strong ion pairing. Understanding the molecular-scale processes occurring in these electrolytes would aid in overcoming these performance limitations. Toward this goal, the present study examines the solvation, agglomeration, and transport properties of a family of Mg electrolytes based on the Mg(BH 4 ) 2 salt using classical molecular dynamics. These properties were examined across five different solvents (tetrahydrofuran and the glymes G1-G4) and at four salt concentrations ranging from the dilute limit up to 0.4 M. Significant and irreversible salt agglomeration was observed in all solvents at all nondilute Mg(BH 4 ) 2 concentrations. The degree of clustering observed in these divalent Mg systems is much larger than that reported for electrolytes containing monovalent cations, such as Li. The salt agglomeration rate and diffusivity of Mg 2+ were both observed to correlate with solvent self-diffusivity: electrolytes using longer- (shorter-) chain solvents had the lowest (highest) Mg 2+ diffusivity and agglomeration rates. Incorporation of Mg 2+ into Mg 2+ -BH 4 - clusters significantly reduces the diffusivity of Mg 2+ by restricting displacements to localized motion within largely immobile agglomerates. Consequently, diffusion is increasingly impeded with increasing Mg(BH 4 ) 2 concentration. These data are consistent with the solubility limitations observed experimentally for Mg(BH 4 ) 2 -based electrolytes and highlight the need for strategies that minimize salt agglomeration in electrolytes containing divalent cations.

An investigation into the characteristics and drug release properties of multiple W/O/W emulsion systems containing low concentration of lipophilic polymeric emulsifier.

PubMed

Vasiljevic, Dragana; Parojcic, Jelena; Primorac, Marija; Vuleta, Gordana

2006-02-17

Multiple W/O/W emulsions with high content of inner phase (Phi1=Phi2=0.8) were prepared using relatively low concentrations of lipophilic polymeric primary emulsifier, PEG 30-dipolyhydroxystearate, and diclofenac diethylamine (DDA) as a model drug. The investigated formulations were characterized and their stability over the time was evaluated by dynamic and oscillatory rheological measurements, microscopic analysis and in vitro drug release study. In vitro release profiles of the selected model drug were evaluated in terms of the effective diffusion coefficients and flux of the released drug. The multiple emulsion samples exhibited good stability during the ageing time. Concentration of the lipophilic primary emulsifier markedly affected rheological behaviour as well as the droplet size and in vitro drug release kinetics of the investigated systems. The multiple emulsion systems with highest concentration (2.4%, w/w) of the primary emulsifier had the lowest droplet size and the highest apparent viscosity and highest elastic characteristics. Drug release data indicated predominately diffusional drug release mechanism with sustained and prolonged drug release accomplished with 2.4% (w/w) of lipophilic emulsifier employed.

Preparation of an Adhesive in Emulsion for Maxillofacial Prosthetic

PubMed Central

Sánchez-García, Judith A.; Ortega, Alejandra; Barceló-Santana, Federico H.; Palacios-Alquisira, Joaquín

2010-01-01

Maxillofacial prostheses is a dental medicine specialty aimed at restoring anatomical facial defects caused by cancer, trauma or congenital malformations through an artificial device, which is commonly attached to the skin with the help of an adhesive. The purpose of our research was to develop a pressure-sensitive adhesive (PSA) based on acrylic monomers, characterizing and determining its drying kinetics, that is to say the time it takes to lose 50 to 90% of its moisture. The adhesive synthesis was realized by means of emulsion polymerization; the composition of formulations was: (AA-MMA-EA) and (AA-MMA-2EHA) with different molar ratios. The formulation based on (AA-MMA-2EHA) with 50 w% of solids, presented good adhesive properties such as tack, bond strength, and short drying time. We propose this formulation as a PSA, because it offers an alternative for systemically compromised patients, by less irritation compared to organic solvent-based adhesives. PMID:21152308

Asphaltene dispersants as demulsification aids

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

Manek, M.B.

1995-11-01

Destabilization of petroleum asphaltenes may cause a multitude of problems in crude oil recovery and production. One major problem is their agglomeration at the water-oil interface of crude oil emulsions. Once agglomeration occurs, destabilized asphaltenes can form a thick pad in the dehydration equipment, which significantly reduces the demulsification rate. Certain polymeric dispersants increase asphaltene solubilization in hydrocarbon media, and when used in conjunction with emulsion breakers, facilitate the demulsification process. Two case studies are presented that demonstrate how asphaltene dispersants can efficiently inhibit pad formation and help reduce demulsifier dosage. Criteria for dispersant application and selection are discussed, whichmore » include the application of a novel laboratory technique to assess asphaltene stabilization in the crude oil. The technique monitors asphaltene agglomeration while undergoing titration with an incompatible solvent (precipitant). The method was used to evaluate stabilization of asphaltenes in the crude oil and to screen asphaltene dispersants.« less

Application of micro- and nanocrystalline cellulose

NASA Astrophysics Data System (ADS)

Sotnikova, Yu S.; Demina, T. S.; Istomin, A. V.; Goncharuk, G. P.; Grandfils, Ch; Akopova, T. A.; Zelenetskii, A. N.; Babayevsky, P. G.

2018-04-01

Micro- and nanocrystalline forms of cellulose were extracted from flax stalks and evaluated in terms of their applicability for various materials science tasks. It was revealed that both form of cellulose had anisometric morphology with length of 27.1 μm and 159 nm; diameter of 8.7 μm and 85 nm, respectively. They were used as reinforcing fillers for fabrication of composite films based on hydroxyethylcellulose. Film-forming and mechanical properties of the composite materials were significantly varied in dependence on filler content (0–10 wt.%) and size. As a second option of micro- and nanocrystalline cellulose application, a study of their effectiveness as stabilizing agents for oil/water Pickering emulsions was carried out. In contrast to micron-sized cellulose the nanocrystalline form appeared to be successful in the process of CH2Cl2/water interface stabilization and fabrication of polylactide microparticles via oil/water Pickering emulsion solvent evaporation technique.

Indomethacin-5-fluorouracil-methyl ester dry emulsion: a potential oral delivery system for 5-fluorouracil.

PubMed

Wang, Jing; Hu, Yanchen; Li, Ling; Jiang, Tongying; Wang, Siling; Mo, Fengkui

2010-06-01

To produce a combined effect of indomethacin (IDM) and 5-fluorouracil (5FU) for cancer therapy, the side effects of IDM on the gastrointestinal (GI) tract were reduced and the oral adsorption of 5FU was improved. Indomethacin-5-fluorouracil-methyl ester (IFM) dry emulsion was prepared and evaluated as a potential oral delivery system for 5FU. IFM was synthesized by formation of an ester between IDM and 5FU intermediate and then characterized by structure, melting point, solubility, apparent partition coefficient, and incubation with GI tract contents and plasma. Gum acacia and sodium carboxymethyl cellulose (CMC-Na) were applied as the adsorbent and solid carrier to prepare IFM dry emulsion. IFM dry emulsion was then characterized by reconstitution in water and in situ intestinal perfusion experiment. Physicochemical properties of the new synthesized compound confirmed the formation of IFM. Incubation of IFM in the contents of the GI tract and plasma revealed that IFM was not relatively stable in GI contents during the time period of transit through the GI tract, whereas it was very unstable in plasma and released 5FU rapidly. The IFM dry emulsion could be easily reconstituted in water, and the mean particle size was 2.416 microm. The absorption rate constant (K) for IFM with concentration of 2, 5, and 10 microg/mL in the in situ perfusion experiment were 0.473, 0.423, and 0.433/h, respectively, demonstrating passive diffusion of IFM across the biological membranes. This study indicates that the IFM dry emulsion may represent a potentially useful oral delivery system for 5FU.

Application of mercapto-silica polymerized high internal phase emulsions for the solid-phase extraction and preconcentration of trace lead(II).

PubMed

Su, Rihui; Ruan, Guihua; Chen, Zhengyi; Du, Fuyou; Li, Jianping

2015-12-01

A new class of solid-phase extraction column prepared with grafted mercapto-silica polymerized high internal phase emulsion particles was used for the preconcentration of trace lead. First, mercapto-silica polymerized high internal phase emulsion particles were synthesized by using high internal phase emulsion polymerization and carefully assembled in a polyethylene syringe column. The influences of various parameters including adsorption pH value, adsorption and desorption solvents, flow rate of the adsorption and desorption procedure were optimized, respectively, and the suitable uploading sample volumes, adsorption capacity, and reusability of solid phase extraction column were also investigated. Under the optimum conditions, Pb(2+) could be preconcentrated quantitatively over a wide pH range (2.0-5.0). In the presence of foreign ions, such as Na(+) , K(+) , Ca(2+) , Zn(2+) , Mg(2+) , Cu(2+) , Fe(2+) , Cd(2+) , Cl(-) and NO3 (-) , Pb(2+) could be recovered successfully. The prepared solid-phase extraction column performed with high stability and desirable durability, which allowed more than 100 replicate extractions without measurable changes of performance. The feasibility of the developed method was further validated by the extraction of Pb(2+) in rice samples. At three spiked levels of 40.0, 200 and 800 μg/kg, the average recoveries for Pb(2+) in rice samples ranged from 87.3 to 105.2%. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Integration of Gas Enhanced Oil Recovery in Multiphase Fermentations for the Microbial Production of Fuels and Chemicals.

PubMed

Pedraza-de la Cuesta, Susana; Keijzers, Lore; van der Wielen, Luuk A M; Cuellar, Maria C

2018-04-01

In multiphase fermentations where the product forms a second liquid phase or where solvents are added for product extraction, turbulent conditions disperse the oil phase as droplets. Surface-active components (SACs) present in the fermentation broth can stabilize the product droplets thus forming an emulsion. Breaking this emulsion increases process complexity and consequently the production cost. In previous works, it has been proposed to promote demulsification of oil/supernatant emulsions in an off-line batch bubble column operating at low gas flow rate. The aim of this study is to test the performance of this recovery method integrated to a fermentation, allowing for continuous removal of the oil phase. A 500 mL bubble column is successfully integrated with a 2 L reactor during 24 h without affecting cell growth or cell viability. However, higher levels of surfactants and emulsion stability are measured in the integrated system compared to a base case, reducing its capacity for oil recovery. This is related to release of SACs due to cellular stress when circulating through the recovery column. Therefore, it is concluded that the gas bubble-induced oil recovery method allows for oil separation and cell recycling without compromising fermentation performance; however, tuning of the column parameters considering increased levels of SACs due to cellular stress is required for improving oil recovery. © 2018 The Authors. Biotechnology Journal Published by Wiley-VCHVerlag GmbH & Co. KGaA, Weinheim.

Water-in-Water Emulsion Based Synthesis of Hydrogel Nanospheres with Tunable Release Kinetics

NASA Astrophysics Data System (ADS)

Aydın, Derya; Kızılel, Seda

2017-07-01

Poly(ethylene glycol) (PEG) micro/nanospheres have several unique advantages as polymer based drug delivery systems (DDS) such as tunable size, large surface area to volume ratio, and colloidal stability. Emulsification is one of the widely used methods for facile synthesis of micro/nanospheres. Two-phase aqueous system based on polymer-polymer immiscibility is a novel approach for preparation of water-in-water (w/w) emulsions. This method is promising for the synthesis of PEG micro/nanospheres for biological systems, since the emulsion is aqueous and do not require organic solvents or surfactants. Here, we report the synthesis of nano-scale PEG hydrogel particles using w/w emulsions using phase separation of dextran and PEG prepolymer. Dynamic light scattering (DLS) and scaning electron microscopy (SEM) results demonstrated that nano-scale hydrogel spheres could be obtained with this approach. We investigated the release kinetics of a model drug, pregabalin (PGB) from PEG nanospheres and demonstrated the influence of polymerization conditions on loading and release of the drug as well as the morphology and size distribution of PEG nanospheres. The experimental drug release data was fitted to a stretched exponential function which suggested high correlation with experimental results to predict half-time and drug release rates from the model equation. The biocompatibility of nanospheres on human dermal fibroblasts using cell-survival assay suggested that PEG nanospheres with altered concentrations are non-toxic, and can be considered for controlled drug/molecule delivery.

Femtosecond dynamics in hydrogen-bonded solvents

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

Castner, E.W. Jr.; Chang, Y.J.

1993-09-01

We present results on the ultrafast dynamics of pure hydrogen-bonding solvents, obtained using femtosecond Fourier-transform optical-heterodyne-detected, Raman-induced Kerr effect spectroscopy. Solvent systems we have studied include the formamides, water, ethylene glycol, and acetic acid. Inertial and diffusive motions are clearly resolved. We comment on the effect that such ultrafast solvent motions have on chemical reactions in solution.

Influence of the Formulation Parameters on the Particle Size and Encapsulation Efficiency of Resveratrol in PLA and PLA-PEG Blend Nanoparticles: A Factorial Design.

PubMed

Lindner, Gabriela da Rocha; Dalmolin, Luciana Facco; Khalil, Najeh Maissar; Mainardes, Rubiana Mara

2015-12-01

Polymeric nanoparticles are colloidal systems that promote protection and modification of physicochemical characteristics of a drug and that also ensure controlled and extended drug release. This paper reports a 2(3) factorial design study to optimize poly(lactide) (PLA) and poly(lactide)-polyethylene glycol (PLA-PEG) blend nanoparticles containing resveratrol (RVT) for prolonged release. The independent variables analyzed were solvent composition, surfactant concentration and ratio of aqueous to organic phase (two levels each factor). Mean particle size and RVT encapsulation efficiency were set as the dependent variables. The selected optimized parameters were set as organic phase comprised of a mixture of dichloromethane and ethyl acetate, 1% of surfactant polyvinyl alcohol and a 3:1 ratio of aqueous to organic phase, for both PLA and PLA-PEG blend nanoparticles. This formulation originated nanoparticles with size of 228 ± 10 nm and 185 ± 70 nm and RVT encapsulation efficiency of 82 ± 10% and 76 ± 7% for PLA and PLA-PEG blend nanoparticles, respectively. The in vitro release study showed a biphasic pattern with prolonged RVT release and PEG did not influence the RVT release. The in vitro release data were in favor of Higuchi-diffusion kinetics for both nanoformulations and the Kossmeyer-Peppas coefficient indicated that anomalous transport was the main release mechanism of RVT. PLA and PLA-PEG blend nanoparticles produced with single emulsion-solvent evaporation technology were found to be a promising approach for the incorporation of RVT and promoted its controlled release. The factorial design is a tool of great value in choosing formulations with optimized parameters.

Polymeric nanoparticles containing diazepam: preparation, optimization, characterization, in-vitro drug release and release kinetic study

NASA Astrophysics Data System (ADS)

Bohrey, Sarvesh; Chourasiya, Vibha; Pandey, Archna

2016-03-01

Nanoparticles formulated from biodegradable polymers like poly(lactic-co-glycolic acid) (PLGA) are being extensively investigated as drug delivery systems due to their two important properties such as biocompatibility and controlled drug release characteristics. The aim of this work to formulated diazepam loaded PLGA nanoparticles by using emulsion solvent evaporation technique. Polyvinyl alcohol (PVA) is used as stabilizing agent. Diazepam is a benzodiazepine derivative drug, and widely used as an anticonvulsant in the treatment of various types of epilepsy, insomnia and anxiety. This work investigates the effects of some preparation variables on the size and shape of nanoparticles prepared by emulsion solvent evaporation method. These nanoparticles were characterized by photon correlation spectroscopy (PCS), transmission electron microscopy (TEM). Zeta potential study was also performed to understand the surface charge of nanoparticles. The drug release from drug loaded nanoparticles was studied by dialysis bag method and the in vitro drug release data was also studied by various kinetic models. The results show that sonication time, polymer content, surfactant concentration, ratio of organic to aqueous phase volume, and the amount of drug have an important effect on the size of nanoparticles. Hopefully we produced spherical shape Diazepam loaded PLGA nanoparticles with a size range under 250 nm with zeta potential -23.3 mV. The in vitro drug release analysis shows sustained release of drug from nanoparticles and follow Korsmeyer-Peppas model.

PLGA nanoparticles loaded with the antileishmanial saponin β-aescin: factor influence study and in vitro efficacy evaluation.

PubMed

Van de Ven, H; Vermeersch, M; Matheeussen, A; Vandervoort, J; Weyenberg, W; Apers, S; Cos, P; Maes, L; Ludwig, A

2011-11-25

Colloidal carriers are known to improve the therapeutic index of the conventional drugs in the treatment of visceral leishmaniasis (VL) by decreasing their toxicity whilst maintaining or increasing therapeutic efficacy. This paper describes the development of poly(d,l-lactide-co-glycolide) (PLGA) nanoparticles (NPs) for the antileishmanial saponin β-aescin. NPs were prepared by the W/O/W emulsification solvent evaporation technique and the influence of five preparation parameters on the NPs' size (Z(ave)), zeta potential and entrapment efficiency (EE%) was investigated using a 2(5-2) fractional factorial design. Cytotoxicity of aescin, aescin-loaded and blank PLGA NPs was evaluated in J774 macrophages and non-phagocytic MRC-5 cells, whereas antileishmanial activity was determined in the Leishmania infantum ex vivo model. The developed PLGA NPs were monodispersed with Z(ave)<500 nm and exhibited negative zeta potentials. The process variables 'surfactant primary emulsion', 'concentration aescin' and 'solvent evaporation rate' had a positive effect on EE%. Addition of Tween 80 to the inner aqueous phase rendered the primary emulsion more stable, which in its turn led to better saponin entrapment. The selectivity index (SI) towards the supporting host macrophages increased from 4 to 18 by treating the cells with aescin-loaded NPs instead of free β-aescin. In conclusion, the in vitro results confirmed our hypothesis. Copyright © 2011 Elsevier B.V. All rights reserved.

Solvent annealing of perovskite-induced crystal growth for photovoltaic-device efficiency enhancement

DOE PAGES

Xiao, Zhengguo; Dong, Qingfeng; Bi, Cheng; ...

2014-08-26

Solvent-annealing is found to be an effective method to increase the grain size and carrier diffusion lengths of trihalide perovskite materials. Thus, the carrier diffusion length of MAPbI 3 is increased to over 1 μm. The efficiency remains above 14.5% when the MAPbI 3 thickness changes from 250 nm to 1 μm, with the highest efficiency reaching 15.6%.

Apparatus for diffusion-gap thermal desalination

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

Lowenstein, Andrew

A thermal distillation apparatus including evaporation surfaces that are wetted with a solution, and from which at least some of the volatile solvent contained in the solution evaporates, condensers having an external surface in close proximity to, but not touching, a corresponding one of the one or more evaporation surfaces, and on which vapors of the solvent condense, releasing thermal energy that heats a flow of the solution moving upward within the condensers, spacers that prevent contact between the evaporating surfaces and the condensers, wherein spaces between the evaporating surfaces and the condensers are filled with a gaseous mixture composedmore » of solvent vapor and one or more non-condensable gases, and except for diffusion of the solvent vapor relative to the non-condensable gases, the gaseous mixture is stationary.« less

Ionic conduction and self-diffusion near infinitesimal concentration in lithium salt-organic solvent electrolytes

NASA Astrophysics Data System (ADS)

Aihara, Yuichi; Sugimoto, Kyoko; Price, William S.; Hayamizu, Kikuko

2000-08-01

The Debye-Hückel-Onsager and Nernst-Einstein equations, which are based on two different conceptual approaches, constitute the most widely used equations for relating ionic conduction to ionic mobility. However, both of these classical (simple) equations are predictive of ionic conductivity only at very low salt concentrations. In the present work the ionic conductivity of four organic solvent-lithium salt-based electrolytes were measured. These experimental conductivity values were then contrasted with theoretical values calculated using the translational diffusion (also known as self-diffusion or intradiffusion) coefficients of all of the species present obtained using pulsed-gradient spin-echo (1H, 19F and 7Li) nuclear magnetic resonance self-diffusion measurements. The experimental results verified the applicability of both theoretical approaches at very low salt concentrations for these particular systems as well as helping to clarify the reasons for the divergence between theory and experiment. In particular, it was found that the correspondence between the Debye-Hückel-Onsager equation and experimental values could be improved by using the measured solvent self-diffusion values to correct for salt-induced changes in the solution viscosity. The concentration dependence of the self-diffusion coefficients is discussed in terms of the Jones-Dole equation.

Solvent Exchange Leading to Nanobubble Nucleation: A Molecular Dynamics Study

PubMed Central

2017-01-01

The solvent exchange procedure has become the most-used protocol to produce surface nanobubbles, while the molecular mechanisms behind the solvent exchange are far from being fully understood. In this paper, we build a simple model and use molecular dynamics simulations to investigate the dynamic characteristics of solvent exchange for producing nanobubbles. We find that at the first stage of solvent exchange, there exists an interface between interchanging solvents of different gas solubility. This interface moves toward the substrate gradually as the exchange process proceeds. Our simulations reveal directed diffusion of gas molecules against the gas concentration gradient, driven by the solubility gradient of the liquid composition across the moving solvent–solvent interface. It is this directed diffusion that causes gas retention and produces a local gas oversaturation much higher near the substrate than far from it. At the second stage of solvent exchange, the high local gas oversaturation leads to bubble nucleation either on the solid surface or in the bulk solution, which is found to depend on the substrate hydrophobicity and the degree of local gas oversaturation. Our findings suggest that solvent exchange could be developed into a standard procedure to produce oversaturation and used to a variety of nucleation applications other than generating nanobubbles. PMID:28742364

Conventional and dense gas techniques for the production of liposomes: a review.

PubMed

Meure, Louise A; Foster, Neil R; Dehghani, Fariba

2008-01-01

The aim of this review paper is to compare the potential of various techniques developed for production of homogenous, stable liposomes. Traditional techniques, such as Bangham, detergent depletion, ether/ethanol injection, reverse-phase evaporation and emulsion methods, were compared with the recent advanced techniques developed for liposome formation. The major hurdles for scaling up the traditional methods are the consumption of large quantities of volatile organic solvent, the stability and homogeneity of the liposomal product, as well as the lengthy multiple steps involved. The new methods have been designed to alleviate the current issues for liposome formulation. Dense gas liposome techniques are still in their infancy, however they have remarkable advantages in reducing the use of organic solvents, providing fast, single-stage production and producing stable, uniform liposomes. Techniques such as the membrane contactor and heating methods are also promising as they eliminate the use of organic solvent, however high temperature is still required for processing.

Solvent removal during synthetic and Nephila fiber spinning.

PubMed

Kojic, Nikola; Kojic, Milos; Gudlavalleti, Sauri; McKinley, Gareth

2004-01-01

The process by which spiders make their mechanically superior fiber involves removal of solvent (water) from a concentrated protein solution while the solution flows through a progressively narrowing spinning canal. Our aim was to determine a possible mechanism of spider water removal by using a computational model. To develop appropriate computational techniques for modeling of solvent removal during fiber spinning, a study was first performed using a synthetic solution. In particular, the effect of solvent removal during elongational flow (also exhibited in the spinning canal of the spider) on fiber mechanical properties was examined. The study establishes a model for solvent removal during dry spinning of synthetic fibers, assuming that internal diffusion governs solvent removal and that convective resistance is small. A variable internal solvent diffusion coefficient, dependent on solvent concentration, is also taken into account in the model. An experimental setup for dry (air) spinning was used to make fibers whose diameter was on the order of those made by spiders (approximately 1 microm). Two fibers of different thickness, corresponding to different spinning conditions, were numerically modeled for solvent removal and then mechanically tested. These tests showed that the thinner fiber, which lost more solvent under elongational flow, had 5-fold better mechanical properties (elastic modulus of 100 MPa and toughness of 15 MJ/m3) than the thicker fiber. Even though the mechanical properties were far from those of dragline spider silk (modulus of 10 GPa and toughness of 150 MJ/m3), the experimental methodology and numerical principles developed for the synthetic case proved to be valuable when establishing a model for the Nephila spinning process. In this model, an assumption of rapid convective water removal at the spinning canal wall was made, with internal diffusion of water through the fiber as the governing process. Then the diffusion coefficient of water through the initial spinning solution, obtained ex vivo from the Nephila clavipes major ampullate gland, was determined and incorporated into the numerical procedure, along with the wall boundary conditions and canal geometry. Also, a typical fiber reeling speed during web making, as well as the assumption of a dry exiting fiber, were included in the model. The results show that a cross-section of spinning solution (dope), which is initially 70% water, spends 19 s in the spinning canal in order to emerge dry. While the dope cross-section traverses the canal, its velocity increases from 0.37 mm/s at the entrance to 12.5 mm/s at the canal exit. The obtained results thus indicate that simple diffusion, along with the dry wall boundary condition, is a viable mechanism for water removal during typical Nephila fiber spinning.

Preparation and evaluation of sustained release loxoprofen loaded microspheres.

PubMed

Venkatesan, P; Manavalan, R; Valliappan, K

2011-06-01

The aim of present study was to formulate and evaluate the loxoprofen loaded Sustained release microspheres by emulsion solvent evaporation technique. Ethylcellulose, a biocompatible polymer is used as the retardant material. The effects of process conditions such as drug loading, polymer type and solvent type on the characteristics of microspheres were investigated. The prepared microspheres were characterized for their particle size and drug loading and drug release. The in-vitro release studies were carried out in phosphate buffer at pH 7.4. The prepared microspheres were white, free flowing and spherical in shape. The drug-loaded microspheres showed 71.2% of entrapment and the in-vitro release studies showed that Loxoprofen microspheres of 1:3 ratios showed better sustained effect over a period of 8 hours.

Preparation and evaluation of sustained release loxoprofen loaded microspheres

PubMed Central

Venkatesan, P.; Manavalan, R.; Valliappan, K.

2011-01-01

The aim of present study was to formulate and evaluate the loxoprofen loaded Sustained release microspheres by emulsion solvent evaporation technique. Ethylcellulose, a biocompatible polymer is used as the retardant material. The effects of process conditions such as drug loading, polymer type and solvent type on the characteristics of microspheres were investigated. The prepared microspheres were characterized for their particle size and drug loading and drug release. The in-vitro release studies were carried out in phosphate buffer at pH 7.4. The prepared microspheres were white, free flowing and spherical in shape. The drug-loaded microspheres showed 71.2% of entrapment and the in-vitro release studies showed that Loxoprofen microspheres of 1:3 ratios showed better sustained effect over a period of 8 hours PMID:24826017

Nonlinear Chemical Dynamics and Synchronization

NASA Astrophysics Data System (ADS)

Li, Ning

Alan Turing's work on morphogenesis, more than half a century ago, continues to motivate and inspire theoretical and experimental biologists even today. That said, there are very few experimental systems for which Turing's theory is applicable. In this thesis we present an experimental reaction-diffusion system ideally suited for testing Turing's ideas in synthetic "cells" consisting of microfluidically produced surfactant-stabilized emulsions in which droplets containing the Belousov-Zhabotinsky (BZ) oscillatory chemical reactants are dispersed in oil. The BZ reaction has become the prototype of nonlinear dynamics in chemistry and a preferred system for exploring the behavior of coupled nonlinear oscillators. Our system consists of a surfactant stabilized monodisperse emulsion of drops of aqueous BZ solution dispersed in a continuous phase of oil. In contrast to biology, here the chemistry is understood, rate constants are measured and interdrop coupling is purely diffusive. We explore a large set of parameters through control of rate constants, drop size, spacing, and spatial arrangement of the drops in lines and rings in one-dimension (1D) and hexagonal arrays in two-dimensions (2D). The Turing model is regarded as a metaphor for morphogenesis in biology but not for prediction. Here, we develop a quantitative and falsifiable reaction-diffusion model that we experimentally test with synthetic cells. We quantitatively establish the extent to which the Turing model in 1D describes both stationary pattern formation and temporal synchronization of chemical oscillators via reaction-diffusion and in 2D demonstrate that chemical morphogenesis drives physical differentiation in synthetic cells.

Preparation and characterization of spironolactone-loaded nano-emulsions for extemporaneous applications.

PubMed

Hallouard, François; Dollo, Gilles; Brandhonneur, Nolwenn; Grasset, Fabien; Corre, Pascal Le

2015-01-15

In neonates as well as in adults having swallowing difficulty, oral medication is given through a nasogastric tube making liquid formulations preferable. In this study, we present the high potential of nanometric emulsions formulated by spontaneous surfactant diffusion, as extemporaneous formulations of hydrophobic drug. Spironolactone used as hydrophobic drug model, was incorporated in oil before formulation at a concentration of 13.5mg/g oil. Then, all formulations were evaluated from pharmacotechnical and clinical standpoints, for their use in hospital or community pharmacy. The strength of this new liquid formulation lies on the simplicity, efficiency and reproducibility of their low energy process as on clinical aspects: high dose uniformity, facility to be administered through in nasogastric tube without any retention and a stability of 2 months at least compatible for an extemporaneous use. Moreover, this emulsion presented spironolactone content of 3.75 mg/ml among the most concentrated formulations published. Copyright © 2014 Elsevier B.V. All rights reserved.

Mass transport in polyelectrolyte solutions

NASA Astrophysics Data System (ADS)

Schipper, F. J. M.; Leyte, J. C.

1999-02-01

The self-diffusion coefficients of the three components of a salt-free heavy-water solution of polymethacrylic acid, completely neutralized with tetra-methylammonium hydroxide, were measured over a broad concentration range. Three concentration regions were observed for the self-diffusion of both the polyions and the counterions. At polyion concentrations below 0.01 mol monomer kg-1, the dilute concentration regime for the polymer, the polyion self-diffusion coefficient approaches the self-diffusion coefficient of a freely diffusing rod upon dilution. At polyelectrolyte concentrations above 0.1 mol monomer kg-1, the self-diffusion coefficients of the solvent, the counterions and the polymer decreased with concentration, suggesting that this decrease is due to a topological constraint on the motions of the components. In the intermediate-concentration region, the self-diffusion coefficients of the polyions and the counterions are independent of the concentration. The polyion dynamic behaviour is, in the intermediate- and high-concentration regions, reasonably well described by that of a hard sphere, with a radius of 3.7 nm. A correct prediction for the solvent dynamics is given by the obstruction effect of this hard sphere on the solvent. The relative counterion self-diffusion coefficient is predicted almost quantitatively over the entire concentration range with the Poisson-Boltzmann-Smoluchowski model for the spherical cell, provided that the sphere radius and the number of charges are chosen appropriately (approximately the number of charges in a persistence length). Using this model, the dependence of the counterion self-diffusion coefficient on the ionic strength, polyion concentration and counterion radius is calculated quantitatively over a large concentration range.

Quality by design approach for understanding the critical quality attributes of cyclosporine ophthalmic emulsion.

PubMed

Rahman, Ziyaur; Xu, Xiaoming; Katragadda, Usha; Krishnaiah, Yellela S R; Yu, Lawrence; Khan, Mansoor A

2014-03-03

Restasis is an ophthalmic cyclosporine emulsion used for the treatment of dry eye syndrome. There are no generic products for this product, probably because of the limitations on establishing in vivo bioequivalence methods and lack of alternative in vitro bioequivalence testing methods. The present investigation was carried out to understand and identify the appropriate in vitro methods that can discriminate the effect of formulation and process variables on critical quality attributes (CQA) of cyclosporine microemulsion formulations having the same qualitative (Q1) and quantitative (Q2) composition as that of Restasis. Quality by design (QbD) approach was used to understand the effect of formulation and process variables on critical quality attributes (CQA) of cyclosporine microemulsion. The formulation variables chosen were mixing order method, phase volume ratio, and pH adjustment method, while the process variables were temperature of primary and raw emulsion formation, microfluidizer pressure, and number of pressure cycles. The responses selected were particle size, turbidity, zeta potential, viscosity, osmolality, surface tension, contact angle, pH, and drug diffusion. The selected independent variables showed statistically significant (p < 0.05) effect on droplet size, zeta potential, viscosity, turbidity, and osmolality. However, the surface tension, contact angle, pH, and drug diffusion were not significantly affected by independent variables. In summary, in vitro methods can detect formulation and manufacturing changes and would thus be important for quality control or sameness of cyclosporine ophthalmic products.

Follicular delivery of spironolactone via nanostructured lipid carriers for management of alopecia.

PubMed

Shamma, Rehab Nabil; Aburahma, Mona Hassan

2014-01-01

Spironolactone (SL) is a US Food and Drug Administration-approved drug for the treatment of hypertension and various edematous conditions. SL has gained a lot of attention for treating androgenic alopecia due to its potent antiandrogenic properties. Recently, there has been growing interest for follicular targeting of drug molecules for treatment of hair and scalp disorders using nanocolloidal lipid-based delivery systems to minimize unnecessary systemic side effects associated with oral drug administration. Accordingly, the objective of this study is to improve SL efficiency and safety in treating alopecia through the preparation of colloidal nanostructured lipid carriers (NLCs) for follicular drug delivery. SL-loaded NLCs were prepared by an emulsion solvent diffusion and evaporation method using 23 full factorial design. All of the prepared formulations were spherical in shape with nanometric size range (215.6-834.3 nm) and entrapment efficiency >74%. Differential scanning calorimetry thermograms and X-ray diffractograms revealed that SL exists in amorphous form within the NLC matrices. The drug release behavior from the NLCs displayed an initial burst release phase followed by sustained release of SL. Confocal laser scanning microscopy confirmed the potential of delivering the fluorolabeled NLCs within the follicles, suggesting the possibility of using SL-loaded NLCs for localized delivery of SL into the scalp hair follicles.

Follicular delivery of spironolactone via nanostructured lipid carriers for management of alopecia

PubMed Central

Shamma, Rehab Nabil; Aburahma, Mona Hassan

2014-01-01

Spironolactone (SL) is a US Food and Drug Administration-approved drug for the treatment of hypertension and various edematous conditions. SL has gained a lot of attention for treating androgenic alopecia due to its potent antiandrogenic properties. Recently, there has been growing interest for follicular targeting of drug molecules for treatment of hair and scalp disorders using nanocolloidal lipid-based delivery systems to minimize unnecessary systemic side effects associated with oral drug administration. Accordingly, the objective of this study is to improve SL efficiency and safety in treating alopecia through the preparation of colloidal nanostructured lipid carriers (NLCs) for follicular drug delivery. SL-loaded NLCs were prepared by an emulsion solvent diffusion and evaporation method using 23 full factorial design. All of the prepared formulations were spherical in shape with nanometric size range (215.6–834.3 nm) and entrapment efficiency >74%. Differential scanning calorimetry thermograms and X-ray diffractograms revealed that SL exists in amorphous form within the NLC matrices. The drug release behavior from the NLCs displayed an initial burst release phase followed by sustained release of SL. Confocal laser scanning microscopy confirmed the potential of delivering the fluorolabeled NLCs within the follicles, suggesting the possibility of using SL-loaded NLCs for localized delivery of SL into the scalp hair follicles. PMID:25473283

Study of Antimicrobial Effects of Clarithromycin Loaded PLGA Nanoparticles against Clinical Strains of Helicobacter pylori.

PubMed

Lotfipour, F; Valizadeh, H; Milani, M; Bahrami, N; Ghotaslou, R

2016-01-01

Clarithromycin (CLR) formulation was prepared as PLGA nanoparticles in order to enhance the therapeutic effects using the distinctive features of a nanoparticulate delivery system. CLR loaded PLGA nanoparticles were prepared by Quasi Emulsion Solvent Diffusion (QESD) method using Poly lactic-co-Glycolic Acid (PLGA) as a biodegradable polymer. Antibacterial activity of the prepared formulations was evaluated against clinical strains of Helicobacter pylori, isolated from gastric biopsies of patients with gastritis, duodenal ulcer, peptic ulcer, and gastroesophageal reflux disease undergoing endoscopy, by using agar dilution method.Spherical nanoparticles with relatively narrow size distribution (between 200 and 800 nm) in the size range of 305 ± 138, 344 ± 148 and 362 ± 110 nm were achieved for F22, F23 and F23 respectively. CLR encapsulation percentages were measured to be 57.4 ± 4.3 to 80.2 ± 4.0%. CLR loaded PLGA nanoparticles showed equal or enhanced eradication effect against H. pylori strains according to the declined MIC values in comparison with the untreated CLR.In conclusion, the prepared CLR nanoformulation showed appropriate physicochemical properties and improved activity against H. pylori that could be a suitable candidate for oral preparations. © Georg Thieme Verlag KG Stuttgart · New York.

Preparation of polydopamine nanocapsules in a miscible tetrahydrofuran-buffer mixture.

PubMed

Ni, Yun-Zhou; Jiang, Wen-Feng; Tong, Gang-Sheng; Chen, Jian-Xin; Wang, Jie; Li, Hui-Mei; Yu, Chun-Yang; Huang, Xiao-hua; Zhou, Yong-Feng

2015-01-21

A miscible tetrahydrofuran-tris buffer mixture has been used to fabricate polydopamine hollow capsules with a size of 200 nm and with a shell thickness of 40 nm. An unusual non-emulsion soft template mechanism has been disclosed to explain the formation of capsules. The results indicate that the capsule structure is highly dependent on the volume fraction of tetrahydrofuran as well as the solvent, and the shell thickness of capsules can be controlled by adjusting the reaction time and dopamine concentration.

Concurrent bioremediation of perchlorate and 1,1,1-trichloroethane in an emulsified oil barrier

NASA Astrophysics Data System (ADS)

Borden, Robert C.

2007-10-01

A detailed field pilot test was conducted to evaluate the use of edible oil emulsions for enhanced in situ biodegradation of perchlorate and chlorinated solvents in groundwater. Edible oil substrate (EOS®) was injected into a line of ten direct push injection wells over a 2-day period to form a 15-m-long biologically active permeable reactive barrier (bio-barrier). Field monitoring results over a 2.5-year period indicate the oil injection generated strongly reducing conditions in the oil-treated zone with depletion of dissolved oxygen, nitrate, and sulfate, and increases in dissolved iron, manganese and methane. Perchlorate was degraded from 3100 to 20,000 μg/L to below detection (< 4 μg/L) in the injection and nearby monitor wells within 5 days following the injection. Two years after the single emulsion injection, perchlorate was less than 6 μg/L in every downgradient well compared to an average upgradient concentration of 13,100 μg/L. Immediately after emulsion injection, there were large shifts in concentrations of chlorinated solvents and degradation products due to injection of clean water, sorption to the oil and adaptation of the in situ microbial community. Approximately 4 months after emulsion injection, concentrations of 1,1,1-trichloroethane (TCA), perchloroethene (PCE), trichloroethene (TCE) and their degradation products appeared to reach a quasi steady-state condition. During the period from 4 to 18 months, TCA was reduced from 30-70 μM to 0.2-4 μM during passage through the bio-barrier. However, 1-9 μM 1,1-dichloroethane (DCA) and 8-14 μM of chloroethane (CA) remained indicating significant amounts of incompletely degraded TCA were discharging from the oil-treated zone. During this same period, PCE and TCE were reduced with concurrent production of 1,2- cis-dichloroethene ( cis-DCE). However, very little VC or ethene was produced indicating reductive dechlorination slowed or stopped at cis-DCE. The incomplete removal of TCA, PCE and TCE is likely associated with the short (5-20 days) hydraulic retention time of contaminants in the oil-treated zone. The permeability of the injection wells declined by 39-91% (average = 68%) presumably due to biomass growth and/or gas production. However, non-reactive tracer tests and detailed monitoring of the perchlorate plume demonstrated that the permeability loss did not result in excessive flow bypassing around the bio-barrier. Contaminant transport and degradation within the bio-barrier was simulated using an advection-dispersion-reaction model where biodegradation rate was assumed to be linearly proportional to the residual oil concentration ( Soil) and the contaminant concentration. Using this approach, the calibrated model was able to closely match the observed contaminant distribution. The calibrated model was then used to design a full-scale barrier to treat both ClO 4 and chlorinated solvents.

Concurrent bioremediation of perchlorate and 1,1,1-trichloroethane in an emulsified oil barrier.

PubMed

Borden, Robert C

2007-10-30

A detailed field pilot test was conducted to evaluate the use of edible oil emulsions for enhanced in situ biodegradation of perchlorate and chlorinated solvents in groundwater. Edible oil substrate (EOS) was injected into a line of ten direct push injection wells over a 2-day period to form a 15-m-long biologically active permeable reactive barrier (bio-barrier). Field monitoring results over a 2.5-year period indicate the oil injection generated strongly reducing conditions in the oil-treated zone with depletion of dissolved oxygen, nitrate, and sulfate, and increases in dissolved iron, manganese and methane. Perchlorate was degraded from 3100 to 20,000 microg/L to below detection (<4 microg/L) in the injection and nearby monitor wells within 5 days following the injection. Two years after the single emulsion injection, perchlorate was less than 6 microg/L in every downgradient well compared to an average upgradient concentration of 13,100 microg/L. Immediately after emulsion injection, there were large shifts in concentrations of chlorinated solvents and degradation products due to injection of clean water, sorption to the oil and adaptation of the in situ microbial community. Approximately 4 months after emulsion injection, concentrations of 1,1,1-trichloroethane (TCA), perchloroethene (PCE), trichloroethene (TCE) and their degradation products appeared to reach a quasi steady-state condition. During the period from 4 to 18 months, TCA was reduced from 30-70 microM to 0.2-4 microM during passage through the bio-barrier. However, 1-9 microM 1,1-dichloroethane (DCA) and 8-14 microM of chloroethane (CA) remained indicating significant amounts of incompletely degraded TCA were discharging from the oil-treated zone. During this same period, PCE and TCE were reduced with concurrent production of 1,2-cis-dichloroethene (cis-DCE). However, very little VC or ethene was produced indicating reductive dechlorination slowed or stopped at cis-DCE. The incomplete removal of TCA, PCE and TCE is likely associated with the short (5-20 days) hydraulic retention time of contaminants in the oil-treated zone. The permeability of the injection wells declined by 39-91% (average=68%) presumably due to biomass growth and/or gas production. However, non-reactive tracer tests and detailed monitoring of the perchlorate plume demonstrated that the permeability loss did not result in excessive flow bypassing around the bio-barrier. Contaminant transport and degradation within the bio-barrier was simulated using an advection-dispersion-reaction model where biodegradation rate was assumed to be linearly proportional to the residual oil concentration (Soil) and the contaminant concentration. Using this approach, the calibrated model was able to closely match the observed contaminant distribution. The calibrated model was then used to design a full-scale barrier to treat both ClO4 and chlorinated solvents.

Effects of solvent evaporation on water sorption/solubility and nanoleakage of adhesive systems.

PubMed

Chimeli, Talita Baumgratz Cachapuz; D'Alpino, Paulo Henrique Perlatti; Pereira, Patrícia Nóbrega; Hilgert, Leandro Augusto; Di Hipólito, Vinicius; Garcia, Fernanda Cristina Pimentel

2014-01-01

To evaluate the influence of solvent evaporation in the kinetics of water diffusion (water sorption-WS, solubility-SL, and net water uptake) and nanoleakage of adhesive systems. Disk-shaped specimens (5.0 mm in diameter x 0.8 mm in thickness) were produced (N=48) using the adhesives: Clearfil S3 Bond (CS3)/Kuraray, Clearfil SE Bond - control group (CSE)/Kuraray, Optibond Solo Plus (OS)/Kerr and Scotchbond Universal Adhesive (SBU)/3M ESPE. The solvents were either evaporated for 30 s or not evaporated (N=24/per group), and then photoactivated for 80 s (550 mW/cm2). After desiccation, the specimens were weighed and stored in distilled water (N=12) or mineral oil (N=12) to evaluate the water diffusion over a 7-day period. Net water uptake (%) was also calculated as the sum of WS and SL. Data were submitted to 3-way ANOVA/Tukey's test (α=5%). The nanoleakage expression in three additional specimens per group was also evaluated after ammoniacal silver impregnation after 7 days of water storage under SEM. Statistical analysis revealed that only the factor "adhesive" was significant (p<0.05). Solvent evaporation had no influence in the WS and SL of the adhesives. CSE (control) presented significantly lower net uptake (5.4%). The nanoleakage was enhanced by the presence of solvent in the adhesives. Although the evaporation has no effect in the kinetics of water diffusion, the nanoleakage expression of the adhesives tested increases when the solvents are not evaporated.

Solidification of floating organic droplet in dispersive liquid-liquid microextraction as a green analytical tool.

PubMed

Mansour, Fotouh R; Danielson, Neil D

2017-08-01

Dispersive liquid-liquid microextraction (DLLME) is a special type of microextraction in which a mixture of two solvents (an extracting solvent and a disperser) is injected into the sample. The extraction solvent is then dispersed as fine droplets in the cloudy sample through manual or mechanical agitation. Hence, the sample is centrifuged to break the formed emulsion and the extracting solvent is manually separated. The organic solvents commonly used in DLLME are halogenated hydrocarbons that are highly toxic. These solvents are heavier than water, so they sink to the bottom of the centrifugation tube which makes the separation step difficult. By using solvents of low density, the organic extractant floats on the sample surface. If the selected solvent such as undecanol has a freezing point in the range 10-25°C, the floating droplet can be solidified using a simple ice-bath, and then transferred out of the sample matrix; this step is known as solidification of floating organic droplet (SFOD). Coupling DLLME to SFOD combines the advantages of both approaches together. The DLLME-SFOD process is controlled by the same variables of conventional liquid-liquid extraction. The organic solvents used as extractants in DLLME-SFOD must be immiscible with water, of lower density, low volatility, high partition coefficient and low melting and freezing points. The extraction efficiency of DLLME-SFOD is affected by types and volumes of organic extractant and disperser, salt addition, pH, temperature, stirring rate and extraction time. This review discusses the principle, optimization variables, advantages and disadvantages and some selected applications of DLLME-SFOD in water, food and biomedical analysis. Copyright © 2017 Elsevier B.V. All rights reserved.

Emulsion-Based Intradermal Delivery of Melittin in Rats.

PubMed

Han, Sang Mi; Kim, Se Gun; Pak, Sok Cheon

2017-05-19

Bee venom (BV) has long been used as a traditional medicine. The aim of the present study was to formulate a BV emulsion with good rheological properties for dermal application and investigate the effect of formulation on the permeation of melittin through dermatomed rat skin. A formulated emulsion containing 1% ( w / v ) BV was prepared. The emulsion was compared with distilled water (DW) and 25% ( w / v ) N -methyl-2-pyrrolidone (NMP) in DW. Permeation of melittin from aqueous solution through the dermatomed murine skin was evaluated using the Franz diffusion cells. Samples of receptor cells withdrawn at pre-determined time intervals were measured for melittin amount. After the permeation study, the same skin was used for melittin extraction. In addition, a known amount of melittin (5 μg/mL) was added to stratum corneum, epidermis, and dermis of the rat skin, and the amount of melittin was measured at pre-determined time points. The measurement of melittin from all samples was done with HPLC-MS/MS. No melittin was detected in the receptor phase at all time points in emulsion, DW, or NMP groups. When the amount of melittin was further analyzed in stratum corneum, epidermis, and dermis from the permeation study, melittin was still not detected. In an additional experiment, the amount of melittin added to all skin matrices was corrected against the amount of melittin recovered. While the total amount of melittin was retained in the stratum corneum, less than 10% of melittin remained in epidermis and dermis within 15 and 30 min, respectively. Skin microporation with BV emulsion facilitates the penetration of melittin across the stratum corneum into epidermis and dermis, where emulsified melittin could have been metabolized by locally-occurring enzymes.

DIFFUSED SOLUTE-SOLVENT INTERFACE WITH POISSON-BOLTZMANN ELECTROSTATICS: FREE-ENERGY VARIATION AND SHARP-INTERFACE LIMIT.

PubMed

Li, B O; Liu, Yuan

A phase-field free-energy functional for the solvation of charged molecules (e.g., proteins) in aqueous solvent (i.e., water or salted water) is constructed. The functional consists of the solute volumetric and solute-solvent interfacial energies, the solute-solvent van der Waals interaction energy, and the continuum electrostatic free energy described by the Poisson-Boltzmann theory. All these are expressed in terms of phase fields that, for low free-energy conformations, are close to one value in the solute phase and another in the solvent phase. A key property of the model is that the phase-field interpolation of dielectric coefficient has the vanishing derivative at both solute and solvent phases. The first variation of such an effective free-energy functional is derived. Matched asymptotic analysis is carried out for the resulting relaxation dynamics of the diffused solute-solvent interface. It is shown that the sharp-interface limit is exactly the variational implicit-solvent model that has successfully captured capillary evaporation in hydrophobic confinement and corresponding multiple equilibrium states of underlying biomolecular systems as found in experiment and molecular dynamics simulations. Our phase-field approach and analysis can be used to possibly couple the description of interfacial fluctuations for efficient numerical computations of biomolecular interactions.

Improvement studies on emission and combustion characteristics of DICI engine fuelled with colloidal emulsion of diesel distillate of plastic oil, TiO2 nanoparticles and water.

PubMed

Karisathan Sundararajan, Narayanan; Ammal, Anand Ramachandran Bhagavathi

2018-04-01

Experimentation was conducted on a single cylinder CI engine using processed colloidal emulsions of TiO 2 nanoparticle-water-diesel distillate of crude plastic diesel oil as test fuel. The test fuel was prepared with plastic diesel oil as the principal constituent by a novel blending technique with an aim to improve the working characteristics. The results obtained by the test fuel from the experiments were compared with that of commercial petro-diesel (CPD) fuel for same engine operating parameters. Plastic oil produced from high density polyethylene plastic waste by pyrolysis was subjected to fractional distillation for separating plastic diesel oil (PDO) that contains diesel range hydrocarbons. The blending process showed a little improvement in the field of fuel oil-water-nanometal oxide colloidal emulsion preparation due to the influence of surfactant in electrostatic stabilization, dielectric potential, and pH of the colloidal medium on the absolute value of zeta potential, a measure of colloidal stability. The engine tests with nano-emulsions of PDO showed an increase in ignition delay (23.43%), and decrease in EGT (6.05%), BSNO x (7.13%), and BSCO (28.96%) relative to PDO at rated load. Combustion curve profiles, percentage distribution of compounds, and physical and chemical properties of test fuels ascertains these results. The combustion acceleration at diffused combustion phase was evidenced in TiO 2 emulsion fuels under study.

Critical conditions for the buoyancy-driven detachment of a wall-bound pendant drop

NASA Astrophysics Data System (ADS)

Lamorgese, A.; Mauri, R.

2016-03-01

We investigate numerically the critical conditions for detachment of an isolated, wall-bound emulsion droplet acted upon by surface tension and wall-normal buoyancy forces alone. To that end, we present a simple extension of a diffuse-interface model for partially miscible binary mixtures that was previously employed for simulating several two-phase flow phenomena far and near the critical point [A. G. Lamorgese et al. "Phase-field approach to multiphase flow modeling," Milan J. Math. 79(2), 597-642 (2011)] to allow for static contact angles other than 90°. We use the same formulation of the Cahn boundary condition as first proposed by Jacqmin ["Contact-line dynamics of a diffuse fluid interface," J. Fluid Mech. 402, 57-88 (2000)], which accommodates a cubic (Hermite) interpolation of surface tensions between the wall and each phase at equilibrium. We show that this model can be successfully employed for simulating three-phase contact line problems in stable emulsions with nearly immiscible components. We also show a numerical determination of critical Bond numbers as a function of static contact angle by phase-field simulation.

Measuring Solvent Content of Macromolecular Crystals Using Fluorescence Recovery after Photobleaching

NASA Astrophysics Data System (ADS)

Siewny, Matthew; Kmetko, Jan

2010-10-01

We work out a novel protocol for measuring the solvent content (the fraction of crystal volume occupied by solvent) in biological crystals by the technique of fluorescence recovery after photobleaching (FRAP). Crystals of proteins with widely varying known solvent content (lysozyme, thaumatin, catalase, and ferritin) were grown in their native solution doped with sodium fluorescein dye and hydroxylamine (to prevent dye from binding to amine groups of the proteins.) The crystals were irradiated by a broadband, high intensity light through knife slits, leaving a rectangular area of bleached dye within the crystals. Measuring the flow of dye out of the bleached area allowed us to construct a curve relating the diffusion coefficient of dye to the channel size within the crystals, by solving the diffusion equation analytically. This curve may be used to measure the solvent content of any biological crystal in its native solution and help determine the number of proteins in the crystallographic asymmetric unit cell in x-ray structure solving procedures.

Effect of Aprotic Solvents on the Dynamics of a Room Temperature Ionic Liquid

NASA Astrophysics Data System (ADS)

Osti, Naresh; van Aken, Katherine; Thompson, Matthew; Tiet, Felix; Jiang, De-En; Cummings, Peter; Gogotsi, Yury; Mamontov, Eugene

Room temperature ionic liquids (RTILs) have attracted much attention as electrolytes in energy storage devices because of their peculiar physical and chemical characteristics. However, their remarkably high viscosity, which results in low conductivity and diffusivity, may adversely affect the charging and discharging rates. Despite changing molecular configurations, use of aprotic solvent allows to enhance the transport properties of ionic liquids by disrupting the cation-anion interactions. We explore the impact of dipole moment of aprotic solvents on the cation-anion interaction and transport in 1-butyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide, [BMIM +][Tf2N-], RTIL using molecular dynamics (MD) simulations and quasi-elastic neutrons scattering (QENS) measurements. We observed an increase in cation diffusivity with the increasing dipole moment of the solvent. This effect is due to a decrease in the solvation free energy induced by the increasing solvent polarity. A clear nano-phase separation into ionic liquid-rich and ionic liquid-poor phases as observed by QENS will be also discussed.

Molecular Dynamics Study of the Solution Structure, Clustering, and Diffusion of Four Aqueous Alkanolamines.

PubMed

Melnikov, Sergey M; Stein, Matthias

2018-03-15

CO 2 sequestration from anthropogenic resources is a challenge to the design of environmental processes at a large scale. Reversible chemical absorption by amine-based solvents is one of the most efficient methods of CO 2 removal. Molecular simulation techniques are very useful tools to investigate CO 2 binding by aqueous alkanolamine molecules for further technological application. In the present work, we have performed detailed atomistic molecular dynamics simulations of aqueous solutions of three prototype amines: monoethanolamine (MEA) as a standard, 3-aminopropanol (MPA), 2-methylaminoethanol (MMEA), and 4-diethylamino-2-butanol (DEAB) as potential novel CO 2 absorptive solvents. Solvent densities, radial distribution functions, cluster size distributions, hydrogen-bonding statistics, and diffusion coefficients for a full range of mixture compositions have been obtained. The solvent densities and diffusion coefficients from simulations are in good agreement with those in the experiment. In aqueous solution, MEA, MPA, and MMEA molecules prefer to be fully solvated by water molecules, whereas DEAB molecules tend to self-aggregate. In a range from 30/70-50/50 (w/w) alkanolamine/water mixtures, they form a bicontinuous phase (both alkanolamine and water are organized in two mutually percolating clusters). Among the studied aqueous alkanolamine solutions, the diffusion coefficients decrease in the following order MEA > MPA = MMEA > DEAB. With an increase of water content, the diffusion coefficients increase for all studied alkanolamines. The presented results are a first step for process-scale simulation and provide important qualitative and quantitative information for the design and engineering of efficient new CO 2 removal processes.

Radiation processed polychloroprene-co-ethylene-propene diene terpolymer blends: Effect of radiation vulcanization on solvent transport kinetics

NASA Astrophysics Data System (ADS)

Dubey, K. A.; Bhardwaj, Y. K.; Chaudhari, C. V.; Kumar, Virendra; Goel, N. K.; Sabharwal, S.

2009-03-01

Blends of polychloroprene rubber (PCR) and ethylene propylene diene terpolymer rubber (EPDM) of different compositions were made and exposed to different gamma radiation doses. The radiation sensitivity and radiation vulcanization efficiency of blends was estimated by gel-content analysis, Charlesby-Pinner parameter determination and crosslinking density measurements. Gamma radiation induced crosslinking was most efficient for EPDM ( p0/ q0 ˜ 0.08), whereas it was the lowest for blends containing 40% PCR ( p0/ q0 ˜ 0.34). The vulcanized blends were characterized for solvent diffusion characteristics by following the swelling dynamics. Blends with higher PCR content showed anomalous swelling. The sorption and permeability of the solvent were not strictly in accordance with each other and the extent of variation in two parameters was found to be a function of blend composition. The Δ G values for solvent diffusion were in the range -2.97 to -9.58 kJ/mol and indicated thermodynamically favorable sorption for all blends. These results were corroborated by dynamic swelling, experimental as well as simulated profiles and have been explained on the basis of correlation between crosslinking density, diffusion kinetics, thermodynamic parameters and polymer-polymer interaction parameter.

A new desorption method for removing organic solvents from activated carbon using surfactant.

PubMed

Hinoue, Mitsuo; Ishimatsu, Sumiyo; Fueta, Yukiko; Hori, Hajime

2017-03-28

A new desorption method was investigated, which does not require toxic organic solvents. Efficient desorption of organic solvents from activated carbon was achieved with an ananionic surfactant solution, focusing on its washing and emulsion action. Isopropyl alcohol (IPA) and methyl ethyl ketone (MEK) were used as test solvents. Lauryl benzene sulfonic acid sodium salt (LAS) and sodium dodecyl sulfate (SDS) were used as the surfactant. Activated carbon (100 mg) was placed in a vial and a predetermined amount of organic solvent was added. After leaving for about 24 h, a predetermined amount of the surfactant solution was added. After leaving for another 72 h, the vial was heated in an incubator at 60°C for a predetermined time. The organic vapor concentration was then determined with a frame ionization detector (FID)-gas chromatograph and the desorption efficiency was calculated. A high desorption efficiency was obtained with a 10% surfactant solution (LAS 8%, SDS 2%), 5 ml desorption solution, 60°C desorption temperature, and desorption time of over 24 h, and the desorption efficiency was 72% for IPA and 9% for MEK. Under identical conditions, the desorption efficiencies for another five organic solvents were investigated, which were 36%, 3%, 32%, 2%, and 3% for acetone, ethyl acetate, dichloromethane, toluene, and m-xylene, respectively. A combination of two anionic surfactants exhibited a relatively high desorption efficiency for IPA. For toluene, the desorption efficiency was low due to poor detergency and emulsification power.

A new desorption method for removing organic solvents from activated carbon using surfactant

PubMed Central

Hinoue, Mitsuo; Ishimatsu, Sumiyo; Fueta, Yukiko; Hori, Hajime

2017-01-01

Objectives: A new desorption method was investigated, which does not require toxic organic solvents. Efficient desorption of organic solvents from activated carbon was achieved with an ananionic surfactant solution, focusing on its washing and emulsion action. Methods: Isopropyl alcohol (IPA) and methyl ethyl ketone (MEK) were used as test solvents. Lauryl benzene sulfonic acid sodium salt (LAS) and sodium dodecyl sulfate (SDS) were used as the surfactant. Activated carbon (100 mg) was placed in a vial and a predetermined amount of organic solvent was added. After leaving for about 24 h, a predetermined amount of the surfactant solution was added. After leaving for another 72 h, the vial was heated in an incubator at 60°C for a predetermined time. The organic vapor concentration was then determined with a frame ionization detector (FID)-gas chromatograph and the desorption efficiency was calculated. Results: A high desorption efficiency was obtained with a 10% surfactant solution (LAS 8%, SDS 2%), 5 ml desorption solution, 60°C desorption temperature, and desorption time of over 24 h, and the desorption efficiency was 72% for IPA and 9% for MEK. Under identical conditions, the desorption efficiencies for another five organic solvents were investigated, which were 36%, 3%, 32%, 2%, and 3% for acetone, ethyl acetate, dichloromethane, toluene, and m-xylene, respectively. Conclusions: A combination of two anionic surfactants exhibited a relatively high desorption efficiency for IPA. For toluene, the desorption efficiency was low due to poor detergency and emulsification power. PMID:28132972

Preparation and evaluation of sustained release microballoons of propranolol

PubMed Central

Porwal, A; Swami, G; Saraf, SA

2011-01-01

Background and the purpose of the study The purpose of the present investigation was to characterize, optimize and evaluate microballoons of Propranolol hydrochloride and to increase its boioavailability by increasing the retention time of the drug in the gastrointestinal tract. Methods Propranolol hydrochloride-loaded microballoons were prepared by the non-aqueous O/O emulsion solvent diffusion evaporation method using Eudragit RSPO as polymer. It was found that preparation temperature determined the formation of cavity inside the microballoon and this in turn determined the buoyancy. Microballoons were subjected to particle size determination, micromeritic properties, buoyancy, entrapment efficiency, drug loading, in vitro drug release and IR study. The correlation between the buoyancy, bulk density and porosity of microballoons were elucidated. The release rate was determined in simulated gastric fluid (SGF) of pH 1.2 at 37±0.5°C. Results The microballoons presented spherical and smooth morphologies (SEM) and were porous due to presence of hollow cavity. Microballoons remained buoyant for >12 hrs for the optimized formulation. The formulation demonstrated favorable in vitro floating and release characteristics. The encapsulation efficiency was high. In vitro dissolution kinetics followed the Higuchi model. The drug release from microballoons was mainly controlled by diffusion and showed a biphasic pattern with an initial burst release, followed by sustained release for 12 hrs. The amount of the drug which released up to 12 hrs was 82.05±0.64%. Statistical analysis (ANOVA) showed significant difference (p<0.05) in the cumulative amount of drug released after 30 min, and up to 12 hrs from optimized formulations. Conclusion The designed system for propanolol would possibly be advantageous in terms of increased bioavailability and patient compliance. PMID:22615657

Quality by design case study 1: Design of 5-fluorouracil loaded lipid nanoparticles by the W/O/W double emulsion - Solvent evaporation method.

PubMed

Amasya, Gulin; Badilli, Ulya; Aksu, Buket; Tarimci, Nilufer

2016-03-10

With Quality by Design (QbD), a systematic approach involving design and development of all production processes to achieve the final product with a predetermined quality, you work within a design space that determines the critical formulation and process parameters. Verification of the quality of the final product is no longer necessary. In the current study, the QbD approach was used in the preparation of lipid nanoparticle formulations to improve skin penetration of 5-Fluorouracil, a widely-used compound for treating non-melanoma skin cancer. 5-Fluorouracil-loaded lipid nanoparticles were prepared by the W/O/W double emulsion - solvent evaporation method. Artificial neural network software was used to evaluate the data obtained from the lipid nanoparticle formulations, to establish the design space, and to optimize the formulations. Two different artificial neural network models were developed. The limit values of the design space of the inputs and outputs obtained by both models were found to be within the knowledge space. The optimal formulations recommended by the models were prepared and the critical quality attributes belonging to those formulations were assigned. The experimental results remained within the design space limit values. Consequently, optimal formulations with the critical quality attributes determined to achieve the Quality Target Product Profile were successfully obtained within the design space by following the QbD steps. Copyright © 2016 Elsevier B.V. All rights reserved.

Charge transfer fluorescence and 34 nm exciton diffusion length in polymers with electron acceptor end traps

DOE PAGES

Zaikowski, Lori; Mauro, Gina; Bird, Matthew; ...

2014-12-22

Photoexcitation of conjugated poly-2,7-(9,9-dihexylfluorene) polyfluorenes with naphthylimide (NI) and anthraquinone (AQ) electron-acceptor end traps produces excitons that form charge transfer states at the end traps. Intramolecular singlet exciton transport to end traps was examined by steady state fluorescence for polyfluorenes of 17 to 127 repeat units in chloroform, dimethylformamide (DMF), tetrahydrofuran (THF), and p-xylene. End traps capture excitons and form charge transfer (CT) states at all polymer lengths and in all solvents. The CT nature of the end-trapped states is confirmed by their fluorescence spectra, solvent and trap group dependence and DFT descriptions. Quantum yields of CT fluorescence are asmore » large as 46%. This strong CT emission is understood in terms of intensity borrowing. Energies of the CT states from onsets of the fluorescence spectra give the depths of the traps which vary with solvent polarity. For NI end traps the trap depths are 0.06 (p-xylene), 0.13 (THF) and 0.19 eV (CHCl 3). For AQ, CT fluorescence could be observed only in p-xylene where the trap depth is 0.27 eV. Quantum yields, emission energies, charge transfer energies, solvent reorganization and vibrational energies were calculated. Fluorescence measurements on chains >100 repeat units indicate that end traps capture ~50% of the excitons, and that the exciton diffusion length L D =34 nm, which is much larger than diffusion lengths reported in polymer films or than previously known for diffusion along isolated chains. As a result, the efficiency of exciton capture depends on chain length, but not on trap depth, solvent polarity or which trap group is present.« less

Effects of solvent evaporation on water sorption/solubility and nanoleakage of adhesive systems

PubMed Central

CHIMELI, Talita Baumgratz Cachapuz; D'ALPINO, Paulo Henrique Perlatti; PEREIRA, Patrícia Nóbrega; HILGERT, Leandro Augusto; DI HIPÓLITO, Vinicius; GARCIA, Fernanda Cristina Pimentel

2014-01-01

Objective To evaluate the influence of solvent evaporation in the kinetics of water diffusion (water sorption-WS, solubility-SL, and net water uptake) and nanoleakage of adhesive systems. Material and Methods Disk-shaped specimens (5.0 mm in diameter x 0.8 mm in thickness) were produced (N=48) using the adhesives: Clearfil S3 Bond (CS3)/Kuraray, Clearfil SE Bond - control group (CSE)/Kuraray, Optibond Solo Plus (OS)/Kerr and Scotchbond Universal Adhesive (SBU)/3M ESPE. The solvents were either evaporated for 30 s or not evaporated (N=24/per group), and then photoactivated for 80 s (550 mW/cm2). After desiccation, the specimens were weighed and stored in distilled water (N=12) or mineral oil (N=12) to evaluate the water diffusion over a 7-day period. Net water uptake (%) was also calculated as the sum of WS and SL. Data were submitted to 3-way ANOVA/Tukey's test (α=5%). The nanoleakage expression in three additional specimens per group was also evaluated after ammoniacal silver impregnation after 7 days of water storage under SEM. Results Statistical analysis revealed that only the factor "adhesive" was significant (p<0.05). Solvent evaporation had no influence in the WS and SL of the adhesives. CSE (control) presented significantly lower net uptake (5.4%). The nanoleakage was enhanced by the presence of solvent in the adhesives. Conclusions Although the evaporation has no effect in the kinetics of water diffusion, the nanoleakage expression of the adhesives tested increases when the solvents are not evaporated. PMID:25141201

Asymmetric lipid-polymer particles (LIPOMER) by modified nanoprecipitation: role of non-solvent composition.

PubMed

Jindal, Anil B; Devarajan, Padma V

2015-07-15

Asymmetric lipid polymer nanostructures (LIPOMER) comprising glyceryl monostearate (GMS) as lipid and Gantrez AN 119 (Gantrez) as polymer, revealed enhanced splenic accumulation. In the present paper, we attempt to explain the formation of asymmetric GMS LIPOMER using real time imaging. Particles were prepared by precipitation under static conditions using different non-solvent phase compositions. The process was video recorded and the videos converted to time elapsed images using the FFmpeg 0.10.2 software at 25 frames/sec. Non-solvent compositions comprising >30% of IPA/Acetone revealed significant stranding of the solvent phase and slower onset of precipitation(2-6s). At lower concentrations of IPA and acetone, and in non-solvent compositions comprising ethanol/water the stranding phenomenon was not evident. Further, rapid precipitation(<1 s) was evident. Nanoprecipitation based on the Marangoni effect is a result of diffusion stranding, interfacial turbulence, and mass transfer of solvent and non-solvent resulting in solute precipitation. Enhanced diffusion stranding favored by high interaction of GMS and Gantrez(low ΔPol), and the low solubility parameter(Δδtotal) and high mixing enthalpy(ΔHM) of GMS in IPA resulted in droplets with random shapes analogous to an amoeba with pseudopodia, which on precipitation formed asymmetric particles. Asymmetric particles could be readily designed through appropriate selection of solutes and non-solvent phase by modified nanoprecipitation. Copyright © 2015 Elsevier B.V. All rights reserved.

Analysis of in vitro release through reconstructed human epidermis and synthetic membranes of multi-vitamins from cosmetic formulations.

PubMed

Gabbanini, Simone; Matera, Riccardo; Beltramini, Claudia; Minghetti, Andrea; Valgimigli, Luca

2010-08-01

A convenient method for in vitro investigation of the release of lipid- and water-soluble vitamins from cosmetic formulations was developed. The permeation of (d)-alpha-tocopherol (vitamin E), retinyl acetate (pro-vitamin A), ascorbic acid (vitamin C) and pyridoxine (vitamin B6) through SkinEthic reconstructed human epidermis (RHE), and synthetic polyethersulfone and polycarbonate membranes was studied in vitro using a Franz-type diffusion apparatus, coupled either to a spectrophotometer for continuous reading (dynamic setting) or to HPLC-DAD analysis of the receptor medium (static setting). O/W and W/O emulsions were compared with simple aqueous solutions for their kinetic of vitamins release, to evaluate the influence of the cosmetic formulation on the bioavailability of active ingredients. Results indicate that synthetic membranes offer a limited barrier to the diffusion of vitamins, but may provide information on the release ability of the formulation. Penetration was more effective when water was the external phase of the formulation, i.e. W/O emulsions were less effective in the release of vitamins than O/W emulsion or aqueous solutions. RHE (17 days old) offered a significantly higher barrier to penetration of vitamins, as expected for native human epidermis. The relative ranking in coefficient of permeability (Ps (cm/h)) was: ascorbic acid>pyridoxine>retinyl acetate>alpha-tocopherol approximately 0, the absolute values depending on the formulation. The method herein described showed to be a practical and convenient tool for the quality-control and efficacy evaluation of cosmetic formulations. Copyright (c) 2010 Elsevier B.V. All rights reserved.

Effects of process parameters on peanut skins extract and CO2 diffusivity by supercritical fluid extraction

NASA Astrophysics Data System (ADS)

Putra, N. R.; Yian, L. N.; Nasir, H. M.; Idham, Z. Binti; Yunus, M. A. C.

2018-03-01

Peanut skins (Arachis hypogea) are an agricultural waste product which has received much attention because they contain high nutritional values and can be potentially utilized in difference industries. At present, only a few studies have been conducted to study the effects of parameters on the peanut skins oil extraction. Therefore, this study aimed to determine the best extraction condition in order to obtain the highest extract yield using supercritical carbon dioxide (SC-CO2) with co-solvent Ethanol as compared to Soxhlet extraction method. Diffusivity of carbon dioxide in supercritical fluid extraction was determined using Crank model. The mean particle size used in this study was 425 µm. The supercritical carbon dioxide was performed at temperature (40 – 70 °C), flow rate of co-solvent ethanol (0 - 7.5% Vethanol/Vtotal), and extraction pressure (10 – 30 MPa) were used in this studies. The results showed that the percentage of oil yields and effective diffusivity increase as the pressure, rate of co-solvent, and temperature increased.

Emulsion droplet interactions: a front-tracking treatment

NASA Astrophysics Data System (ADS)

Mason, Lachlan; Juric, Damir; Chergui, Jalel; Shin, Seungwon; Craster, Richard V.; Matar, Omar K.

2017-11-01

Emulsion coalescence influences a multitude of industrial applications including solvent extraction, oil recovery and the manufacture of fast-moving consumer goods. Droplet interaction models are vital for the design and scale-up of processing systems, however predictive modelling at the droplet-scale remains a research challenge. This study simulates industrially relevant moderate-inertia collisions for which a high degree of droplet deformation occurs. A hybrid front-tracking/level-set approach is used to automatically account for interface merging without the need for `bookkeeping' of interface connectivity. The model is implemented in Code BLUE using a parallel multi-grid solver, allowing both film and droplet-scale dynamics to be resolved efficiently. Droplet interaction simulations are validated using experimental sequences from the literature in the presence and absence of background turbulence. The framework is readily extensible for modelling the influence of surfactants and non-Newtonian fluids on droplet interaction processes. EPSRC, UK, MEMPHIS program Grant (EP/K003976/1), RAEng Research Chair (OKM), PETRONAS.

Preparation of polycaprolactone nanoparticles via supercritical carbon dioxide extraction of emulsions.

PubMed

Ajiboye, Adejumoke Lara; Trivedi, Vivek; Mitchell, John C

2017-08-21

Polycaprolactone (PCL) nanoparticles were produced via supercritical fluid extraction of emulsions (SFEE) using supercritical carbon dioxide (scCO 2 ). The efficiency of the scCO 2 extraction was investigated and compared to that of solvent extraction at atmospheric pressure. The effects of process parameters including polymer concentration (0.6-10% w/w in acetone), surfactant concentration (0.07 and 0.14% w/w) and polymer-to-surfactant weight ratio (1:1-16:1 w/w) on the particle size and surface morphology were also investigated. Spherical PCL nanoparticles with mean particle sizes between 190 and 350 nm were obtained depending on the polymer concentration, which was the most important factor where increase in the particle size was directly related to total polymer content in the formulation. Nanoparticles produced were analysed using dynamic light scattering and scanning electron microscopy. The results indicated that SFEE can be applied for the preparation of PCL nanoparticles without agglomeration and in a comparatively short duration of only 1 h.

A scaled-ionic-charge simulation model that reproduces enhanced and suppressed water diffusion in aqueous salt solutions.

PubMed

Kann, Z R; Skinner, J L

2014-09-14

Non-polarizable models for ions and water quantitatively and qualitatively misrepresent the salt concentration dependence of water diffusion in electrolyte solutions. In particular, experiment shows that the water diffusion coefficient increases in the presence of salts of low charge density (e.g., CsI), whereas the results of simulations with non-polarizable models show a decrease of the water diffusion coefficient in all alkali halide solutions. We present a simple charge-scaling method based on the ratio of the solvent dielectric constants from simulation and experiment. Using an ion model that was developed independently of a solvent, i.e., in the crystalline solid, this method improves the water diffusion trends across a range of water models. When used with a good-quality water model, e.g., TIP4P/2005 or E3B, this method recovers the qualitative behaviour of the water diffusion trends. The model and method used were also shown to give good results for other structural and dynamic properties including solution density, radial distribution functions, and ion diffusion coefficients.

Instability Mechanisms of Water-in-Oil Nanoemulsions with Phospholipids: Temporal and Morphological Structures.

PubMed

Sommerling, Jan-Hendrik; de Matos, Maria B C; Hildebrandt, Ellen; Dessy, Alberto; Kok, Robbert Jan; Nirschl, Hermann; Leneweit, Gero

2018-01-16

Many food preparations, pharmaceuticals, and cosmetics use water-in-oil (W/O) emulsions stabilized by phospholipids. Moreover, recent technological developments try to produce liposomes or lipid coated capsules from W/O emulsions, but are faced with colloidal instabilities. To explore these instability mechanisms, emulsification by sonication was applied in three cycles, and the sample stability was studied for 3 h after each cycle. Clearly identifiable temporal structures of instability provide evidence about the emulsion morphology: an initial regime of about 10 min is shown to be governed by coalescence after which Ostwald ripening dominates. Transport via molecular diffusion in Ostwald ripening is commonly based on the mutual solubility of the two phases and is therefore prohibited in emulsions composed of immiscible phases. However, in the case of water in oil emulsified by phospholipids, these form water-loaded reverse micelles in oil, which enable Ostwald ripening despite the low solubility of water in oil, as is shown for squalene. As is proved for the phospholipid dipalmitoylphosphatidylcholine (DPPC), concentrations below the critical aggregation concentration (CAC) form monolayers at the interfaces and smaller droplet sizes. In contrast, phospholipid concentrations above the CAC create complex multilayers at the interface with larger droplet sizes. The key factors for stable W/O emulsions in classical or innovative applications are first, the minimization of the phospholipids' capacity to form reversed micelles, and second, the adaption of the initial phospholipid concentration to the water content to enable an optimized coverage of phospholipids at the interfaces for the intended drop size.

Structurally Stable Attractive Nanoscale Emulsions with Dipole-Dipole Interaction-Driven Interdrop Percolation.

PubMed

Shin, Kyounghee; Gong, Gyeonghyeon; Cuadrado, Jonas; Jeon, Serim; Seo, Mintae; Choi, Hong Sung; Hwang, Jae Sung; Lee, Youngbok; Fernandez-Nieves, Alberto; Kim, Jin Woong

2017-03-28

This study introduces an extremely stable attractive nanoscale emulsion fluid, in which the amphiphilic block copolymer, poly(ethylene oxide)-block-poly(ϵ-caprolactone) (PEO-b-PCL), is tightly packed with lecithin, thereby forming a mechanically robust thin-film at the oil-water interface. The molecular association of PEO-b-PCL with lecithin is critical for formation of a tighter and denser molecular assembly at the interface, which is systematically confirmed by T 2 relaxation and DSC analyses. Moreover, suspension rheology studies also reflect the interdroplet attractions over a wide volume fraction range of the dispersed oil phase; this results in a percolated network of stable drops that exhibit no signs of coalescence or phase separation. This unique rheological behavior is attributed to the dipolar interaction between the phosphorylcholine groups of lecithin and the methoxy end groups of PEO-b-PCL. Finally, the nanoemulsion system significantly enhances transdermal delivery efficiency due to its favorable attraction to the skin, as well as high diffusivity of the nanoscale emulsion drops. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Controlled assembly of organic whispering-gallery-mode microlasers as highly sensitive chemical vapor sensors.

PubMed

Gao, Miaomiao; Wei, Cong; Lin, Xianqing; Liu, Yuan; Hu, Fengqin; Zhao, Yong Sheng

2017-03-09

We demonstrate the fabrication of organic high Q active whispering-gallery-mode (WGM) resonators from π-conjugated polymer by a controlled emulsion-solvent-evaporation method, which can simultaneously provide optical gain and act as an effective resonant cavity. By measuring the shift of their lasing modes on exposure to organic vapor, we successfully monitored the slight concentration variation in the chemical gas. These microlaser sensors demonstrated high detection sensitivity and good signal repeatability under continuous chemical gas treatments. The results offer an effective strategy to design miniaturized optical sensors.

Communication: Contrasting effects of glycerol and DMSO on lipid membrane surface hydration dynamics and forces

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

Schrader, Alex M.; Cheng, Chi-Yuan; Israelachvili, Jacob N.

2016-07-28

Glycerol and dimethyl sulfoxide (DMSO) are commonly used cryoprotectants in cellular systems, but due to the challenges of measuring the properties of surface-bound solvent, fundamental questions remain regarding the concentration, interactions, and conformation of these solutes at lipid membrane surfaces. We measured the surface water diffusivity at gel-phase dipalmitoylphosphatidylcholine (DPPC) bilayer surfaces in aqueous solutions containing ≤7.5 mol. % of DMSO or glycerol using Overhauser dynamic nuclear polarization. We found that glycerol similarly affects the diffusivity of water near the bilayer surface and that in the bulk solution (within 20%), while DMSO substantially increases the diffusivity of surface water relativemore » to bulk water. We compare these measurements of water dynamics with those of equilibrium forces between DPPC bilayers in the same solvent mixtures. DMSO greatly decreases the range and magnitude of the repulsive forces between the bilayers, whereas glycerol increases it. We propose that the differences in hydrogen bonding capability of the two solutes leads DMSO to dehydrate the lipid head groups, while glycerol affects surface hydration only as much as it affects the bulk water properties. The results suggest that the mechanism of the two most common cryoprotectants must be fundamentally different: in the case of DMSO by decoupling the solvent from the lipid surface, and in the case of glycerol by altering the hydrogen bond structure and intermolecular cohesion of the global solvent, as manifested by increased solvent viscosity.« less

A Sensitive Microplate Assay for Lipase Activity Measurement Using Olive Oil Emulsion Substrate: Modification of the Copper Soap Colorimetric Method.

PubMed

Mustafa, Ahmad; Karmali, Amin; Abdelmoez, Wael

2016-01-01

The present work involves a sensitive high-throughput microtiter plate based colorimetric assay for estimating lipase activity using cupric acetate pyridine reagent (CAPR). In the first approach, three factors two levels factorial design methodology was used to evaluate the interactive effect of different parameters on the sensitivity of the assay method. The optimization study revealed that the optimum CAPR concentration was 7.5% w/v, the optimum solvent was heptane and the optimum CAPR pH was 6. In the second approach, the optimized colorimetric microplate assay was used to measure lipase activity based on enzymatic hydrolysis of olive oil emulsion substrate at 37°C and 150 rpm. The emulsion substrates were formulated by using olive oil, triton X-100 (10% v/v in pH 8) and sodium phosphate buffer of pH 8 in ratio of 1:1:1 in the case of Candida sp. lipase. While in the case of immobilized lipozyme RMIM, The emulsion substrates were formulated by using olive oil, triton X-100 (1% v/v in pH 8) and sodium phosphate buffer of pH 8 in ratio of 2:1:1. Absorbance was measured at 655 nm. The stability of this assay (in terms of colored heptane phase absorbance readings) retained more than 92.5% after 24 h at 4°C compared to the absorbance readings measured at zero time. In comparison with other lipase assay methods, beside the developed sensitivity, the reproducibility and the lower limit of detection (LOD) of the proposed method, it permits analyzing of 96 samples at one time in a 96-well microplate. Furthermore, it consumes small quantities of chemicals and unit operations.

Lipid transfer in oil-in-water isasome emulsions: influence of arrested dynamics of the emulsion droplets entrapped in a hydrogel.

PubMed

Iglesias, Guillermo Ramón; Pirolt, Franz; Sadeghpour, Amin; Tomšič, Matija; Glatter, Otto

2013-12-17

The transfer kinetics of lipids between internally self-assembled droplets of O/W emulsions is studied. The droplets (isasomes) consist of various liquid-crystalline phases or W/O microemulsions stabilized by a polymeric stabilizer F127. The various internal phases were identified by the relative peak positions in the small-angle X-ray scattering (SAXS) curves. An arrested system composed of isasomes embedded in a gel matrix actually provides an additional possibility to control these systems in terms of the release of various host molecules. These experiments have been applied to examine the kinetics of the internal phase reorganization imposed by the lipids' release and uptake by the droplets embedded in a κ-carrageenan (KC) hydrogel network. Increasing the concentration of the gelling agent slows down the transfer from one droplet to the other through the aqueous phase. We examined the region where the free diffusion is stopped. i.e., the point where the system changes from the ergodic to the nonergodic state and the kinetics is essentially slowed down. This effect can be balanced by the addition of small amounts of free polymeric stabilizer, which speeds up the kinetics. This is even possible in the case of highly arrested dynamics of the emulsion droplets, as found for the highest KC hydrogel concentrations forming nonergodic systems.

Influence of interfacial slip on the suspension rheology of a dilute emulsion of surfactant-laden deformable drops in linear flows

NASA Astrophysics Data System (ADS)

Das, Sayan; Bhattacharjee, Anirban; Chakraborty, Suman

2018-03-01

The present study deals with the effect of interfacial slip on the deformation and emulsion rheology of a dilute suspension of droplets in a linear flow. The droplets are laden with surfactants that are bulk-insoluble and get transported only along the interface. An asymptotic approach is adopted for the present analysis in order to tackle the nonlinearity present due to deformation of droplets. The analysis is carried out for two different limiting scenarios, namely, surface diffusion-dominated-surfactant transport and surface convection-dominated surfactant transport. For either of the limiting cases, we look into the droplet dynamics for two commonly encountered bulk flows—uniaxial extensional and simple shear flow. Under the assumption of negligible fluid inertia in either phase, it is shown that slip at the droplet interface significantly affects the surfactant-induced Marangoni stress and hence droplet deformation and emulsion rheology. The presence of interfacial slip not only brings about a decrease in the droplet deformation but also reduces the effective viscosity of the emulsion. The fall in both droplet deformation and effective viscosity is found to be more severe for the limiting case of surface convection-dominated surfactant transport. For the case of an imposed simple shear flow, the normal stress differences generated due to droplet deformation are affected as well due to the presence of interfacial slip.

Hypersensitivity to total parenteral nutrition fat-emulsion component in an egg-allergic child.

PubMed

Lunn, Michael; Fausnight, Tracy

2011-10-01

Immunoglobulin E (IgE)-mediated food allergies affect 6% to 8% of children in the United States with symptoms ranging from localized hives to life-threatening anaphylaxis. Intravenous fat emulsions (IFEs) are a vital component of total parental nutrition, because they provide essential fatty acids. IFE is a sterile fat emulsion that contains egg-yolk phospholipids. Although egg allergy is listed as a contraindication, adverse reactions are uncommon. We report here the case of a hypersensitivity to IFE in a 2-year-old patient with previously undocumented egg allergy. Our patient was placed on total parental nutrition and a 20% IFE postoperatively and developed diffuse pruritus 14 days after initiation of therapy. She showed transient improvement with intravenous antihistamine, but her symptoms did not resolve until the IFE was stopped. On the basis of clinical history, including aversion to egg, we performed skin-prick testing, the results of which were positive for egg white allergy. Serum testing confirmed allergy to both egg yolk and egg white. To our knowledge, this is the first reported case of a pediatric patient with a history suggestive of egg allergy, positive skin-prick and serum testing to egg, and reaction to IFE infusion. Although ingestion of egg lecithin in cooked food is generally tolerated by egg-allergic people, administration of intravenous egg-containing lipid emulsions may cause significant adverse reactions.

Electrochemical synthesis of copper nanoparticles using cuprous oxide as a precursor in choline chloride-urea deep eutectic solvent: nucleation and growth mechanism.

PubMed

Zhang, Q B; Hua, Y X

2014-12-28

The electrochemical nucleation and growth kinetics of copper nanoparticles on a Ni electrode have been studied with cyclic voltammetry and chronoamperometry in the choline chloride (ChCl)-urea based deep eutectic solvent (DES). The copper source was introduced into the solvent by the dissolution of Cu(I) oxide (Cu2O). Cyclic voltammetry indicates that the electroreduction of Cu(I) species in the DES is a diffusion-controlled quasi-reversible process. The analysis of the chronoamperometric transient behavior during electrodeposition suggests that the deposition of copper on the Ni electrode at low temperatures follows a progressive nucleation and three-dimensional growth controlled by diffusion. The effect of temperature on the diffusion coefficient of Cu(I) species that is present in the solvent and electron transfer rate constant obeys the Arrhenius law, according to which the activation energies are estimated to be 49.20 and 21.72 kJ mol(-1), respectively. The initial stage of morphological study demonstrates that both electrode potential and temperature play important roles in controlling the nucleation and growth kinetics of the nanocrystals during the electrodeposition process. Electrode potential is observed to affect mainly the nucleation process, whereas temperature makes a major contribution to the growth process.

Nanoparticle and Gelation Stabilized Functional Composites of an Ionic Salt in a Hydrophobic Polymer Matrix

PubMed Central

Kanyas, Selin; Aydın, Derya; Kizilel, Riza; Demirel, A. Levent; Kizilel, Seda

2014-01-01

Polymer composites consisted of small hydrophilic pockets homogeneously dispersed in a hydrophobic polymer matrix are important in many applications where controlled release of the functional agent from the hydrophilic phase is needed. As an example, a release of biomolecules or drugs from therapeutic formulations or release of salt in anti-icing application can be mentioned. Here, we report a method for preparation of such a composite material consisted of small KCOOH salt pockets distributed in the styrene-butadiene-styrene (SBS) polymer matrix and demonstrate its effectiveness in anti-icing coatings. The mixtures of the aqueous KCOOH and SBS-cyclohexane solutions were firstly stabilized by adding silica nanoparticles to the emulsions and, even more, by gelation of the aqueous phase by agarose. The emulsions were observed in optical microscope to check its stability in time and characterized by rheological measurements. The dry composite materials were obtained via casting the emulsions onto the glass substrates and evaporations of the organic solvent. Composite polymer films were characterized by water contact angle (WCA) measurements. The release of KCOOH salt into water and the freezing delay experiments of water droplets on dry composite films demonstrated their anti-icing properties. It has been concluded that hydrophobic and thermoplastic SBS polymer allows incorporation of the hydrophilic pockets/phases through our technique that opens the possibility for controlled delivering of anti-icing agents from the composite. PMID:24516593

Novel formulations of taxanes: a review. Old wine in a new bottle?

PubMed

Hennenfent, K L; Govindan, R

2006-05-01

Over the past two decades, the taxanes have played a significant role in the treatment of various malignancies. However, the poor solubility of these compounds necessitates the inclusion of surfactant vehicles in their commercial formulations. Cremophor EL and polysorbate 80 have long comprised the standard solvent system for paclitaxel and docetaxel, respectively. A number of pharmacologic and biologic effects related to both of these drug formulations have been described, including clinically relevant acute hypersensitivity reactions and peripheral neuropathy. In addition, these solvents affect the disposition of intravenously administered solubilized drugs and leach plasticizers from polyvinylchloride infusion sets. A number of strategies to develop formulations of surfactant-free taxanes have been developed. They include albumin nanoparticles, polyglutamates, taxane analogs and prodrugs, emulsions, and lipsomes. An overview of these novel formulations of taxanes, their mechanisms of action, pharmacokinetics, dose and administration, adverse effects, and clinical efficacy will be discussed.

Multifunctional nanocomposite hollow fiber membranes by solvent transfer induced phase separation.

PubMed

Haase, Martin F; Jeon, Harim; Hough, Noah; Kim, Jong Hak; Stebe, Kathleen J; Lee, Daeyeon

2017-11-01

The decoration of porous membranes with a dense layer of nanoparticles imparts useful functionality and can enhance membrane separation and anti-fouling properties. However, manufacturing of nanoparticle-coated membranes requires multiple steps and tedious processing. Here, we introduce a facile single-step method in which bicontinuous interfacially jammed emulsions are used to form nanoparticle-functionalized hollow fiber membranes. The resulting nanocomposite membranes prepared via solvent transfer-induced phase separation and photopolymerization have exceptionally high nanoparticle loadings (up to 50 wt% silica nanoparticles) and feature densely packed nanoparticles uniformly distributed over the entire membrane surfaces. These structurally well-defined, asymmetric membranes facilitate control over membrane flux and selectivity, enable the formation of stimuli responsive hydrogel nanocomposite membranes, and can be easily modified to introduce antifouling features. This approach forms a foundation for the formation of advanced nanocomposite membranes comprising diverse building blocks with potential applications in water treatment, industrial separations and as catalytic membrane reactors.

Particle Formation and Product Formulation Using Supercritical Fluids.

PubMed

Knez, Željko; Knez Hrnčič, Maša; Škerget, Mojca

2015-01-01

Traditional methods for solids processing involve either high temperatures, necessary for melting or viscosity reduction, or hazardous organic solvents. Owing to the negative impact of the solvents on the environment, especially on living organisms, intensive research has focused on new, sustainable methods for the processing of these substances. Applying supercritical fluids for particle formation may produce powders and composites with special characteristics. Several processes for formation and design of solid particles using dense gases have been studied intensively. The unique thermodynamic and fluid-dynamic properties of supercritical fluids can be used also for impregnation of solid particles or for the formation of solid powderous emulsions and particle coating, e.g., for formation of solids with unique properties for use in different applications. We give an overview of the application of sub- and supercritical fluids as green processing media for particle formation processes and present recent advances and trends in development.

Thermal diffusivity measurement for urchin-like gold nanofluids with different solvents, sizes and concentrations/shapes.

PubMed

López-Muñoz, Gerardo A; Balderas-López, José Abraham; Ortega-Lopez, Jaime; Pescador-Rojas, José A; Salazar, Jaime Santoyo

2012-12-06

The thermal properties of nanofluids are an especially interesting research topic because of the variety of potential applications, which range from bio-utilities to next-generation heat-transfer fluids. In this study, photopyroelectric calorimetry for measuring the thermal diffusivity of urchin-like colloidal gold nanofluids as a function of particle size, concentration and shape in water, ethanol and ethylene glycol is reported. Urchin-like gold nanoparticles were synthesised in the presence of hydroquinone through seed-mediated growth with homogeneous shape and size ranging from 55 to 115 nm. The optical response, size and morphology of these nanoparticles were characterised using UV-visible spectroscopy and transmission electron microscopy. The thermal diffusivity of these nanofluids decreased as the size of the nanoparticles increased, and the enhancement depended on the thermal diffusivity of the solvent. The opposite effect (increase in thermal diffusivity) was observed when the nanoparticle concentration was increased. These effects were more evident for urchin-like gold nanofluids than for the corresponding spherical gold nanofluids.

Synthesis of size controllable cu-phthalocyanine nanofibers by simple solvent diffusion method and their electrochemical properties.

PubMed

Gao, Junshan; Cheng, Chuanwei; Zhou, Xuechao; Li, Yingying; Xu, Xiaoqi; Du, Xiguang; Zhang, Haiqian

2010-02-15

Tetra (2-isopropyl-5-methylphenoxy) substituted Cu-phthalocyanine nanofibers were obtained in large scale by a simple solvent diffusion method. The sizes of the fibers can be finely tuned under different solvent temperature. FE-SEM micrographs indicate that the length of the fibers changed from several hundreds micrometers to several hundreds nanometers and the width changed from several micrometers to several decade nanometers. XRD measurement showed a highly long-range ordered lamellar arrangement of the substituted Cu-phthalocyanine molecules in the microfiber and the UV-vis absorption spectrum of the fibers indicated an H-aggregate of the phthalocyanine molecules. The CV curves elucidate the CuPc fibers can be fabricated Faraday pseudocapacitor. Crown Copyright 2009. Published by Elsevier Inc. All rights reserved.

Biodiesel production from ethanolysis of DPO using deep eutectic solvent (DES) based choline chloride - ethylene glycol as co-solvent

NASA Astrophysics Data System (ADS)

Taslim, Indra, Leonardo; Manurung, Renita; Winarta, Agus; Ramadhani, Debbie Aditia

2017-03-01

Biodiesel is usually produced from transesterification using methanol or ethanol as alcohol. However, biodiesel produced using methanol has several disadvantages because methanol is toxic and not entirely bio-based as it is generally produced from petroleum, natural gas and coal. On the other hand, ethanol also has several disadvantages such as lower reactivity in transesterification process and formation of stable emulsion between ester and glycerol. To improve ethanolysis process, deep eutectic solvent (DES) was prepared from choline chloride and ethylene glycol to be used as co-solvent in ethanolysis. Deep eutectic solvent was prepared by mixing choline chloride and ethylene glycol at molar ratio of 1:2, temperature of 80 °C, and stirring speed of 300 rpm for 1 hour. The DES was characterized by its density and viscosity. The ethanolysis of DPO / Degummed Palm Oil was performed at 70 °C, ethanol to oil molar ratio of 9:1, catalyst (potassium hydroxide) concentration of 0.75 wt.% concentration, co-solvent (DES) concentration of 1, 2, 3, 4, 5 and 6 wt.%, stirring speed of 600 rpm, and reaction time of 1 hour. The obtained biodiesel was then characterized by its density, viscosity and ester content. The oil - ethanol phase condition was observed in reaction tube. The oil - ethanol phase with DES tends to form meniscus compared to that without DES. Which implied that oil and ethanol become more slightly miscible, which favours the reaction. Using DES as co-solvent in ethanolysis resulted in an increase in yield and easier purification. The esters properties met the international standards ASTM D6751, with highest yield achieved at 81.72 % with 99.35 % ethyl ester contents at 4% DES concentration.

Tuning crystalline ordering by annealing and additives to study its effect on exciton diffusion in a polyalkylthiophene copolymer.

PubMed

Chowdhury, Mithun; Sajjad, Muhammad T; Savikhin, Victoria; Hergué, Noémie; Sutija, Karina B; Oosterhout, Stefan D; Toney, Michael F; Dubois, Philippe; Ruseckas, Arvydas; Samuel, Ifor D W

2017-05-17

The influence of various processing conditions on the singlet exciton diffusion is explored in films of a conjugated random copolymer poly-(3-hexylthiophene-co-3-dodecylthiophene) (P3HT-co-P3DDT) and correlated with the degree of crystallinity probed by grazing incidence X-ray scattering and with exciton bandwidth determined from absorption spectra. The exciton diffusion coefficient is deduced from exciton-exciton annihilation measurements and is found to increase by more than a factor of three when thin films are annealed using CS 2 solvent vapour. A doubling of exciton diffusion coefficient is observed upon melt annealing at 200 °C and the corresponding films show about 50% enhancement in the degree of crystallinity. In contrast, films fabricated from polymer solutions containing a small amount of either solvent additive or nucleating agent show a decrease in exciton diffusion coefficient possibly due to formation of traps for excitons. Our results suggest that the enhancement of exciton diffusivity occurs because of increased crystallinity of alkyl-stacking and longer conjugation of aggregated chains which reduces the exciton bandwidth.

Conformational dynamics of a crystalline protein from microsecond-scale molecular dynamics simulations and diffuse X-ray scattering.

PubMed

Wall, Michael E; Van Benschoten, Andrew H; Sauter, Nicholas K; Adams, Paul D; Fraser, James S; Terwilliger, Thomas C

2014-12-16

X-ray diffraction from protein crystals includes both sharply peaked Bragg reflections and diffuse intensity between the peaks. The information in Bragg scattering is limited to what is available in the mean electron density. The diffuse scattering arises from correlations in the electron density variations and therefore contains information about collective motions in proteins. Previous studies using molecular-dynamics (MD) simulations to model diffuse scattering have been hindered by insufficient sampling of the conformational ensemble. To overcome this issue, we have performed a 1.1-μs MD simulation of crystalline staphylococcal nuclease, providing 100-fold more sampling than previous studies. This simulation enables reproducible calculations of the diffuse intensity and predicts functionally important motions, including transitions among at least eight metastable states with different active-site geometries. The total diffuse intensity calculated using the MD model is highly correlated with the experimental data. In particular, there is excellent agreement for the isotropic component of the diffuse intensity, and substantial but weaker agreement for the anisotropic component. Decomposition of the MD model into protein and solvent components indicates that protein-solvent interactions contribute substantially to the overall diffuse intensity. We conclude that diffuse scattering can be used to validate predictions from MD simulations and can provide information to improve MD models of protein motions.

Influence of the Oil Phase and Topical Formulation on the Wound Healing Ability of a Birch Bark Dry Extract

PubMed Central

Steinbrenner, Isabel; Houdek, Pia; Pollok, Simone; Brandner, Johanna M.; Daniels, Rolf

2016-01-01

Triterpenes from the outer bark of birch are known for various pharmacological effects including enhanced wound healing (WH). A birch bark dry extract (TE) obtained by accelerated solvent extraction showed the ability to form oleogels when it is suspended in oils. Consistency of the oleogels and the dissolved amount of triterpenes varies largely with the used oil. Here we wanted to know to what extent different oils and formulations (oleogel versus o/w emulsion) influence WH. Looking at the plain oils, medium-chain triglycerides (MCT) enhanced WH (ca. 1.4-fold), while e.g. castor oil (ca.0.3-fold) or light liquid paraffin (LLP; ca. 0.5-fold) significantly decreased WH. Concerning the respective oleogels, TE-MCT showed no improvement although the solubility of the TE was high. In contrast, the oleogel of sunflower oil which alone showed a slight tendency to impair WH, enhanced WH significantly (ca. 1.6-fold). These results can be explained by release experiments where the release rate of betulin, the main component of TE, from MCT oleogels was significantly lower than from sunflower oil oleogels. LLP impaired WH as plain oil and even though it released betulin comparable to sunflower oil it still results in an overall negative effect of the oleogel on WH. As a further formulation option also surfactant free o/w emulsions were prepared using MCT, sunflower oil and LLP as a nonpolar oil phase. Depending on the preparation method (suspension or oleogel method) the distribution of the TE varied markedly and affected also release kinetics. However, the released betulin was clearly below the values measured with the respective oleogels. Consequently, none of the emulsions showed a significantly positive effect on WH. In conclusion, our data show that the oil used as a vehicle influences wound healing not only by affecting the release of the extract, but also by having its own vehicle effect on wound healing. This is also of importance for other applications where drugs have to be applied in non-polar vehicles because these solvents likely influence the outcome of the experiment substantially. PMID:27219110

Encapsulation and release of the hypnotic agent zolpidem from biodegradable polymer microparticles containing hydroxypropyl-beta-cyclodextrin.

PubMed

Trapani, Giuseppe; Lopedota, Angela; Boghetich, Giancarlo; Latrofa, Andrea; Franco, Massimo; Sanna, Enrico; Liso, Gaetano

2003-12-11

The goal of this study was to design a prolonged release system of the hypnotic agent zolpidem (ZP) useful for the treatment of insomnia. In this work, ZP alone or in the presence of HP-beta-CD was encapsulated in microparticles constituted by poly(DL-lactide) (PDLLA) and poly(DL-lactide-co-glycolide) (PLGA) and the drug release from these systems was evaluated. ZP alone-loaded microparticles were prepared by the classical O/W emulsion-solvent evaporation method. Conversely, ZP/HP-beta-CD containing microparticles were prepared by the W/O/W emulsion-solvent evaporation method following two different procedures (i.e. A and B). Following procedure A, the previously produced ZP/HP-beta-CD solid complex was added to the water phase of primary emulsion. In the procedure B, HP-beta-CD was added to the aqueous phase and ZP to the organic phase. The resulting microparticles were characterized about morphology, size, encapsulation efficiency and release rates. FT-IR, X-ray, and DSC results suggest the drug is in an essentially amorphous state within the microparticles. The release profiles of ZP from microparticles were in general biphasic, being characterized by an initial burst effect and a subsequent slow ZP release. It resulted that co-encapsulating ZP with or without HP-beta-CD in PDLLA and PLGA the drug release from the corresponding microparticles was protracted. Moreover, in a preliminary pharmacological screening, the ataxic activity in rats was investigated and it was found that intragastric administration of the ZP/HP-beta-CD/PLGA microparticles prepared according to procedure B produced the same ataxic induction time as the one induced by the currently used formulation Stilnox. Interestingly moreover, there was a longer ataxic lasting and a lower intensity of ataxia produced by the ZP/HP-beta-CD/PLGA-B-formulation already after 60 min following the administration. However, a need for further pharmacokinetic and pharmacodynamic studies resulted to fully evaluate the utility of this last formulation for the sustained delivery of ZP.

Tuning aggregation of microemulsion droplets and silica nanoparticles using solvent mixtures.

PubMed

Salabat, Alireza; Eastoe, Julian; Mutch, Kevin J; Tabor, Rico F

2008-02-15

The effect of solvent on stability of water-in-oil microemulsions has been studied with AOT (sodium bis(2-ethylhexyl)sulfosuccinate) and different solvent mixtures of n-heptane, toluene and dodecane. Dynamic light scattering DLS was used to monitor the apparent diffusion coefficient D(A) and effective microemulsion droplet diameter on changing composition of the solvent. Interdroplet attractive interactions, as indicated by variations in D(A), can be tuned by formulation of appropriate solvent mixtures using heptane, toluene, and dodecane. In extreme cases, solvent mixtures can be used to induce phase transitions in the microemulsions. Aggregation and stability of model AOT-stabilized silica nanoparticles in different solvents were also investigated to explore further these solvent effects. For both systems the state of aggregation can be correlated with the effective molecular volume of the solvent V(mol)(eff) mixture.

Non-destructive testing method for determining the solvent diffusion coefficient in the porous materials products

NASA Astrophysics Data System (ADS)

Belyaev, V. P.; Mishchenko, S. V.; Belyaev, P. S.

2018-01-01

Ensuring non-destructive testing of products in industry is an urgent task. Most of the modern methods for determining the diffusion coefficient in porous materials have been developed for bodies of a given configuration and size. This leads to the need for finished products destruction to make experimental samples from them. The purpose of this study is the development of a dynamic method that allows operatively determine the diffusion coefficient in finished products from porous materials without destroying them. The method is designed to investigate the solvents diffusion coefficient in building constructions from materials having a porous structure: brick, concrete and aerated concrete, gypsum, cement, gypsum or silicate solutions, gas silicate blocks, heat insulators, etc. A mathematical model of the method is constructed. The influence of the design and measuring device operating parameters on the method accuracy is studied. The application results of the developed method for structural porous products are presented.

Molecular dynamics of acetamide based ionic deep eutectic solvents

NASA Astrophysics Data System (ADS)

Srinivasan, H.; Dubey, P. S.; Sharma, V. K.; Biswas, R.; Mitra, S.; Mukhopadhyay, R.

2018-04-01

Deep eutectic solvents are multi-component mixtures that have freezing point lower than their individual components. Mixture of acetamide+ lithium nitrate in the molar ratio 78:22 and acetamide+ lithium perchlorate in the molar ratio 81:19 are found to form deep eutectic solvents with melting point lower than the room temperature. It is known that the depression in freezing point is due to the hydrogen bond breaking ability of anions in the system. Quasielastic neutron scattering experiments on these systems were carried out to study the dynamics of acetamide molecules which may be influenced by this hydrogen bond breaking phenomena. The motion of acetamide molecules is modeled using jump diffusion mechanism to demonstrate continuous breaking and reforming hydrogen bonds in the solvent. Using the jump diffusion model, it is inferred that the jump lengths of acetamide molecules are better approximated by a Gaussian distribution. The shorter residence time of acetamide in presence of perchlorate ions suggest that the perchlorate ions have a higher hydrogen bond breaking ability compared to nitrate ions.

Dispersed phase volume fraction, weak acids and Tween 80 in a model emulsion: Effect on the germination and growth of Bacillus weihenstephanensis KBAB4 spores.

PubMed

Léonard-Akkari, Lucie; Guégan, Stéphanie; Courand, Fabienne; Couvert, Olivier; Lepage, Jean-François; Rondeau-Mouro, Corinne; Desriac, Noémie; Mathot, Anne-Gabrielle; Leguérinel, Ivan; Coroller, Louis; Decourcelle, Nicolas

2018-07-01

In foodstuffs, physico-chemical interactions and/or physical constraints between spores, inhibitors and food components may exist. Thus, the objective of this study was to investigate such interactions using a model emulsion as a microbial medium in order to improve bacterial spore control with better knowledge of the interactions in the formulation. Emulsions were prepared with hexadecane mixed with nutrient broth using sonication and were stabilized by Tween 80 and Span 80. The hexadecane ratio was either 35% (v/v) or 50% (v/v) and each emulsion was studied in the presence of organic acid (acetic, lactic or hexanoic) at two pH levels (5.5 and 6). Self-diffusion coefficients of emulsion components and the organic acids were measured by Pulsed Field Gradient-Nuclear Magnetic Resonance (PFG-NMR). The inhibition effect on the spore germination and cell growth of Bacillus weihenstephanensis KBAB4 was characterized by the measure of the probability of growth using the most probable number methodology, and the measure of the time taken for the cells to germinate and grow using a single cell Bioscreen® method and using flow cytometry. The inhibition of spore germination and growth in the model emulsion depended on the dispersed phase volume fraction and the pH value. The effect of the dispersed phase volume fraction was due to a combination of (i) the lipophilicity of the biocide, hexanoic acid, that may have had an impact on the distribution of organic acid between hexadecane and the aqueous phases and (ii) the antimicrobial activity of the emulsifier Tween 80 detected at the acidic pH value. The interface phenomena seemed to have a major influence. Future work will focus on the exploration of these phenomena at the interface. Copyright © 2018 Elsevier Ltd. All rights reserved.

Methotrexate loaded alginate microparticles and effect of Ca2+ post-crosslinking: An in vitro physicochemical and biological evaluation.

PubMed

Dhanka, Mukesh; Shetty, Chaitra; Srivastava, Rohit

2018-04-15

Methotrexate (MTX) loaded alginate microparticles were produced by simple water-in-oil (W/O) emulsion solvent diffusion method with homogenization and then subsequently cross-linked by Ca 2+ . The mean sizes of developed microparticles (bare non-crosslinked, crosslinked, drug-loaded non-crosslinked, and drug-loaded cross-linked) were found to be <11μm. The morphology of bare non-crosslinked and crosslinked microparticles were observed to be spherical with smooth surface morphology. However, MTX loaded non-crosslinked and crosslinked microparticles were found to have an irregular shape with rough surface morphology. The encapsulation efficiency (% EE) and loading capacity (% LC) of MTX loaded non-crosslinked microparticles were estimated to be 92.19±1.85 and 9.35±0.22, respectively. However, in case of cross-linked microparticles, the % EE and % LC values slightly decreased, i.e., 83.26±1.69% and 8.44±0.21%, respectively. Crosslinked microparticles were found to release MTX at a slower rate as compared to non-crosslinked microparticles. The physicochemical characterizations of microparticles by Fourier Transform Infrared Spectroscopy and High-Resolution X-Ray Diffraction have shown that drug encapsulated in the microparticles without chemical interactions has lost its crystalline nature. The biocompatibility and hemocompatibility studies of the microparticles have demonstrated that microparticles are biocompatible and were non-hemolytic at low concentrations. Copyright © 2017 Elsevier B.V. All rights reserved.

Bioadhesive floating microsponges of cinnarizine as novel gastroretentive delivery: Capmul GMO bioadhesive coating versus acconon MC 8-2 EP/NF with intrinsic bioadhesive property

PubMed Central

Raghuvanshi, Smita; Pathak, Kamla

2016-01-01

Introduction: The study was aimed at the development of low-density gastroretentive bioadhesive microsponges of cinnarizine by two-pronged approach (i) coating with bioadhesive material and (ii) exploration of acconon MC 8-2 EP/NF as bioadhesive raw material for fabrication. Materials and Methods: Microsponges were prepared by quasi-emulsion solvent diffusion method using 32 factorial design. Capmul GMO was employed for bioadhesive coating. In parallel, potential of acconon for the fabrication of bioadhesive floating microsponges (A8) was assessed. Results: Formulation with entrapment efficiency = 82.4 ± 3.4%, buoyancy = 82.3 ± 2.5%, and correlation of drug release (CDR8h) = 88.7% ± 2.9% was selected as optimized formulation (F8) and subjected to bioadhesive coating (BF8). The %CDR8h for A8 was similar to BF8 (87.2% ± 3.5%). Dynamic in vitro bioadhesion test revealed comparable bioadhesivity with BF8. The ex vivo permeation across gastric mucin displayed 63.16% for BF8 against 56.74% from A8; affirmed the bioadhesivity of both approaches. Conclusion: The study concluded with the development of novel bioadhesive floating microsponges of cinnarizine employing capmul GMO as bioadhesive coating material and confirmed the viability of acconon MC 8-2EP/NF as bioadhesive raw material for sustained targeted delivery of drug. PMID:28123987

Preparation and properties of BSA-loaded microspheres based on multi-(amino acid) copolymer for protein delivery

PubMed Central

Chen, Xingtao; Lv, Guoyu; Zhang, Jue; Tang, Songchao; Yan, Yonggang; Wu, Zhaoying; Su, Jiacan; Wei, Jie

2014-01-01

A multi-(amino acid) copolymer (MAC) based on ω-aminocaproic acid, γ-aminobutyric acid, L-alanine, L-lysine, L-glutamate, and hydroxyproline was synthetized, and MAC microspheres encapsulating bovine serum albumin (BSA) were prepared by a double-emulsion solvent extraction method. The experimental results show that various preparation parameters including surfactant ratio of Tween 80 to Span 80, surfactant concentration, benzyl alcohol in the external water phase, and polymer concentration had obvious effects on the particle size, morphology, and encapsulation efficiency of the BSA-loaded microspheres. The sizes of BSA-loaded microspheres ranged from 60.2 μm to 79.7 μm, showing different degrees of porous structure. The encapsulation efficiency of BSA-loaded microspheres also ranged from 38.8% to 50.8%. BSA release from microspheres showed the classic biphasic profile, which was governed by diffusion and polymer erosion. The initial burst release of BSA from microspheres at the first week followed by constant slow release for the next 7 weeks were observed. BSA-loaded microspheres could degrade gradually in phosphate buffered saline buffer with pH value maintained at around 7.1 during 8 weeks incubation, suggesting that microsphere degradation did not cause a dramatic pH drop in phosphate buffered saline buffer because no acidic degradation products were released from the microspheres. Therefore, the MAC microspheres might have great potential as carriers for protein delivery. PMID:24855351

Preparation of polyamide nanocapsules of Aloe vera L. delivery with in vivo studies.

PubMed

Esmaeili, Akbar; Ebrahimzadeh, Maryam

2015-04-01

Aloe vera is the oldest medicinal plant ever known and the most applied medicinal plant worldwide. The purpose of this study was to prepare polyamide nanocapsules containing A. vera L. by an emulsion diffusion technique with in vivo studies. Diethyletriamine (DETA) was used as the encapsulating polymer with acetone ethyl acetate and dimethyl sulfoxide (DMSO) as the organic solvents and Tween and gelatin in water as the stabilizers. Sebacoyl chloride (SC) monomer, A. vera L. extract, and olive oil were mixed with the acetone and then water containing DETA monomer was added to the solution using a magnetic stirrer. Finally, the acetone was removed under vacuum, and nanocapsules were obtained using a freeze drier. This study showed that the size of the nanocapsule depends on a variety of factors such as the ratio of polymer to oil, the concentration of polymers, and the plant extract. The first sample is without surfactant and the size of nanocapsules in the sample is 115 nm. By adding surfactant, nanocapsules size was reduced to 96 nm. Nanocapsules containing A. vera were administered to rats and the effects were compared with a normal control group. The results showed that in the A. vera group, the effect is higher. The nanocapsules were identified by scanning electron microscopy (SEM), zeta potential sizer (ZPS), and Fourier-transform infrared spectroscopy (FT-IR).

Ionic complexation as a non-covalent approach for the design of folate anchored rifampicin Gantrez nanoparticles.

PubMed

Date, Praveen V; Patel, Mitesh D; Majee, Sharmila B; Samad, Abdul; Devarajan, Padma V

2013-05-01

The present study discloses the design of folate anchored Rifampicin-Poly methylvinylether maleic anhydride copolymer (Gantrez AN-119, Gantrez) nanoparticles (RFMGzFa) by ionic complexation. Folic acid was anchored to the preformed drug loaded nanoparticles. Folic acid was anchored in different concentration by simply varying the amount of folic acid added during preparation. RFMGzFa nanoparticles were prepared by emulsion solvent diffusion method. Gantrez AN-119 rapidly hydrolyzes in aqueous medium releasing carboxylic acid groups, to create an acidic environment. This facilitates protonation and subsequent ionic complexation of folic acid with the carboxylic groups, to enable anchoring. FTIR spectra confirmed this interaction. Infrared imaging revealed distribution of folic acid across the nanoparticle surface. Nanoparticles were obtained in the size range 350-450 nm with RFM loading of 12-14% w/w. Zeta potential confirmed colloidal stability. TEM/SEM revealed spherical morphology. RFMGzFa nanoparticles exhibited sustained release of RFM and folic acid. Folic acid showed sustained release upto 12 h, which was ion exchange mediated. A 480% enhancement in RFM uptake with RFMGzFa nanoparticles compared to 300% with RFMGz nanoparticles in-vitro, in human macrophage cell line U-937, suggested the role of folic acid in folate receptor mediated uptake. Ionic complexation represents a simple non-covalent approach for anchoring folic acid on polymeric nanoparticles of Gantrez.

Bioadhesive floating microsponges of cinnarizine as novel gastroretentive delivery: Capmul GMO bioadhesive coating versus acconon MC 8-2 EP/NF with intrinsic bioadhesive property.

PubMed

Raghuvanshi, Smita; Pathak, Kamla

2016-01-01

The study was aimed at the development of low-density gastroretentive bioadhesive microsponges of cinnarizine by two-pronged approach (i) coating with bioadhesive material and (ii) exploration of acconon MC 8-2 EP/NF as bioadhesive raw material for fabrication. Microsponges were prepared by quasi-emulsion solvent diffusion method using 3 2 factorial design. Capmul GMO was employed for bioadhesive coating. In parallel, potential of acconon for the fabrication of bioadhesive floating microsponges (A8) was assessed. Formulation with entrapment efficiency = 82.4 ± 3.4%, buoyancy = 82.3 ± 2.5%, and correlation of drug release (CDR 8h ) = 88.7% ± 2.9% was selected as optimized formulation (F8) and subjected to bioadhesive coating (BF8). The %CDR 8h for A8 was similar to BF8 (87.2% ± 3.5%). Dynamic in vitro bioadhesion test revealed comparable bioadhesivity with BF8. The ex vivo permeation across gastric mucin displayed 63.16% for BF8 against 56.74% from A8; affirmed the bioadhesivity of both approaches. The study concluded with the development of novel bioadhesive floating microsponges of cinnarizine employing capmul GMO as bioadhesive coating material and confirmed the viability of acconon MC 8-2EP/NF as bioadhesive raw material for sustained targeted delivery of drug.

Absorption of ethanol, acetone, benzene and 1,2-dichloroethane through human skin in vitro: a test of diffusion model predictions.

PubMed

Gajjar, Rachna M; Kasting, Gerald B

2014-11-15

The overall goal of this research was to further develop and improve an existing skin diffusion model by experimentally confirming the predicted absorption rates of topically-applied volatile organic compounds (VOCs) based on their physicochemical properties, the skin surface temperature, and the wind velocity. In vitro human skin permeation of two hydrophilic solvents (acetone and ethanol) and two lipophilic solvents (benzene and 1,2-dichloroethane) was studied in Franz cells placed in a fume hood. Four doses of each (14)C-radiolabed compound were tested - 5, 10, 20, and 40μLcm(-2), corresponding to specific doses ranging in mass from 5.0 to 63mgcm(-2). The maximum percentage of radiolabel absorbed into the receptor solutions for all test conditions was 0.3%. Although the absolute absorption of each solvent increased with dose, percentage absorption decreased. This decrease was consistent with the concept of a stratum corneum deposition region, which traps small amounts of solvent in the upper skin layers, decreasing the evaporation rate. The diffusion model satisfactorily described the cumulative absorption of ethanol; however, values for the other VOCs were underpredicted in a manner related to their ability to disrupt or solubilize skin lipids. In order to more closely describe the permeation data, significant increases in the stratum corneum/water partition coefficients, Ksc, and modest changes to the diffusion coefficients, Dsc, were required. The analysis provided strong evidence for both skin swelling and barrier disruption by VOCs, even by the minute amounts absorbed under these in vitro test conditions. Copyright © 2014 Elsevier Inc. All rights reserved.

Tracer diffusion in active suspensions

NASA Astrophysics Data System (ADS)

Burkholder, Eric W.; Brady, John F.

2017-05-01

We study the diffusion of a Brownian probe particle of size R in a dilute dispersion of active Brownian particles of size a , characteristic swim speed U0, reorientation time τR, and mechanical energy ksTs=ζaU02τR/6 , where ζa is the Stokes drag coefficient of a swimmer. The probe has a thermal diffusivity DP=kBT /ζP , where kBT is the thermal energy of the solvent and ζP is the Stokes drag coefficient for the probe. When the swimmers are inactive, collisions between the probe and the swimmers sterically hinder the probe's diffusive motion. In competition with this steric hindrance is an enhancement driven by the activity of the swimmers. The strength of swimming relative to thermal diffusion is set by Pes=U0a /DP . The active contribution to the diffusivity scales as Pes2 for weak swimming and Pes for strong swimming, but the transition between these two regimes is nonmonotonic. When fluctuations in the probe motion decay on the time scale τR, the active diffusivity scales as ksTs/ζP : the probe moves as if it were immersed in a solvent with energy ksTs rather than kBT .

Experimental and theoretical aspects of studying themodynamics and mass transport in polymer-solvent systems

NASA Astrophysics Data System (ADS)

Davis, Peter Kennedy

Mass transport and thermodynamics in polymer-solvent systems are two key areas of importance to the polymer industry. Numerous processes including polymerization reactors, membrane separations, foam production, devolatilization processes, film and coating drying, supercritical extractions, drug delivery, and even nano-technology require fundamental phase equilibria and diffusion information. Although such information is vital in equipment design and optimization, acquisition and modeling of these data are still in the research and development stages. This thesis is rather diverse as it addresses many realms of this broad research area. From high pressure to low pressure, experimental to theoretical, and infinite dilution to finite concentration, the thesis covers a wide range of topics that are of current importance to the industrial and academic polymer community. Chapter 1 discusses advances in the development of a new volumetric sorption pressure decay technique to make phase equilibrium and diffusion measurements in severe temperature-pressure environments. Chapter 2 provides the derivations and results of a new completely predictive Group Contribution Lattice Fluid Equation of State for multi-component polymer-solvent systems. The remaining four chapters demonstrate advances in the modeling of inverse gas chromatography (IGC) experiments. IGC has been used extensively of the last 50 years to make low pressure sorption and diffusion measurements at infinitely dilute and finite solvent concentrations. Chapter 3 proposes a new IGC experiment capable of obtaining ternary vapor-liquid equilibria in polymer-solvent-solvent systems. Also in that chapter, an extensive derivation is provided for a continuum model capable of describing the results of such an experiment. Chapter 4 presents new data collected on a packed column IGC experiment and a new model that can be used with those experimental data to obtain diffusion and partition coefficients. Chapter 5 addresses a rather controversial topic about IGC experiments near the polymer glass transition temperature. Using a new IGC model capable of describing both bulk absorption and surface adsorption, IGC behavior around the glass transition was able to be better understood. Finally, Chapter 6 presents an IGC model that can be used to separate bulk effects from surface effects in capillary column IGC experiments.

Development and characterization of PLGA nanoparticles as delivery systems of a prodrug of zidovudine obtained by its conjugation with ursodeoxycholic acid.

PubMed

Dalpiaz, Alessandro; Contado, Catia; Mari, Lara; Perrone, Daniela; Pavan, Barbara; Paganetto, Guglielmo; Hanuskovà, Miriam; Vighi, Eleonora; Leo, Eliana

2014-05-01

Zidovudine (AZT) is employed against AIDS and hepatitis; its use is limited by active efflux transporters (AETs) that induce multidrug resistance for intracellular therapies and hamper AZT to reach the brain. Ursodeoxycholic acid (UDCA) conjugation with AZT (prodrug UDCA-AZT) allows to elude the AET systems. To investigate the effect of the Pluronic F68 coating on the loading, release and stability of poly(D,L lactide-co-glicolide) nanoparticles (NPs) embedded with UDCA-AZT. The mean diameter of the NP prepared by nanoprecipitation or emulsion/solvent evaporation methods was determined using both photon correlation spectroscopy and sedimentation field-flow fractionation; particle morphology was detected by scanning electron microscope. The stability of the free and encapsulated UDCA-AZT was evaluated in rat liver homogenates by high-performance liquid chromatography analysis. The mean diameter of the NPs was found to be ∼ 600 nm with a relatively high polydispersity. The NPs obtained by emulsion/solvent evaporation were not able to control the prodrug release, differently from NPs obtained by nanoprecipitation. The presence of the Pluronic coating did not substantially modify the kinetics of the drug release, or the extent of the burst effect that were instead only influenced by the preparation parameters. UDCA-AZT incorporated in the NPs was more stable in the rat liver homogenates than the free prodrug and no influence of the Pluronic coating was observed. Considering the different potential applications of nanoparticles coated and uncoated with Pluronic (brain and macrophage targeting, respectively), both of these nanoparticle systems could be useful in the therapies against HIV.

One-step fabrication of multifunctional micromotors

NASA Astrophysics Data System (ADS)

Gao, Wenlong; Liu, Mei; Liu, Limei; Zhang, Hui; Dong, Bin; Li, Christopher Y.

2015-08-01

Although artificial micromotors have undergone tremendous progress in recent years, their fabrication normally requires complex steps or expensive equipment. In this paper, we report a facile one-step method based on an emulsion solvent evaporation process to fabricate multifunctional micromotors. By simultaneously incorporating various components into an oil-in-water droplet, upon emulsification and solidification, a sphere-shaped, asymmetric, and multifunctional micromotor is formed. Some of the attractive functions of this model micromotor include autonomous movement in high ionic strength solution, remote control, enzymatic disassembly and sustained release. This one-step, versatile fabrication method can be easily scaled up and therefore may have great potential in mass production of multifunctional micromotors for a wide range of practical applications.Although artificial micromotors have undergone tremendous progress in recent years, their fabrication normally requires complex steps or expensive equipment. In this paper, we report a facile one-step method based on an emulsion solvent evaporation process to fabricate multifunctional micromotors. By simultaneously incorporating various components into an oil-in-water droplet, upon emulsification and solidification, a sphere-shaped, asymmetric, and multifunctional micromotor is formed. Some of the attractive functions of this model micromotor include autonomous movement in high ionic strength solution, remote control, enzymatic disassembly and sustained release. This one-step, versatile fabrication method can be easily scaled up and therefore may have great potential in mass production of multifunctional micromotors for a wide range of practical applications. Electronic supplementary information (ESI) available: Videos S1-S4 and Fig. S1-S3. See DOI: 10.1039/c5nr03574k

Influence of some formulation variables on the optimization of pH-dependent, colon-targeted, sustained-release mesalamine microspheres.

PubMed

El-Bary, Ahmed Abd; Aboelwafa, Ahmed A; Al Sharabi, Ibrahim M

2012-03-01

The aim of this work was to understand the influence of different formulation variables on the optimization of pH-dependent, colon-targeted, sustained-release mesalamine microspheres prepared by O/O emulsion solvent evaporation method, employing pH-dependent Eudragit S and hydrophobic pH-independent ethylcellulose polymers. Formulation variables studied included concentration of Eudragit S in the internal phase and the ratios between; internal to external phase, drug to Eudragit S and Eudragit S to ethylcellulose to mesalamine. Prepared microspheres were evaluated by carrying out in vitro release studies and determination of particle size, production yield, and encapsulation efficiency. In addition, morphology of microspheres was examined using optical and scanning electron microscopy. Emulsion solvent evaporation method was found to be sensitive to the studied formulation variables. Particle size and encapsulation efficiency increased by increasing Eudragit S concentration in the internal phase, ratio of internal to external phase, and ratio of Eudragit S to the drug. Employing Eudragit S alone in preparation of the microspheres is only successful in forming acid-resistant microspheres with pulsatile release pattern at high pH. Eudragit S and ethylcellulose blend microspheres were able to control release under acidic condition and to extend drug release at high pH. The stability studies carried out at 40°C/75% RH for 6 months proved the stability of the optimized formulation. From the results of this investigation, microencapsulation of mesalamine in microspheres using blend of Eudragit S and ethylcellulose could constitute a promising approach for site-specific and controlled delivery of drug in colon.

Development of biodegradable drug delivery system to treat addiction.

PubMed

Mandal, T K

1999-06-01

Opiate addiction is a serious problem that has now spread worldwide to all levels of society. Buprenorphine has been used for several years for the treatment of opiate addiction. The objective of this project was to develop sustained-release biodegradable microcapsules for the parenteral delivery of buprenorphine. Biodegradable microcapsules of buprenorphine/poly(lactide-co-glycolide) were prepared using two main procedures based on an in-water drying process in a complex emulsion system. These procedures differ in the way the organic solvent was eliminated: evaporation or extraction. The effect of drug loading and the effect of partial saturation of the aqueous phase with the core material during the in-water solvent evaporation were also studied. The efficiency of encapsulation increased from 11% to 34% when the drug loading was decreased from 20% to 5%. There was no significant change in the efficiency of encapsulation when the aqueous phase was partially saturated with buprenorphine. In changing the solvent removal process from evaporation to extraction, no significant change in the efficiency of encapsulation was observed. The microcapsules prepared by the solvent evaporation were smooth and spherical. However, the microcapsules prepared by the extraction of the organic solvent lost their surface smoothness and became slightly irregular and porous compared with the other batches. The average particle size of the microcapsules was between 14 and 49 microns. The cumulative drug release was between 2% and 4% within the first 24 hr. A sustained drug release continued over 45 days.

Genesis of emulsion texture due to magma mixing: a case study from Chotanagpur Granite Gneiss Complex of Eastern India

NASA Astrophysics Data System (ADS)

Gogoi, Bibhuti; Saikia, Ashima; Ahmad, Mansoor

2016-04-01

The emulsion texture is a rare magma mixing feature in which rounded bodies of one magmatic phase remain dispersed in the other coherent phase (Freundt and Schmincke, 1992). This type of special texture in hybrid rocks can significantly contribute toward understanding the mechanisms facilitating magma mixing and magma chamber dynamics involving two disparate magmas as the exact processes by which mixing occurs still remain unclear. Recent developments in microfluidics have greatly helped us to understand the complex processes governing magma mixing occurring at micro-level. Presented work uses some of the results obtained from microfluidic experiments with a view to understand the formation mechanism of emulsions preserved in the hybrid rocks of the Ghansura Rhyolite Dome (GRD) of Proterozoic Chotanagpur Granite Gneiss Complex (CGGC), Eastern India. The GRD has preserved hybrid rocks displaying emulsion texture that formed due to the interaction of a phenocryst-rich basaltic magma and host rhyolite magma. The emulsions are more or less spherical in shape and dominantly composed of amphibole having biotite rinds set in a matrix of biotite, plagioclase, K-feldspar and quartz. Amphibole compositions were determined from the core of the emulsions to the rim with a view to check for cationic substitutions. The amphibole constituting the emulsions is actinolite in composition, and commonly shows tschermakite (Ts) and pargasite (Prg) substitutions. From petrographical and mineral-chemical analyses we infer that when mafic magma, containing phenocrysts of augite, came in contact with felsic magma, diffusion of cations like H+, Al3+and others occurred from the felsic to the mafic system. These cations reacted with the clinopyroxene phenocrysts in the mafic magma to form amphibole (actinolite) crystals. The formation of amphibole crystals in the mafic system greatly increased the viscosity of the system allowing the amphibole crystals to venture into the adjacent felsic magma as veins. As these veins traversed in the felsic medium they underwent sinuous perturbations as a result of the competition between the viscous torque, due to difference in drag on each side of the veins, and the dynamic viscous bending resistance (Cubaud and Mason, 2009). Further downstream, the undulations amplified and swirls started to develop on the sinuous veins by accumulating the high viscosity mafic phase into central bulbs and depleting the regions in between them forming tails. Gradually the tails thinned out and blended into the surrounding felsic melt forming discrete viscous emulsions/swirls. After separation, the amphibole constituting the emulsions started interacting with the surrounding felsic magma forming biotite at the periphery of the emulsions. Eventually, biotite is eroded away and new rinds simultaneously form on freshly eroded surfaces of emulsions facilitating the mixing process (Farner et al., 2014). Cubaud T and Mason TG (2009) New J. Phys. 11, 075029. Farner et al. (2014) Earth and Planetary Science Letters 393, 49-59. Freundt A and Schmincke HU (1992) Contrib Mineral Petrol 112, 1-19.

Laser inhibited diffusion in rhodamine-ethanol solutions

NASA Technical Reports Server (NTRS)

Lawandy, N. M.; Fuhr, P. L.; Robinson, D. W.

1981-01-01

The diffusion of rhodamine-6G dye in ethanol is observed to be inhibited by optical pumping by a cadmium laser. The diffusion process is observed as a function of the solution temperature. The relative difference in diffusion coefficients with and without optical pumping is calculated. The effect is interpreted as being due to a stronger solvent-dye interaction in the first excited singlet state of rhodamine-6G.

Application of Molecular Dynamics Simulations in Molecular Property Prediction II: Diffusion Coefficient

PubMed Central

Wang, Junmei; Hou, Tingjun

2011-01-01

In this work, we have evaluated how well the General AMBER force field (GAFF) performs in studying the dynamic properties of liquids. Diffusion coefficients (D) have been predicted for 17 solvents, 5 organic compounds in aqueous solutions, 4 proteins in aqueous solutions, and 9 organic compounds in non-aqueous solutions. An efficient sampling strategy has been proposed and tested in the calculation of the diffusion coefficients of solutes in solutions. There are two major findings of this study. First of all, the diffusion coefficients of organic solutes in aqueous solution can be well predicted: the average unsigned error (AUE) and the root-mean-square error (RMSE) are 0.137 and 0.171 ×10−5 cm−2s−1, respectively. Second, although the absolute values of D cannot be predicted, good correlations have been achieved for 8 organic solvents with experimental data (R2 = 0.784), 4 proteins in aqueous solutions (R2 = 0.996) and 9 organic compounds in non-aqueous solutions (R2 = 0.834). The temperature dependent behaviors of three solvents, namely, TIP3P water, dimethyl sulfoxide (DMSO) and cyclohexane have been studied. The major MD settings, such as the sizes of simulation boxes and with/without wrapping the coordinates of MD snapshots into the primary simulation boxes have been explored. We have concluded that our sampling strategy that averaging the mean square displacement (MSD) collected in multiple short-MD simulations is efficient in predicting diffusion coefficients of solutes at infinite dilution. PMID:21953689

Diffusion affected magnetic field effect in exciplex fluorescence

NASA Astrophysics Data System (ADS)

Burshtein, Anatoly I.; Ivanov, Anatoly I.

2014-07-01

The fluorescence of the exciplex, 1[D+δA-δ], formed at contact of photoexcited acceptor 1A* with an electron donor 1D, is known to be very sensitive to an external magnetic field, reducing the spin conversion efficiency in the resulting geminate radical ion pair, 1, 3[D+…A-]. The relative increase of the exciplex fluorescence in the highest magnetic field compared to the lowest one, known as the magnetic field effect, crucially depends on the viscosity of the solvent. This phenomenon first studied experimentally is at first reproduced here theoretically. The magnetic field effect is shown to vanish in both limits of high and low solvent diffusivity reaching a maximum in between. It is also very sensitive to the solvent dielectric constant and to the exciplex and radical-ion pair conversion rates.

Diffusion affected magnetic field effect in exciplex fluorescence.

PubMed

Burshtein, Anatoly I; Ivanov, Anatoly I

2014-07-14

The fluorescence of the exciplex, (1)[D(+δ)A(-δ)], formed at contact of photoexcited acceptor (1)A(*) with an electron donor (1)D, is known to be very sensitive to an external magnetic field, reducing the spin conversion efficiency in the resulting geminate radical ion pair, (1, 3)[D(+)…A(-)]. The relative increase of the exciplex fluorescence in the highest magnetic field compared to the lowest one, known as the magnetic field effect, crucially depends on the viscosity of the solvent. This phenomenon first studied experimentally is at first reproduced here theoretically. The magnetic field effect is shown to vanish in both limits of high and low solvent diffusivity reaching a maximum in between. It is also very sensitive to the solvent dielectric constant and to the exciplex and radical-ion pair conversion rates.

A Colorful Solubility Exercise for Organic Chemistry

ERIC Educational Resources Information Center

Shugrue, Christopher R.; Mentzen, Hans H., II; Linton, Brian R.

2015-01-01

A discovery chemistry laboratory has been developed for the introductory organic chemistry student to investigate the concepts of polarity, miscibility, solubility, and density. The simple procedure takes advantage of the solubility of two colored dyes in a series of solvents or solvent mixtures, and the diffusion of colors can be easily…

Mathematical Model of Transfer and Deposition of Finely Dispersed Particles in a Turbulent Flow of Emulsions and Suspensions

NASA Astrophysics Data System (ADS)

Laptev, A. G.; Basharov, M. M.

2018-05-01

The problem of modeling turbulent transfer of finely dispersed particles in liquids has been considered. An approach is used where the transport of particles is represented in the form of a variety of the diffusion process with the coefficient of turbulent transfer to the wall. Differential equations of transfer are written for different cases, and a solution of the cell model is obtained for calculating the efficiency of separation in a channel. Based on the theory of turbulent transfer of particles and of the boundary layer model, an expression has been obtained for calculating the rate of turbulent deposition of finely dispersed particles. The application of this expression in determining the efficiency of physical coagulation of emulsions in different channels and on the surface of chaotic packings is shown.

Mathematical Model of Transfer and Deposition of Finely Dispersed Particles in a Turbulent Flow of Emulsions and Suspensions

NASA Astrophysics Data System (ADS)

Laptev, A. G.; Basharov, M. M.

2018-03-01

The problem of modeling turbulent transfer of finely dispersed particles in liquids has been considered. An approach is used where the transport of particles is represented in the form of a variety of the diffusion process with the coefficient of turbulent transfer to the wall. Differential equations of transfer are written for different cases, and a solution of the cell model is obtained for calculating the efficiency of separation in a channel. Based on the theory of turbulent transfer of particles and of the boundary layer model, an expression has been obtained for calculating the rate of turbulent deposition of finely dispersed particles. The application of this expression in determining the efficiency of physical coagulation of emulsions in different channels and on the surface of chaotic packings is shown.

X-Ray Fluorescence Solvent Detection at the Substrate-Adhesive Interface

NASA Technical Reports Server (NTRS)

Wurth, Laura; Evans, Kurt; Weber, Bart; Headrick, Sarah

2005-01-01

With environmental regulations limiting the use of volatile organic compounds, low-vapor pressure solvents have replaced traditional degreasing solvents for bond substrate preparation. When used to clean and prepare porous bond substrates such as phenolic composites, low vapor pressure solvents can penetrate deep into substrate pore networks and remain there for extended periods. Trapped solvents can interact with applied adhesives either prior to or during cure, potentially compromising bond properties. Currently, methods for characterizing solvent time-depth profiles in bond substrates are limited to bulk gravimetric or sectioning techniques. While sectioning techniques such as microtome allow construction of solvent depth profiles, their depth resolution and reliability are limited by substrate type. Sectioning techniques are particularly limited near the adhesive-substrate interface where depth resolution is further limited by adhesive-substrate hardness and, in the case of a partially cured adhesive, mechanical properties differences. Additionally, sectioning techniques cannot provide information about lateral solvent diffusion. Cross-section component mapping is an alternative method for measuring solvent migration in porous substrates that eliminates the issues associated with sectioning techniques. With cross-section mapping, the solvent-wiped substrate is sectioned perpendicular rather than parallel to the wiped surface, and the sectioned surface is analyzed for the solvent or solvent components of interest using a two-dimensional mapping or imaging technique. Solvent mapping can be performed using either direct or indirect methods. With a direct method, one or more solvent components are mapped using red or Raman spectroscopy together with a moveable sample stage and/or focal plane array detector. With an indirect method, an elemental "tag" not present in the substrate is added to the solvent before the substrate is wiped. Following cross sectioning, the tag element can then be mapped by its characteristic x-ray emission using either x-ray fluorescence, or electron-beam energy-and wavelength-dispersive x-ray spectrometry. The direct mapping techniques avoid issues of different diffusion or migration rates of solvents and elemental tags, while the indirect techniques avoid spectral resolution issues in cases where solvents and substrates have adjacent or overlapping peaks. In this study, cross-section component indirect mapping is being evaluated as a method for measuring migration of d-limonene based solvents in glass-cloth phenolic composite (GCP) prior to and during subsequent bonding and epoxy adhesive cure.

Steric effects on diffusion into bituminous coals

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

John W. Larsen; Doyoung Lee

2006-02-01

The reactions of maleic anhydride, cis-maleate esters, and acetylenedicarboxylate esters with Pittsburgh No. 8 or Illinois No. 6 coal using o-xylene or o-dichlorobenzene solvent are diffusion controlled. Diffusion is Fickian in all cases. The measured activation energies are between 5.4 and 7.6 kcal/mol. Diffusion rates decrease slowly with increasing alkyl chain length and sharply with branching. Diffusion rates are slightly faster with o-xylene than when o-dichlorobenzene is used. 40 refs., 5 figs., 4 tabs.

OBSERVATIONS OF HIGH-ENERGY COSMIC-RAY ELECTRONS FROM 30 GeV TO 3 TeV WITH EMULSION CHAMBERS

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

Kobayashi, T.; Komori, Y.; Yoshida, K.

2012-12-01

We have performed a series of cosmic-ray electron observations using balloon-borne emulsion chambers since 1968. While we previously reported the results from subsets of the exposures, the final results of the total exposures up to 2001 are presented here. Our successive experiments have yielded a total exposure of 8.19 m{sup 2} sr day at altitudes of 4.0-9.4 g cm{sup -2}. The performance of the emulsion chambers was examined by accelerator beam tests and Monte Carlo simulations, and the on-board calibrations were carried out by using the flight data. In this work, we present the cosmic-ray electron spectrum in the energymore » range from 30 GeV to 3 TeV at the top of the atmosphere, which is well represented by a power-law function with an index of -3.28 {+-} 0.10. The observed data can also be interpreted in terms of diffusive propagation models. The evidence of cosmic-ray electrons up to 3 TeV suggests the existence of cosmic-ray electron sources at distances within {approx}1 kpc and times within {approx}1 Multiplication-Sign 10{sup 5} yr ago.« less

Theories of binary fluid mixtures: from phase-separation kinetics to active emulsions

NASA Astrophysics Data System (ADS)

Cates, Michael E.; Tjhung, Elsen

2018-02-01

Binary fluid mixtures are examples of complex fluids whose microstructure and flow are strongly coupled. For pairs of simple fluids, the microstructure consists of droplets or bicontinuous demixed domains and the physics is controlled by the interfaces between these domains. At continuum level, the structure is defined by a composition field whose gradients which are steep near interfaces drive its diffusive current. These gradients also cause thermodynamic stresses which can drive fluid flow. Fluid flow in turn advects the composition field, while thermal noise creates additional random fluxes that allow the system to explore its configuration space and move towards the Boltzmann distribution. This article introduces continuum models of binary fluids, first covering some well-studied areas such as the thermodynamics and kinetics of phase separation, and emulsion stability. We then address cases where one of the fluid components has anisotropic structure at mesoscopic scales creating nematic (or polar) liquid-crystalline order; this can be described through an additional tensor (or vector) order parameter field. We conclude by outlining a thriving area of current research, namely active emulsions, in which one of the binary components consists of living or synthetic material that is continuously converting chemical energy into mechanical work.

Polyamide nanocapsules and nano-emulsions containing Parsol® MCX and Parsol® 1789: in vitro release, ex vivo skin penetration and photo-stability studies.

PubMed

Hanno, Ibrahim; Anselmi, Cecilia; Bouchemal, Kawthar

2012-02-01

To prepare polyamide nanocapsules for skin photo-protection, encapsulating α-tocopherol, Parsol®MCX (ethylhexyl methoxycinnamate) and/or Parsol®1789 (butyl methoxydibenzoylmethane). Nanocapsules were obtained by combining spontaneous emulsification and interfacial polycondensation reaction between sebacoyl chloride and diethylenetriamine. Nano-emulsions used as control were obtained by the same process without monomers. The influence of carrier on release rate was studied in vitro with a membrane-free model. Epidermal penetration of encapsulated sunscreens was ex vivo evaluated using Franz diffusion cells. Ability of encapsulated sunscreens to improve photo-stability was verified by comparing percentage of degradation after UV radiation exposure. Sunscreen-containing nanocapsules (260-400 nm) were successfully prepared; yield of encapsulation was >98%. Parsol®MCX and Parsol®1789 encapsulation led to decreased release rate by up to 60% in comparison with nano-emulsion and allowed minimum penetration through pig ear epidermis. Presence of polyamide shell protected encapsulated sunscreen filters from photo-degradation without affecting their activity. Encapsulation of Parsol®MCX and Parsol®1789 into oil-core of polyamide nanocapsules allowed protection from photo-degradation, controlled release from nanocapsules, and limited penetration through pig ear epidermis.

Conformational dynamics of a crystalline protein from microsecond-scale molecular dynamics simulations and diffuse X-ray scattering

DOE PAGES

Wall, Michael E.; Van Benschoten, Andrew H.; Sauter, Nicholas K.; ...

2014-12-01

X-ray diffraction from protein crystals includes both sharply peaked Bragg reflections and diffuse intensity between the peaks. The information in Bragg scattering is limited to what is available in the mean electron density. The diffuse scattering arises from correlations in the electron density variations and therefore contains information about collective motions in proteins. Previous studies using molecular-dynamics (MD) simulations to model diffuse scattering have been hindered by insufficient sampling of the conformational ensemble. To overcome this issue, we have performed a 1.1-μs MD simulation of crystalline staphylococcal nuclease, providing 100-fold more sampling than previous studies. This simulation enables reproducible calculationsmore » of the diffuse intensity and predicts functionally important motions, including transitions among at least eight metastable states with different active-site geometries. The total diffuse intensity calculated using the MD model is highly correlated with the experimental data. In particular, there is excellent agreement for the isotropic component of the diffuse intensity, and substantial but weaker agreement for the anisotropic component. The decomposition of the MD model into protein and solvent components indicates that protein–solvent interactions contribute substantially to the overall diffuse intensity. In conclusion, diffuse scattering can be used to validate predictions from MD simulations and can provide information to improve MD models of protein motions.« less

Conformational dynamics of a crystalline protein from microsecond-scale molecular dynamics simulations and diffuse X-ray scattering

PubMed Central

Wall, Michael E.; Van Benschoten, Andrew H.; Sauter, Nicholas K.; Adams, Paul D.; Fraser, James S.; Terwilliger, Thomas C.

2014-01-01

X-ray diffraction from protein crystals includes both sharply peaked Bragg reflections and diffuse intensity between the peaks. The information in Bragg scattering is limited to what is available in the mean electron density. The diffuse scattering arises from correlations in the electron density variations and therefore contains information about collective motions in proteins. Previous studies using molecular-dynamics (MD) simulations to model diffuse scattering have been hindered by insufficient sampling of the conformational ensemble. To overcome this issue, we have performed a 1.1-μs MD simulation of crystalline staphylococcal nuclease, providing 100-fold more sampling than previous studies. This simulation enables reproducible calculations of the diffuse intensity and predicts functionally important motions, including transitions among at least eight metastable states with different active-site geometries. The total diffuse intensity calculated using the MD model is highly correlated with the experimental data. In particular, there is excellent agreement for the isotropic component of the diffuse intensity, and substantial but weaker agreement for the anisotropic component. Decomposition of the MD model into protein and solvent components indicates that protein–solvent interactions contribute substantially to the overall diffuse intensity. We conclude that diffuse scattering can be used to validate predictions from MD simulations and can provide information to improve MD models of protein motions. PMID:25453071

Aquivion Perfluorosulfonic Superacid as an Efficient Pickering Interfacial Catalyst for the Hydrolysis of Triglycerides.

PubMed

Shi, Hui; Fan, Zhaoyu; Hong, Bing; Pera-Titus, Marc

2017-09-11

Rational design of the surface properties of heterogeneous catalysts can boost the interfacial activity in biphasic reactions through the generation of Pickering emulsions. This concept, termed Pickering interfacial catalysis (PIC), has shown promising credentials in acid-catalyzed transesterification, ester hydrolysis, acetalization, etherification, and alkylation reactions. PIC has now been applied to the efficient, solvent-free hydrolysis of the triglyceride glyceryl trilaurate to lauric acid, catalyzed by Aquivion perfluorosulfonic superacid at mild conditions (100 °C and ambient pressure). © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Human Health Concenrs of Metalworking Fluid Components

NASA Astrophysics Data System (ADS)

Gerulová, Kristína; Buranská, Eva; Soldán, Maroš

2017-06-01

Exploration of 209 available Material safety data sheets of 85 straight oils, 46 emulsions, 51 semi-synthetics and 27 synthetics was carried out to provide a report on the most widely used components defined as dangerous substances. As many as 217 of different substances of which 15 were identified as biocides, 17 as corrosion inhibitors or neutralizing agent, 17 were lubricity improvers and 38 different base fluids, lubricity solvents or surfactants, while 93 substances were not identified specifically and 37 substances occurred only once. This article is focused on the list of base fluids in straight oils and their possible health effects.

The neutral oil in commercial linear alkylbenzenesulfonate and its effect on organic solute solubility in water

USGS Publications Warehouse

Chiou, C.T.; Kile, D.E.; Rutherford, D.W.

1991-01-01

Apparent water solubilities of 1,1-bis(p-chlorophenyl)-2,2,2-trichloroethane (DDT), 2,4,5,2???,5???-penta-chlorobiphenyl (PCB), and 1,2,3-trichlorobenzene (TCB) were determined at room temperature in aqueous solutions of commercial linear alkylbenzenesulfonate (LAS), oil-free (solvent-extracted) LAS, and single-molecular 4-dodecyl-benzenesulfonate. The extent of solute solubility enhancement by commercial LAS is markedly greater than that by other ionic surfactants below the measured critical micelle concentration (CMC); above the CMC, the enhancement data with LAS are comparable with other surfactants as micelles. The small amount of neutral oils in commercial LAS (1.7%), comprising linear alkylbenzenes (LABs) and bis(alkylphenyl) sulfones, contributes significantly to the enhanced solubility of DDT and PCB below the CMC; the effect is ascribed to formation of oil-surfactant emulsions. The oil-surfactant emulsion formed corresponds to ???9-10% of the commercial LAS below the CMC. The data suggest that discharge of wastewater containing a significant level of oils and surface-active agents could lead to potential mobilization of organic pollutants and LABs in aquatic environments.

Using bio-dispersive solution of chitosan for green dispersive liquid-liquid microextraction of trace amounts of Cu(II) in edible oils prior to analysis by ICP-OES.

PubMed

Limchoowong, Nunticha; Sricharoen, Phitchan; Techawongstien, Suchila; Chanthai, Saksit

2017-09-01

A green approach using chitosan solution as a novel bio-dispersive agent for the dispersive liquid-liquid microextraction (DLLME) of trace amounts of Cu(II) in edible oils is presented. An emulsion was formed by mixing the oil sample with 300µL of 0.25% (w/v) chitosan solution containing 200µL of 6molL -1 HCl. Deionized water was used to induce emulsion breaking without centrifugation. The centrifuged Cu(II) extract was collected and analyzed using an inductively coupled plasma-optical emission spectrometer. The detection and quantitation limits were 2.1 and 6.8µgL -1 , respectively. Trace amounts of Cu(II) in six edible oil samples were tested under optimum conditions for DLLME, with a recovery ranging from 90.3% to 109.3%. Therefore, the new dispersive agent in DLLME offers superior performance owing to the non-toxic nature of the solvent, short extraction time, high sensitivity, and easy operation. Copyright © 2017 Elsevier Ltd. All rights reserved.

Absorption and resonance Raman characteristics of β-carotene in water-ethanol mixtures, emulsion and hydrogel

NASA Astrophysics Data System (ADS)

Meinhardt-Wollweber, Merve; Suhr, Christian; Kniggendorf, Ann-Kathrin; Roth, Bernhard

2018-05-01

Absorption or resonance Raman scattering are often used to identify and even quantify carotenoids in situ. We studied the absorption spectra, the Raman spectra and their resonance behavior of β-carotene in different molecular environments set up as mixtures from lipid (emulsion) and non-polar (ethanol) solvents and a polar component (water) with regard to their application as references for in situ measurement. We show how both absorption profiles and resonance spectra of β-carotene strongly depend on the molecular environment. Most notably, our data suggests that the characteristic bathochromic absorption peak of J-aggregates does not contribute to carotenoid resonance conditions, and show how the Raman shift of the C=C stretching mode is dependent on both, the molecular environment and the excitation wavelength. Overall, the spectroscopic data collected here is highly relevant for the interpretation of in situ spectroscopic data in terms of carotenoid identification and quantification by resonance Raman spectroscopy as well as the preparation of reference samples. In particular, our data promotes careful consideration of appropriate molecular environment for reference samples.

Submicron polycaprolactone particles as a carrier for imaging contrast agent for in vitro applications.

PubMed

Iqbal, Muhammad; Robin, Sophie; Humbert, Philippe; Viennet, Céline; Agusti, Geraldine; Fessi, Hatem; Elaissari, Abdelhamid

2015-12-01

Fluorescent materials have recently attracted considerable attention due to their unique properties and high performance as imaging agent in biomedical fields. Different imaging agents have been encapsulated in order to restrict its delivery to a specific area. In this study, a fluorescent contrast agent was encapsulated for in vitro application by polycaprolactone (PCL) polymer. The encapsulation was performed using modified double emulsion solvent evaporation technique with sonication. Fluorescent nanoparticles (20 nm) were incorporated in the inner aqueous phase of double emulsion. A number of samples were fabricated using different concentrations of fluorescent contrast agent. The contrast agent-containing submicron particle was characterized by a zetasizer for average particle size, SEM and TEM for morphology observations and fluorescence spectrophotometer for encapsulation efficiency. Moreover, contrast agent distribution in the PCL matrix was determined by confocal microscopy. The incorporation of contrast agent in different concentrations did not affect the physicochemical properties of PCL particles and the average size of encapsulated particles was found to be in the submicron range. Copyright © 2015 Elsevier B.V. All rights reserved.

Understanding of Relationship between Phospholipid Membrane Permeability and Self-Diffusion Coefficients of Some Drugs and Biologically Active Compounds in Model Solvents.

PubMed

Blokhina, Svetlana V; Volkova, Tatyana V; Golubev, Vasiliy A; Perlovich, German L

2017-10-02

In this work we measured self-diffusion coefficients of 5 drugs (aspirin, caffeine, ethionamide, salicylic acid, and paracetamol) and 11 biologically active compounds of similar structure in deuterated water and 1-octanol by NMR. It has been found that an increase in the van der Waals volume of the molecules of the studied substances result in reduction of their diffusion mobility in both solvents. The analysis of the experimental data showed the influence of chemical nature and structural isomerization of the molecules on the diffusion mobility. Apparent permeability coefficients of the studied compounds were determined using an artificial phospholipid membrane made of egg lecithin as a model of in vivo absorption. Distribution coefficients in 1-octanol/buffer pH 7.4 system were measured. For the first time the model of the passive diffusion through the phospholipid membrane was validated based on the experimental data. To this end, the passive diffusion was considered as an additive process of molecule passage through the aqueous boundary layer before the membrane and 1-octanol barrier simulating the lipid layer of the membrane.

Structure and Dynamics of Solvent Landscapes in Charge-Transfer Reactions

NASA Astrophysics Data System (ADS)

Leite, Vitor B. Pereira

The dynamics of solvent polarization plays a major role in the control of charge transfer reactions. The success of Marcus theory describing the solvent influence via a single collective quadratic polarization coordinate has been remarkable. Onuchic and Wolynes have recently proposed (J. Chem Phys 98 (3) 2218, 1993) a simple model demonstrating how a many-dimensional-complex model composed by several dipole moments (representing solvent molecules or polar groups in proteins) can be reduced under the appropriate limits into the Marcus Model. This work presents a dynamical study of the same model, which is characterized by two parameters, an average dipole-dipole interaction as a term associated with the potential energy landscape roughness. It is shown why the effective potential, obtained using a thermodynamic approach, is appropriate for the dynamics of the system. At high temperatures, the system exhibits effective diffusive one-dimensional dynamics, where the Born-Marcus limit is recovered. At low temperatures, a glassy phase appears with a slow non-self-averaging dynamics. At intermediate temperatures, the concept of equivalent diffusion paths and polarization dependence effects are discussed. This approach is extended to treat more realistic solvent models. Real solvents are discussed in terms of simple parameters described above, and an analysis of how different regimes affect the rate of charge transfer is presented. Finally, these ideas are correlated to analogous problems in other areas.

A simple and effective solution to the constrained QM/MM simulations

NASA Astrophysics Data System (ADS)

Takahashi, Hideaki; Kambe, Hiroyuki; Morita, Akihiro

2018-04-01

It is a promising extension of the quantum mechanical/molecular mechanical (QM/MM) approach to incorporate the solvent molecules surrounding the QM solute into the QM region to ensure the adequate description of the electronic polarization of the solute. However, the solvent molecules in the QM region inevitably diffuse into the MM bulk during the QM/MM simulation. In this article, we developed a simple and efficient method, referred to as the "boundary constraint with correction (BCC)," to prevent the diffusion of the solvent water molecules by means of a constraint potential. The point of the BCC method is to compensate the error in a statistical property due to the bias potential by adding a correction term obtained through a set of QM/MM simulations. The BCC method is designed so that the effect of the bias potential completely vanishes when the QM solvent is identical with the MM solvent. Furthermore, the desirable conditions, that is, the continuities of energy and force and the conservations of energy and momentum, are fulfilled in principle. We applied the QM/MM-BCC method to a hydronium ion(H3O+) in aqueous solution to construct the radial distribution function (RDF) of the solvent around the solute. It was demonstrated that the correction term fairly compensated the error and led the RDF in good agreement with the result given by an ab initio molecular dynamics simulation.

High-resolution direct 3D printed PLGA scaffolds: print and shrink.

PubMed

Chia, Helena N; Wu, Benjamin M

2014-12-17

Direct three-dimensional printing (3DP) produces the final part composed of the powder and binder used in fabrication. An advantage of direct 3DP is control over both the microarchitecture and macroarchitecture. Prints which use porogen incorporated in the powder result in high pore interconnectivity, uniform porosity, and defined pore size after leaching. The main limitations of direct 3DP for synthetic polymers are the use of organic solvents which can dissolve polymers used in most printheads and limited resolution due to unavoidable spreading of the binder droplet after contact with the powder. This study describes a materials processing strategy to eliminate the use of organic solvent during the printing process and to improve 3DP resolution by shrinking with a non-solvent plasticizer. Briefly, poly(lactic-co-glycolic acid) (PLGA) powder was prepared by emulsion solvent evaporation to form polymer microparticles. The printing powder was composed of polymer microparticles dry mixed with sucrose particles. After printing with a water-based liquid binder, the polymer microparticles were fused together to form a network by solvent vapor in an enclosed vessel. The sucrose is removed by leaching and the resulting scaffold is placed in a solution of methanol. The methanol acts as a non-solvent plasticizer and allows for polymer chain rearrangement and efficient packing of polymer chains. The resulting volumetric shrinkage is ∼80% at 90% methanol. A complex shape (honey-comb) was designed, printed, and shrunken to demonstrate isotropic shrinking with the ability to reach a final resolution of ∼400 μm. The effect of type of alcohol (i.e. methanol or ethanol), concentration of alcohol, and temperature on volumetric shrinking was studied. This study presents a novel materials processing strategy to overcome the main limitations of direct 3DP to produce high resolution PLGA scaffolds.

[Advances in studies on multi-stage countercurrent extraction technology in traditional Chinese medicine].

PubMed

Xie, Zhi-Peng; Liu, Xue-Song; Chen, Yong; Cai, Ming; Qu, Hai-Bin; Cheng, Yi-Yu

2007-05-01

Multi-stage countercurrent extraction technology, integrating solvent extraction, repercolation with dynamic and countercurrent extraction, is a novel extraction technology for the traditional Chinese medicine. This solvent-saving, energy-saving and high-extraction-efficiency technology can at the most drive active compounds to diffuse from the herbal materials into the solvent stage by stage by creating concentration differences between the herbal materials and the solvents. This paper reviewed the basic principle, the influence factors and the research progress and trends of the equipments and the application of the multi-stage countercurrent extraction.

Dielectric relaxation of ethylene carbonate and propylene carbonate from molecular dynamics simulations

DOE PAGES

Chaudhari, Mangesh I.; You, Xinli; Pratt, Lawrence R.; ...

2015-11-24

Ethylene carbonate (EC) and propylene carbonate (PC) are widely used solvents in lithium (Li)-ion batteries and supercapacitors. Ion dissolution and diffusion in those media are correlated with solvent dielectric responses. Here, we use all-atom molecular dynamics simulations of the pure solvents to calculate dielectric constants and relaxation times, and molecular mobilities. The computed results are compared with limited available experiments to assist more exhaustive studies of these important characteristics. As a result, the observed agreement is encouraging and provides guidance for further validation of force-field simulation models for EC and PC solvents.

Anti-obesity effects of escins extracted from the seeds of Aesculus turbinata BLUME (Hippocastanaceae).

PubMed

Hu, Jiang-Ning; Zhu, Xue-Mei; Han, Li-Kun; Saito, Masato; Sun, Yin-Shi; Yoshikawa, Masayuki; Kimura, Yoshiyuki; Zheng, Yi-Nan

2008-01-01

To investigate the anti-obesity effects of escins extracted from the seeds of Aesculus turbinata BLUME, anti-obesity models in vitro and in vivo were employed. In a preliminary experiment, different solvent fractions of Aesculus turbinata BlUME as well as two isolated compounds were tested for their effects on pancreatic lipase (PL) in vitro. Subsequently, female ICR mice were fed a high fat diet with or without different concentrations of total escins for 11 weeks to examine body weight, parametrial adipose tissue weight, and hepatic triacylglycerol (TG) and total cholesterol (TC) contents. Plasma triacylglycerol levels (TG) after oral administration of lipid emulsions to rats were also investigated. The results showed that total escins (1 mg/ml) as well as two compounds isolated from total escins, namely escin Ib and IIa, showed inhibitory effects on PL activity. In vivo, total escins suppressed the increase in body weight, parametrial adipose tissue weight, TG content, and TC content in mice's liver; TG content in rat plasma was also reduced at 1, 2 and 3 h after oral administration of the lipid emulsion plus different concentrations of escins compared to those in the lipid emulsion groups. Meanwhile, mice fed a high fat diet plus 2% total escins for 3 d had an increased TG level in the feces compared to the HF group. The reason for this may be due to a delay in the intestinal absorption of dietary fat by inhibiting PL activity.

Classification of nine malathion emulsion samples by using carbon isotope ratios and the ratio of organic solvents.

PubMed

Suto, Nana; Kawashima, Hiroto

2017-01-01

The compound specific isotope analysis is nowadays an important and powerful tool in geochemical, environmental and forensics field. On November 2013, Aqli Foods Corporation in Japan dealt with complaints about stench from frozen foods produced. Subsequently, very high concentrations of organophosphorus pesticide as malathion, ethylbenzene and xylene were detected in recovered frozen foods. In particular case, we present the method to measure the stable carbon isotope ratio (δ 13 C) of nine malathion emulsion pesticides using gas chromatography/isotope ratio mass spectrometry (GC/IRMS) to identify the source. The δ 13 C values of malathion ranged from -30.6‰ to -29.5‰. Because malathion used in all malathion emulsions sold in Japan is imported from the same overseas company, Cheminova, Denmark. The δ 13 C values of ethylbenzene ranged from -28.2‰ to -20.8‰ and those of m,p-xylene from -28.7‰ to -25.2‰. The differences in the δ 13 C values may be because of the material itself and chemical processing. We also determined the ratio of ethylbenzene to m,p-xylene and finally categorized the nine malathion samples into five groups on the basis of this ratio and the δ 13 C values of ethylbenzene and m,p-xylene. The results of isotopic fractionation during volatilization (refrigerate, room temperature and incubator) was negligible small. Copyright © 2016 The Chartered Society of Forensic Sciences. Published by Elsevier Ireland Ltd. All rights reserved.

Homogenization Theory for the Prediction of Obstructed Solute Diffusivity in Macromolecular Solutions.

PubMed

Donovan, Preston; Chehreghanianzabi, Yasaman; Rathinam, Muruhan; Zustiak, Silviya Petrova

2016-01-01

The study of diffusion in macromolecular solutions is important in many biomedical applications such as separations, drug delivery, and cell encapsulation, and key for many biological processes such as protein assembly and interstitial transport. Not surprisingly, multiple models for the a-priori prediction of diffusion in macromolecular environments have been proposed. However, most models include parameters that are not readily measurable, are specific to the polymer-solute-solvent system, or are fitted and do not have a physical meaning. Here, for the first time, we develop a homogenization theory framework for the prediction of effective solute diffusivity in macromolecular environments based on physical parameters that are easily measurable and not specific to the macromolecule-solute-solvent system. Homogenization theory is useful for situations where knowledge of fine-scale parameters is used to predict bulk system behavior. As a first approximation, we focus on a model where the solute is subjected to obstructed diffusion via stationary spherical obstacles. We find that the homogenization theory results agree well with computationally more expensive Monte Carlo simulations. Moreover, the homogenization theory agrees with effective diffusivities of a solute in dilute and semi-dilute polymer solutions measured using fluorescence correlation spectroscopy. Lastly, we provide a mathematical formula for the effective diffusivity in terms of a non-dimensional and easily measurable geometric system parameter.

Tracer diffusion in active suspensions.

PubMed

Burkholder, Eric W; Brady, John F

2017-05-01

We study the diffusion of a Brownian probe particle of size R in a dilute dispersion of active Brownian particles of size a, characteristic swim speed U_{0}, reorientation time τ_{R}, and mechanical energy k_{s}T_{s}=ζ_{a}U_{0}^{2}τ_{R}/6, where ζ_{a} is the Stokes drag coefficient of a swimmer. The probe has a thermal diffusivity D_{P}=k_{B}T/ζ_{P}, where k_{B}T is the thermal energy of the solvent and ζ_{P} is the Stokes drag coefficient for the probe. When the swimmers are inactive, collisions between the probe and the swimmers sterically hinder the probe's diffusive motion. In competition with this steric hindrance is an enhancement driven by the activity of the swimmers. The strength of swimming relative to thermal diffusion is set by Pe_{s}=U_{0}a/D_{P}. The active contribution to the diffusivity scales as Pe_{s}^{2} for weak swimming and Pe_{s} for strong swimming, but the transition between these two regimes is nonmonotonic. When fluctuations in the probe motion decay on the time scale τ_{R}, the active diffusivity scales as k_{s}T_{s}/ζ_{P}: the probe moves as if it were immersed in a solvent with energy k_{s}T_{s} rather than k_{B}T.

Three-Dimensional Morphology Control Yielding Enhanced Hole Mobility in Air-Processed Organic Photovoltaics: Demonstration with Grazing-Incidence Wide-Angle X-ray Scattering

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

Moore, Levi M. J.; Bhattacharya, Mithun; Wu, Qi

Polymer organic photovoltaic (OPV) device performance is defined by the three-dimensional morphology of the phase-separated domains in the active layer. Here, we determine the evolution of morphology through different stages of tailored solvent vapor and thermal annealing techniques in air-processed poly(3-hexylthiophene-2,5-diyl)/phenyl-C61-butyric acid methyl ester-based OPV blends. A comparative evaluation of the effect of solvent type used for vapor annealing was performed using grazing-incidence wide-angle X-ray scattering, atomic force microscopy, and UV–vis spectroscopy to probe the active-layer morphology. A nonhalogenated orthogonal solvent was found to impart controlled morphological features within the exciton diffusion length scales, enhanced absorbance, greater crystallinity, increased paracrystallinemore » disorder, and improved charge-carrier mobility. Low-boiling, fast-diffusing isopropanol allowed the greatest control over the nanoscale structure of the solvents evaluated and yielded a cocontinuous morphology with narrowed domains and enhanced paths for the charge carrier to reach the anode.« less

Preparation of acetazolamide composite microparticles by supercritical anti-solvent techniques.

PubMed

Duarte, Ana Rita C; Roy, Christelle; Vega-González, Arlette; Duarte, Catarina M M; Subra-Paternault, Pascale

2007-03-06

The possibility of preparation of ophthalmic drug delivery systems using compressed anti-solvent technology was evaluated. Eudragit RS 100 and RL 100 were used as drug carriers, acetazolamide was the model drug processed. Compressed anti-solvent experiments were carried out as a semi-continuous or a batch operation from a liquid solution of polymer(s)+solute dissolved in acetone. Both techniques allowed the recovery of composite particles, but the semi-continuous operation yielded smaller and less aggregated populations than the batch operation. The release behaviour of acetazolamide from the prepared microparticles was studied and most products exhibited a slower release than the single drug. Moreover, the release could be controlled to some extent by varying the ratio of the two Eudragit used in the formulation and by selecting one or the other anti-solvent technique. Simple diffusion models satisfactorily described the release profiles. Composites specifically produced by semi-continuous technique have a drug release rate controlled by a diffusion mechanism, whereas for composites produced by the batch operation, the polymer swelling also contributes to the overall transport mechanism.

Hydrodynamically induced fluid transfer and non-convective double-diffusion in microgravity sliding solvent diffusion cells

NASA Technical Reports Server (NTRS)

Pollmann, Konrad W.; Stodieck, Louis S.; Luttges, Marvin W.

1994-01-01

Microgravity can provide a diffusion-dominated environment for double-diffusion and diffusion-reaction experiments otherwise disrupted by buoyant convection or sedimentation. In sliding solvent diffusion cells, a diffusion interface between two liquid columns is achieved by aligning two offset sliding wells. Fluid in contact with the sliding lid of the cavities is subjected to an applied shear stress. The momentum change by the start/stop action of the well creates an additional hydrodynamical force. In microgravity, these viscous and inertial forces are sufficiently large to deform the diffusion interface and induce hydrodynamic transfer between the wells. A series of KC-135 parabolic flight experiments were conducted to characterize these effects and establish baseline data for microgravity diffusion experiments. Flow visualizations show the diffusion interface to be deformed in a sinusoidal fashion following well alignment. After the wells were separated again in a second sliding movement, the total induced liquid transfer was determined and normalized by the well aspect ratio. The normalized transfer decreased linearly with Reynolds number from 3.3 to 4.0% (w/v) for Re = 0.4 (Stokes flow) to a minimum of 1.0% for Re = 23 to 30. Reynolds numbers that provide minimum induced transfers are characterized by an interface that is highly deformed and unsuitable for diffusion measurements. Flat diffusion interfaces acceptable for diffusion measurements are obtained with Reynolds numbers on the order of 7 to 10. Microgravity experiments aboard a sounding rocket flight verified counterdiffusion of different solutes to be diffusion dominated. Ground control experiments showed enhanced mixing by double-diffusive convection. Careful selection of experimental parameters improves initial conditions and minimizes induced transfer rates.

A surprising method for green extraction of essential oil from dry spices: Microwave dry-diffusion and gravity.

PubMed

Farhat, Asma; Fabiano-Tixier, Anne-Sylvie; Visinoni, Franco; Romdhane, Mehrez; Chemat, Farid

2010-11-19

Without adding any solvent or water, we proposed a novel and green approach for the extraction of secondary metabolites from dried plant materials. This "solvent, water and vapor free" approach based on a simple principle involves the application of microwave irradiation and earth gravity to extract the essential oil from dried caraway seeds. Microwave dry-diffusion and gravity (MDG) has been compared with a conventional technique, hydrodistillation (HD), for the extraction of essential oil from dried caraway seeds. Essential oils isolated by MDG were quantitatively (yield) and qualitatively (aromatic profile) similar to those obtained by HD, but MDG was better than HD in terms of rapidity (45min versus 300min), energy saving, and cleanliness. The present apparatus permits fast and efficient extraction, reduces waste, avoids water and solvent consumption, and allows substantial energy savings. Copyright © 2010 Elsevier B.V. All rights reserved.

Monitoring single-cell bioenergetics via the coarsening of emulsion droplets

PubMed Central

Boitard, L.; Cottinet, D.; Kleinschmitt, C.; Bremond, N.; Baudry, J.; Yvert, G.; Bibette, J.

2012-01-01

Microorganisms are widely used to generate valuable products, and their efficiency is a major industrial focus. Bioreactors are typically composed of billions of cells, and available measurements only reflect the overall performance of the population. However, cells do not equally contribute, and process optimization would therefore benefit from monitoring this intrapopulation diversity. Such monitoring has so far remained difficult because of the inability to probe concentration changes at the single-cell level. Here, we unlock this limitation by taking advantage of the osmotically driven water flux between a droplet containing a living cell toward surrounding empty droplets, within a concentrated inverse emulsion. With proper formulation, excreted products are far more soluble within the continuous hydrophobic phase compared to initial nutrients (carbohydrates and salts). Fast diffusion of products induces an osmotic mismatch, which further relaxes due to slower diffusion of water through hydrophobic interfaces. By measuring droplet volume variations, we can deduce the metabolic activity down to isolated single cells. As a proof of concept, we present the first direct measurement of the maintenance energy of individual yeast cells. This method does not require any added probes and can in principle apply to any osmotically sensitive bioactivity, opening new routes for screening, and sorting large libraries of microorganisms and biomolecules. PMID:22538813

Emulsification Of Eutectic Salt Mixtures In Fluid Vehicles

NASA Astrophysics Data System (ADS)

Vanderhoff, J. W.; El-Aasser, M. S.; Hawkins, T. W.

1988-05-01

High-internal-phase-volume emulsions of 75 volt 3/18/79 potassium iodide/sodium iodide/ urea model eutectic salt mixture in 83.5/16.5 Sartomer R-45HT hydroxy-terminated polybutadi-ene/Nujol mineral oil binder mixture were prepared at 60°C using water-in-oil emulsifiers and cured with isophorone diisocyanate or Desmodur N-100. The Nujol mineral oil enhanced the emulsification with a negligible reduction in the tensile properties of the cured elastomer. The average emulsion droplet sizes were ca. 200 nm initially, but increased slowly during curing to 500-1000 nm. The coalescence of the emulsion droplets followed the second-order dependence predicted by the von Smoluchowski diffusion-controlled flocculation; the rate constants were 1.05x10-18 and 9.58x10-18 cc/droplet-sec for dirnethyldioctadecylammonium bromide and Span 85 sorbitan trioleate, respectively. The isophorone diisocyanate reacted with emulsifiers containing primary hydroxyl or amine groups, to give unstable emulsions or no emulsions at all. Dimethyldioctadecylammonium bromide with no primary hydroxyl or amine groups, however, did not react with isocyanates and gave stable emulsions. The reaction of the R-45HT hydroxy-terminated polybutadiene with isophorone diisocyanate followed the expec-ted second-order kinetics with a rate constant of 3.42x10-4 liters/mole-sec at 60°C. The tensile properties of the cured elastomers and emulsions generally increased with increasing NCO/OH ratio up to 1.6/1.0. With increasing volume fraction of dispersed phase, the maximum stress (tensile strength) decreased, the maximum strain (percent elongation) increased, and the initial modulus (tensile modulus) decreased, in contrast to the behavior of conventional filled polymer systems; however, the maximum stresses were in accord with theoretical values for a filled polymer in which the filler particles bear no load, the initial moduli were in accord with the predictions of an isostrain model, and the maximum strain increased with in-creasing volume fraction of dispersed phase; these unusual variations, which were attributed to the liquid nature of the emulsion droplets, were used to estimate the elastomer proper-ties required to give the desired properties: 60-100 psi maximum stress, 80-150% maximum strain, and 500-2000 psi initial modulus for an 88/12 eutectic salt/crosslinked polybutadi-ene composite containing 20% aluminum particles. The addition of 20% aluminum particles gave a modest improvement in tensile properties, and the addition of 2.5% or 3.5% submicroscopic carbon black particles gave a greater improvement; however, the tensile properties were still slightly short of the desired properties.

Application of molecular dynamics simulations in molecular property prediction II: diffusion coefficient.

PubMed

Wang, Junmei; Hou, Tingjun

2011-12-01

In this work, we have evaluated how well the general assisted model building with energy refinement (AMBER) force field performs in studying the dynamic properties of liquids. Diffusion coefficients (D) have been predicted for 17 solvents, five organic compounds in aqueous solutions, four proteins in aqueous solutions, and nine organic compounds in nonaqueous solutions. An efficient sampling strategy has been proposed and tested in the calculation of the diffusion coefficients of solutes in solutions. There are two major findings of this study. First of all, the diffusion coefficients of organic solutes in aqueous solution can be well predicted: the average unsigned errors and the root mean square errors are 0.137 and 0.171 × 10(-5) cm(-2) s(-1), respectively. Second, although the absolute values of D cannot be predicted, good correlations have been achieved for eight organic solvents with experimental data (R(2) = 0.784), four proteins in aqueous solutions (R(2) = 0.996), and nine organic compounds in nonaqueous solutions (R(2) = 0.834). The temperature dependent behaviors of three solvents, namely, TIP3P water, dimethyl sulfoxide, and cyclohexane have been studied. The major molecular dynamics (MD) settings, such as the sizes of simulation boxes and with/without wrapping the coordinates of MD snapshots into the primary simulation boxes have been explored. We have concluded that our sampling strategy that averaging the mean square displacement collected in multiple short-MD simulations is efficient in predicting diffusion coefficients of solutes at infinite dilution. Copyright © 2011 Wiley Periodicals, Inc.

Diffusional Motion of Redox Centers in Carbonate Electrolytes

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

Han, Kee Sung; Rajput, Nav Nidhi; Wei, Xiaoliang

2014-09-14

Ferrocene (Fc) and N-(ferrocenylmethyl)-N,N-dimethyl-N-ethylammonium bistrifluoromethyl-sulfonimide (Fc1N112-TFSI) were dissolved in carbonate solvents and self diffusion coefficents (D) of solutes and solvents were measured by 1H and 19F pulsed field gradient (PFG) nuclear magnetic resonance (NMR) spectroscopy. The organic solvents were propylene carbonate (PC), ethyl methyl carbonate (EMC) and a ternary mixture that also includes ethylene carbonate (EC). Results from NMR studies over the temperature range of 0-50 °C and for various concentrations (0.25 - 1.7 M) of Fc1N112-TFSI are compared to values of D simulated with classical molecular dynamics (MD). The measured self-diffusion coefficients gradually decreased as the Fc1N112-TFSI concentration increasedmore » in all solvents. Since the peaks for the two ions (Fc1N212 and TFSI) are separated in one-dimensional NMR spectra, separate diffusion coefficients could be measured and DTFSI is larger than DFc1N112 in all samples measured. The EC, PC and EMC have the same D in the neat solvent mixture and when Fc is dissolved in EC/PC/EMC at a concentration of 0.2 M, probably due to the interactions between common carbonyl structures within EC, PC and EMC. A difference in D (DPC < DEC < DEMC), and both a higher Ea for translational motion and higher effective viscosity for PC in the mixture containing Fc1N112-TFSI reflect the interaction between PC and Fc1N112+, which is a relatively stronger interaction than that between Fc1N112+ and other solvent species. In the EC/PC/EMC solution that is saturated with Fc1N112-TFSI, we find that DPC = DEC = DEMC and Fc1N112+ and all components of the EC/PC/EMC solution have the same Ea for translational motion, while the ratio DEC/PC/EMC/DFc1N112+ is approximately 3. These results reflect the lack of available free volume for independent diffusion in the saturated solution. The Fc1N112+ transference numbers lie around 0.4 and increases slightly as the temperature is increased in the PC and EMC solvents. The trends observed for D from simulations are in good agreement with experimental results and provide molecular level understanding of the solvation structure of Fc1N112-TFSI dissolved in EC/PC/EMC.« less

Holographic Methods for the Investigation of Photophysical Properties.

DTIC Science & Technology

1983-04-22

terphenyl doped with 10- 3 mol/mol of pentacene . Obtaining k from decay curves as in * A -Fig. 14a and plotting k as a function of 02 (see Fig. 14b...translation diffusion of molecules in liquid solvents can be used to probe solute conformations, solvent-solute interactions and local solvent structure...eiion of 1.7omoAr WauW by TrArWAOn GFarinP So far, local heating by the absorption of the two interfering light pulses has not been taken into

Multi-residue method for determination of 58 pesticides, pharmaceuticals and personal care products in water using solvent demulsification dispersive liquid-liquid microextraction combined with liquid chromatography-tandem mass spectrometry.

PubMed

Caldas, Sergiane Souza; Rombaldi, Caroline; Arias, Jean Lucas de Oliveira; Marube, Liziane Cardoso; Primel, Ednei Gilberto

2016-01-01

A rapid and efficient sample pretreatment using solvent-based de-emulsification dispersive liquid-liquid microextraction (SD-DLLME) coupled with liquid chromatography-tandem mass spectrometry (LC-MS/MS) was studied for the extraction of 58 pharmaceuticals and personal care products (PPCPs) and pesticides from water samples. Type and volume of extraction and disperser solvents, pH, salt addition, amount of salt and type of demulsification solvent were evaluated. Limits of quantification (LOQ) in the range from 0.0125 to 1.25 µg L(-1) were reached, and linearity was in the range from the LOQ of each compound to 25 μg L(-1). Recoveries ranged from 60% to 120% for 84% of the compounds, with relative standard deviations lower than 29%. The proposed method demonstrated, for the first time, that sample preparation by SD-DLLME with determination by LC-MS/MS can be successfully used for the simultaneous extraction of 32 pesticides and 26 PPCPs from water samples. The entire procedure, including the extraction of 58 organic compounds from the aqueous sample solution and the breaking up of the emulsion after extraction with water, rather than with an organic solvent, was environmentally friendly. In addition, this technique was less expensive and faster than traditional techniques. Finally, the analytical method under study was successfully applied to the analysis of all 58 pesticides and PPCPs in surface water samples. Copyright © 2015 Elsevier B.V. All rights reserved.

Nevirapine Loaded Core Shell Gold Nanoparticles by Double Emulsion Solvent Evaporation: In vitro and In vivo Evaluation.

PubMed

Dalvi, Bhagyashree R; Siddiqui, Ejaz A; Syed, Asad S; Velhal, Shilpa M; Ahmad, Absar; Bandivdekar, Atmaram B; Devarajan, Padma V

2016-01-01

HIV/AIDS is a macrophage resident infection localized in the reticuloendothelial system and remote locations of brain and bone marrow. We present core shell nanoparticles of gold(AuNPs) and nevirapine(NVP) for targeted delivery to the multiple HIV reservoirs. The aim of the study was to design core shell NVP loaded AuNPs with high drug loading and to evaluate biodistribution of the nanoparticles in possible HIV reservoirs in vivo. A specific objective was to assess the possible synergy of AuNPs with NVP on anti-HIV activity in vitro. Core shell nanoparticles were prepared by double emulsion solvent evaporation method and characterized. Glyceryl monostearate-nevirapine-gold nanoparticles(GMS-NVP-AuNPs) revealed high entrapment efficiency (>70%), high loading (~40%), particle size <250 nm and zeta potential -35.9± 1.41mv and exhibited sustained release with good stability. Surface plasmon resonance indicated shell formation while SEM coupled EDAX confirmed the presence of Au. TEM confirmed formation of spherical core shell nanoparticles. GMS-NVP-AuNPs revealed low hemolysis (<10 %) and serum stability upto 6 h. GMS-NVP-AuNPs exhibited rapid, high and sustained accumulation in the possible HIV reservoir organs, including the major organs of liver, spleen, lymph nodes, thymus and also remote locations of brain, ovary and bone marrow. High cell viability and enhanced uptake in PBMC's and TZM-bl cells were observed. While uptake in PBMC's proposed monocytes/macrophages enabled brain delivery. GMS-NVP-AuNPs demonstrated synergistic anti-HIV activity. The superior anti-HIV activity in vitro coupled with extensive localization of the nanoparticles in multiple HIV reservoirs suggests great promise of the core shell GMS-NVP-AuNPs for improved therapy of HIV.

Effect of Variation in Viscosity Grade of Ethycellulose on Theophylline Microcapsule Properties Prepared by Emulsion Solvent Evaporation.

PubMed

Garekani, Hadi Afrasiabi; Ahmadi, Behzad; Sadeghi, Fatemeh

2017-01-01

There are conflicting reports regarding the effect of polymer viscosity grade on microcapsule properties. The aim of the present study was to investigate the effect of just viscosity grade of ethylcellulose (EC) (not polymeric solution) on properties of theophylline microcapsules prepared by emulsion solvent evaporation. The effect of EC viscosity grade and drug:polymer ratio was investigated on microcapsule properties (yield, particle size, morphology, surface characteristics and drug release). Differential scanning calorimetry (DSC) and X-ray powder diffraction (XRD) were implemented to study the interaction and solid state of drug. The microcapsules were compressed in the presence of excipients and drug release was evaluated. The yield of microencapsulation and encapsulation efficiency at 1:1 drug:polymer ratio was dependent on EC viscosity. Microcapsules were spherical with some pores on their surfaces. The number of pores was more and their size was bigger for EC 100 cP microcapsules. Theophylline remained in crystalline form after encapsulation. DSC studies confirmed lack of interaction between drug and polymer. The drug release was rapid at 2:1 drug:polymer whilst it was slowed down at 1:1 drug:polymer ratio. Microcapsules obtained from EC 100 cP showed slightly faster drug release at latter ratio. Marginal changes in release rate were observed after compression of microcapsules. All viscosity grades of EC were able to sustain the release of the drug from microcapsules. Considering the similar release profiles for microcapsules prepared from different viscosities of EC, the use of lower viscosity grade of EC is recommended due to the ease of production and also less processing time. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

Injectable PolyMIPE Scaffolds for Soft Tissue Regeneration

PubMed Central

Moglia, Robert S.; Robinson, Jennifer L.; Muschenborn, Andrea D.; Touchet, Tyler J.; Maitland, Duncan J.; Cosgriff-Hernandez, Elizabeth

2013-01-01

Injury caused by trauma, burns, surgery, or disease often results in soft tissue loss leading to impaired function and permanent disfiguration. Tissue engineering aims to overcome the lack of viable donor tissue by fabricating synthetic scaffolds with the requisite properties and bioactive cues to regenerate these tissues. Biomaterial scaffolds designed to match soft tissue modulus and strength should also retain the elastomeric and fatigue-resistant properties of the tissue. Of particular design importance is the interconnected porous structure of the scaffold needed to support tissue growth by facilitating mass transport. Adequate mass transport is especially true for newly implanted scaffolds that lack vasculature to provide nutrient flux. Common scaffold fabrication strategies often utilize toxic solvents and high temperatures or pressures to achieve the desired porosity. In this study, a polymerized medium internal phase emulsion (polyMIPE) is used to generate an injectable graft that cures to a porous foam at body temperature without toxic solvents. These poly(ester urethane urea) scaffolds possess elastomeric properties with tunable compressive moduli (20–200 kPa) and strengths (4–60 kPa) as well as high recovery after the first conditioning cycle (97–99%). The resultant pore architecture was highly interconnected with large voids (0.5–2 mm) from carbon dioxide generation surrounded by water-templated pores (50–300 μm). The ability to modulate both scaffold pore architecture and mechanical properties by altering emulsion chemistry was demonstrated. Permeability and form factor were experimentally measured to determine the effects of polyMIPE composition on pore interconnectivity. Finally, initial human mesenchymal stem cell (hMSC) cytocompatibility testing supported the use of these candidate scaffolds in regenerative applications. Overall, these injectable polyMIPE foams show strong promise as a biomaterial scaffold for soft tissue repair. PMID:24563552

Grounding electrode and method of reducing the electrical resistance of soils

DOEpatents

Koehmstedt, Paul L.

1980-01-01

A first solution of an electrolyte is injected underground into a volume of soil having negative surface charges on its particles. A cationic surfactant suspended in this solution neutralizes these surface charges of the soil particles within the volume. Following the first solution, a cationic asphalt emulsion suspended in a second solution is injected into the volume. The asphalt emulsion diffuses through the volume and electrostatically bonds with additional soil surrounding the volume such that an electrically conductive water repellant shell enclosing the volume is formed. This shell prevents the leaching of electrolyte from the volume into the additional soil. The second solution also contains a dissolved deliquescent salt which draws water into the volume prior to the formation of the shell. When electrically connected to an electrical installation such as a power line tower, the volume constitutes a grounding electrode for the tower.

Assessment of extracts of Helichrysum arenarium, Crataegus monogyna, Sambucus nigra in photoprotective UVA and UVB; photostability in cosmetic emulsions.

PubMed

Jarzycka, Anna; Lewińska, Agnieszka; Gancarz, Roman; Wilk, Kazimiera A

2013-11-05

The aim of our study was to investigate the photoprotective activity and photostability efficacy of sunscreen formulations containing Helichrysum arenarium, Sambucus nigra, Crataegus monogyna extracts and their combination. UV transmission of the emulsion films was performed by using diffuse transmittance measurements coupling to an integrating sphere. In vitro photoprotection and photostability efficacy were evaluated according to the following parameters: sun protection factor (SPF), UVA protection factor (PF-UVA), UVA/UVB ratio and critical wavelength (λc) before and after UV irradiation. The results obtained show that the formulations containing polyphenols fulfill the official requirements for sunscreen products due to their broad spectrum of UV protection combined with their high photostability and remarkable antioxidant properties. Therefore H. arenarium, S. nigra, C. monogyna extracts represent useful additives for cosmetic formulation. Copyright © 2013 Elsevier B.V. All rights reserved.

Preparation of cerium halide solvate complexes

DOEpatents

Vasudevan, Kalyan V; Smith, Nickolaus A; Gordon, John C; McKigney, Edward A; Muenchaussen, Ross E

2013-08-06

Crystals of a solvated cerium(III) halide solvate complex resulted from a process of forming a paste of a cerium(III) halide in an ionic liquid, adding a solvent to the paste, removing any undissolved solid, and then cooling the liquid phase. Diffusing a solvent vapor into the liquid phase also resulted in crystals of a solvated cerium(III) halide complex.

Simple liquid models with corrected dielectric constants

PubMed Central

Fennell, Christopher J.; Li, Libo; Dill, Ken A.

2012-01-01

Molecular simulations often use explicit-solvent models. Sometimes explicit-solvent models can give inaccurate values for basic liquid properties, such as the density, heat capacity, and permittivity, as well as inaccurate values for molecular transfer free energies. Such errors have motivated the development of more complex solvents, such as polarizable models. We describe an alternative here. We give new fixed-charge models of solvents for molecular simulations – water, carbon tetrachloride, chloroform and dichloromethane. Normally, such solvent models are parameterized to agree with experimental values of the neat liquid density and enthalpy of vaporization. Here, in addition to those properties, our parameters are chosen to give the correct dielectric constant. We find that these new parameterizations also happen to give better values for other properties, such as the self-diffusion coefficient. We believe that parameterizing fixed-charge solvent models to fit experimental dielectric constants may provide better and more efficient ways to treat solvents in computer simulations. PMID:22397577

Doxycycline delivery from PLGA microspheres prepared by a modified solvent removal method.

PubMed

Patel, Roshni S; Cho, Daniel Y; Tian, Cheng; Chang, Amy; Estrellas, Kenneth M; Lavin, Danya; Furtado, Stacia; Mathiowitz, Edith

2012-01-01

We report on the development of a modified solvent removal method for the encapsulation of hydrophilic drugs within poly(lactic-co-glycolic acid) (PLGA). Using a water/oil/oil double emulsion, hydrophilic doxycycline was encapsulated within PLGA spheres with particle diameters ranging from approximately 600 nm to 19 µm. Encapsulation efficiencies of up to 74% were achieved for theoretical loadings from 1% to 10% (w/w), with biphasic release over 85 days with nearly complete release at the end of this time course. About 1% salt was added to the formulations to examine its effects on doxycycline release; salt modulated release only by increasing the magnitude of initial release without altering kinetics. Fourier transform infrared spectroscopy indicated no characteristic differences between doxycycline-loaded and control spheres. Differential scanning calorimetry and X-ray diffraction suggest that there may be a molecular dispersion of the doxycycline within the spheres and the doxycycline may be in an amorphous state, which could explain the slow, prolonged release of the drug.

Safety assessment of propylene glycol, tripropylene glycol, and PPGs as used in cosmetics.

PubMed

Fiume, Monice M; Bergfeld, Wilma F; Belsito, Donald V; Hill, Ronald A; Klaassen, Curtis D; Liebler, Daniel; Marks, James G; Shank, Ronald C; Slaga, Thomas J; Snyder, Paul W; Andersen, F Alan

2012-01-01

Propylene glycol is an aliphatic alcohol that functions as a skin conditioning agent, viscosity decreasing agent, solvent, and fragrance ingredient in cosmetics. Tripropylene glycol functions as a humectant, antioxidant, and emulsion stabilizer. Polypropylene glycols (PPGs), including PPG-3, PPG-7, PPG-9, PPG-12, PPG-13, PPG-15, PPG-16, PPG-17, PPG-20, PPG-26, PPG-30, PPG-33, PPG-34, PPG-51, PPG-52, and PPG-69, function primarily as skin conditioning agents, with some solvent use. The majority of the safety and toxicity information presented is for propylene glycol (PG). Propylene glycol is generally nontoxic and is noncarcinogenic. Clinical studies demonstrated an absence of dermal sensitization at use concentrations, although concerns about irritation remained. The CIR Expert Panel determined that the available information support the safety of tripropylene glycol as well as all the PPGs. The Expert Panel concluded that PG, tripropylene glycol, and PPGs ≥3 are safe as used in cosmetic formulations when formulated to be nonirritating.

Fast internal dynamics in alcohol dehydrogenase

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

Monkenbusch, M.; Stadler, A., E-mail: a.stadler@fz-juelich.de; Biehl, R.

2015-08-21

Large-scale domain motions in alcohol dehydrogenase (ADH) have been observed previously by neutron spin-echo spectroscopy (NSE). We have extended the investigation on the dynamics of ADH in solution by using high-resolution neutron time-of-flight (TOF) and neutron backscattering (BS) spectroscopy in the incoherent scattering range. The observed hydrogen dynamics were interpreted in terms of three mobility classes, which allowed a simultaneous description of the measured TOF and BS spectra. In addition to the slow global protein diffusion and domain motions observed by NSE, a fast internal process could be identified. Around one third of the protons in ADH participate in themore » fast localized diffusive motion. The diffusion coefficient of the fast internal motions is around two third of the value of the surrounding D{sub 2}O solvent. It is tempting to associate the fast internal process with solvent exposed amino acid residues with dangling side chains.« less

Influence of the oil globule fraction on the release rate profiles from multiple W/O/W emulsions.

PubMed

Bonnet, Marie; Cansell, Maud; Placin, Frédéric; Monteil, Julien; Anton, Marc; Leal-Calderon, Fernando

2010-06-15

Water-in-oil-in-water (W/O/W) double emulsions were prepared and the kinetics of release of magnesium ions from the internal to the external water phase was investigated as a function of the formulation and the globule volume fraction. All the emulsions were formulated using the same surface-active species (polyglycerol polyricinoleate and sodium caseinate). Also, the internal droplet and oil globule diameters were almost identical for all the systems. Two types of W/O/W emulsions were prepared based either on a synthetic oil (miglyol) or on an edible oil (olive oil). The globule volume fraction varied from 11% to 72%. At constant temperature (T=25 degrees C) and irrespective of the oil type, the percentage of magnesium released was lowered by increasing the globule fraction. In all cases, magnesium leakage occurred without film rupturing (no coalescence). Thus, the experimental data were interpreted within the frame of a model based on diffusion. The rate of release was determined by the permeation coefficient of magnesium across the oil phase and by the binding (chelation) of magnesium by caseinate molecules. The data could be adequately fitted by considering a time-dependant permeation coefficient. The better retention of magnesium at high globule fractions could account for two distinct phenomena: (i) the reduction of the relative volume of the outer phase, and (ii) the attenuation of the permeation coefficient over time induced by interfacial magnesium binding, all the more important than the globule fraction increased. Copyright 2010 Elsevier B.V. All rights reserved.

Numerical Analysis of Transient Temperature Response of Soap Film

NASA Astrophysics Data System (ADS)

Tanaka, Seiichi; Tatesaku, Akihiro; Dantsuka, Yuki; Fujiwara, Seiji; Kunimine, Kanji

2015-11-01

Measurements of thermophysical properties of thin liquid films are important to understand interfacial phenomena due to film structures composed of amphiphilic molecules in soap film, phospholipid bilayer of biological cell and emulsion. A transient hot-wire technique for liquid films less than 1 \\upmu m thick such as soap film has been proposed to measure the thermal conductivity and diffusivity simultaneously. Two-dimensional heat conduction equations for a solid cylinder with a liquid film have been solved numerically. The temperature of a thin wire with liquid film increases steeply with its own heat generation. The feasibility of this technique is verified through numerical experiments for various thermal conductivities, diffusivities, and film thicknesses. Calculated results indicate that the increase in the volumetric average temperature of the thin wire sufficiently varies with the change of thermal conductivity and diffusivity of the soap film. Therefore, the temperature characteristics could be utilized to evaluate both the thermal conductivity and diffusivity using the Gauss-Newton method.

Understanding Solvent Manipulation of Morphology in Bulk-Heterojunction Organic Solar Cells.

PubMed

Chen, Yuxia; Zhan, Chuanlang; Yao, Jiannian

2016-10-06

Film morphology greatly influences the performance of bulk-heterojunction (BHJ)-structure-based solar cells. It is known that an interpenetrating bicontinuous network with nanoscale-separated donor and acceptor phases for charge transfer, an ordered molecular packing for exciton diffusion and charge transport, and a vertical compositionally graded structure for charge collection are prerequisites for achieving highly efficient BHJ organic solar cells (OSCs). Therefore, control of the morphology to obtain an ideal structure is a key problem. For this solution-processing BHJ system, the solvent participates fully in film processing. Its involvement is critical in modifying the nanostructure of BHJ films. In this review, we discuss the effects of solvent-related methods on the morphology of BHJ films, including selection of the casting solvent, solvent mixture, solvent vapor annealing, and solvent soaking. On the basis of a discussion on interaction strength and time between solvent and active materials, we believe that the solvent-morphology-performance relationship will be clearer and that solvent selection as a means to manipulate the morphology of BHJ films will be more rational. © 2016 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Aurora kinase inhibitors attached to iron oxide nanoparticles enhances inhibition of the growth of liver cancer cells

NASA Astrophysics Data System (ADS)

Zhang, Xiquan; Xie, Li; Zheng, Ming; Yao, Juan; Song, Lina; Chang, Weiwei; Zhang, Yu; Ji, Min; Gu, Ning; Zhan, Xi

2015-06-01

We have developed a novel Aurora kinase inhibitor (AKI) AM-005, an analogue of pan-AKI AT-9283. To improve the intracellular efficacy of AM-005 and AT-9283, we utilized magnetite nanoparticles (NPs) to deliver AM-005 and AT-9283 into human SMMC-7721 and HepG2 liver cancer cells. The drug-loaded NPs were prepared through quasi-emulsion solvent diffusion of magnetite NPs with AM-005 or AT-9283. The encapsulated drugs were readily released from NPs, preferentially at low pHs. Upon exposure, cancer cells effectively internalized drug-loaded NPs into lysosome-like vesicles, which triggered a series of cellular changes, including the formation of enlarged cytoplasm, the significant increase of membrane permeability, and the generation of reactive oxygen species (ROS). The increased ROS synthesis sustained over 72 h, whereas that in the cells treated with free-form drugs declined rapidly after 48 h. However, chemical sequestration of the iron core of NPs had a minor influence on the generation of intracellular ROS. On the other hand, uncoupling of AM-005 uptake with NP internalization into cells failed to induce ROS synthesis. Overall, our approach achieved two-fold increase in suppressing the viability of tumor cells in vitro and the growth of tumors in vivo. We conclude that magnetite NPs can be used as pH responsive nanocarriers that are able to improve the efficacy of AKIs.

A microscopy method for scanning transmission electron microscopy imaging of the antibacterial activity of polymeric nanoparticles on a biofilm with an ionic liquid.

PubMed

Takahashi, Chisato; Muto, Shunsuke; Yamamoto, Hiromitsu

2017-08-01

In this study, we developed a scanning transmission electron microscopy (STEM) method for imaging the antibacterial activity of organic polymeric nanoparticles (NPs) toward biofilms formed by Staphylococcus epidermidis bacterial cells, for optimizing NPs to treat biofilm infections. The combination of sample preparation method using a hydrophilic ionic liquid (IL) and STEM observation using the cooling holder eliminates the need for specialized equipment and techniques for biological sample preparation. The annular dark-field STEM results indicated that the two types of biodegradable poly-(DL-lactide-co-glycolide) (PLGA) NPs: PLGA modified with chitosan (CS), and clarithromycin (CAM)-loaded + CS-modified PLGA, prepared by emulsion solvent diffusion exhibited different antibacterial activities in nanoscale. To confirm damage to the sample during STEM observation, we observed the PLGA NPs and the biofilm treated with PLGA NPs by both the conventional method and the newly developed method. The optimized method allows microstructure of the biofilm treated with PLGA NPs to be maintained for 25 min at a current flow of 40 pA. The developed simple sample preparation method would be helpful to understand the interaction of drugs with target materials. In addition, this technique could contribute to the visualization of other deformable composite materials at the nanoscale level. © 2016 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater, 105B: 1432-1437, 2017. © 2016 Wiley Periodicals, Inc.

Evaluation of diffuse-illumination holographic cinematography in a flutter cascade

NASA Technical Reports Server (NTRS)

Decker, A. J.

1986-01-01

Since 1979, the Lewis Research Center has examined holographic cinematography for three-dimensional flow visualization. The Nd:YAG lasers used were Q-switched, double-pulsed, and frequency-doubled, operating at 20 pulses per second. The primary subjects for flow visualization were the shock waves produced in two flutter cascades. Flow visualization was by diffuse-illumination, double-exposure, and holographic interferometry. The performances of the lasers, holography, and diffuse-illumination interferometry are evaluated in single-window wind tunnels. The fringe-contrast factor is used to evaluate the results. The effects of turbulence on shock-wave visualization in a transonic flow are discussed. The depth of field for visualization of a turbulent structure is demonstrated to be a measure of the relative density and scale of that structure. Other items discussed are the holographic emulsion, tests of coherence and polarization, effects of windows and diffusers, hologram bleaching, laser configurations, influence and handling of specular reflections, modes of fringe localization, noise sources, and coherence requirements as a function of the pulse energy. Holography and diffuse illumination interferometry are also reviewed.

Homogenization Theory for the Prediction of Obstructed Solute Diffusivity in Macromolecular Solutions

PubMed Central

Donovan, Preston; Chehreghanianzabi, Yasaman; Rathinam, Muruhan; Zustiak, Silviya Petrova

2016-01-01

The study of diffusion in macromolecular solutions is important in many biomedical applications such as separations, drug delivery, and cell encapsulation, and key for many biological processes such as protein assembly and interstitial transport. Not surprisingly, multiple models for the a-priori prediction of diffusion in macromolecular environments have been proposed. However, most models include parameters that are not readily measurable, are specific to the polymer-solute-solvent system, or are fitted and do not have a physical meaning. Here, for the first time, we develop a homogenization theory framework for the prediction of effective solute diffusivity in macromolecular environments based on physical parameters that are easily measurable and not specific to the macromolecule-solute-solvent system. Homogenization theory is useful for situations where knowledge of fine-scale parameters is used to predict bulk system behavior. As a first approximation, we focus on a model where the solute is subjected to obstructed diffusion via stationary spherical obstacles. We find that the homogenization theory results agree well with computationally more expensive Monte Carlo simulations. Moreover, the homogenization theory agrees with effective diffusivities of a solute in dilute and semi-dilute polymer solutions measured using fluorescence correlation spectroscopy. Lastly, we provide a mathematical formula for the effective diffusivity in terms of a non-dimensional and easily measurable geometric system parameter. PMID:26731550

Effects of the internal friction and the solvent quality on the dynamics of a polymer chain closure.

PubMed

Yu, Wancheng; Luo, Kaifu

2015-03-28

Using 3D Langevin dynamics simulations, we investigate the effects of the internal friction and the solvent quality on the dynamics of a polymer chain closure. We show that the chain closure in good solvents is a purely diffusive process. By extrapolation to zero solvent viscosity, we find that the internal friction of a chain plays a non-ignorable role in the dynamics of the chain closure. When the solvent quality changes from good to poor, the mean closure time τc decreases by about 1 order of magnitude for the chain length 20 ≤ N ≤ 100. Furthermore, τc has a minimum as a function of the solvent quality. With increasing the chain length N, the minimum of τc occurs at a better solvent. Finally, the single exponential distributions of the closure time in poor solvents suggest that the negative excluded volume of segments does not alter the nearly Poisson statistical characteristics of the process of the chain closure.

In vitro permeation and in vivo anti-inflammatory and analgesic properties of nanoscaled emulsions containing ibuprofen for topical delivery

PubMed Central

Abdullah, Ghassan Z; Abdulkarim, Muthanna F; Salman, Ibrahim M; Ameer, Omar Z; Yam, Mun F; Mutee, Ahmed F; Chitneni, Mallikarjun; Mahdi, Elrashid S; Basri, Mahiran; Sattar, Munavvar A; Noor, Azmin M

2011-01-01

Introduction: As a topical delivery system, a nanoscaled emulsion is considered a good carrier of several active ingredients that convey several side effects upon oral administration, such as nonsteroidal anti-inflammatory drugs (NSAIDs). Objective: We investigated the in vitro permeation properties and the in vivo pharmacodynamic activities of different nanoscaled emulsions containing ibuprofen, an NSAID, as an active ingredient and newly synthesized palm olein esters (POEs) as the oil phase. Methodology: A ratio of 25:37:38 of oil phase:aqueous phase:surfactant was used, and different additives were used for the production of a range of nanoscaled emulsions. Carbopol® 940 dispersion neutralized by triethanolamine was employed as a rheology modifier. In some circumstances, menthol and limonene were employed at different concentrations as permeation promoters. All formulae were assessed in vitro using Franz diffusion cell fitted with full-thickness rat skin. This was followed by in vivo evaluation of the anti-inflammatory and analgesic activities of the promising formulae and comparison of the effects with that of the commercially available gel. Results and discussion: Among all other formulae, formula G40 (Carbopol® 940-free formula) had a superior ability in transferring ibuprofen topically compared with the reference. Carbopol® 940 significantly decreased the amount of drug transferred from formula G41 through the skin as a result of swelling, gel formation, and reduction in drug thermodynamic activity. Nonetheless, the addition of 10% w/w of menthol and limonene successfully overcame this drawback since, relative to the reference, higher amount of ibuprofen was transferred through the skin. By contrast, these results were relatively comparable to that of formula G40. Pharmacodynamically, the G40, G45, and G47 formulae exhibited the highest anti-inflammatory and analgesic effects compared with other formulae. Conclusion: The ingredients and the physical properties of the nanoscaled emulsions produced by using the newly synthesized POEs succeeded to deliver ibuprofen competently. PMID:21499428

Effect of emulsification on the skin permeation and UV protection of catechin.

PubMed

Yoshino, Sachie; Mitoma, Tomoaki; Tsuruta, Keiko; Todo, Hiroaki; Sugibayashi, Kenji

2014-06-01

An anti-aging effect may be obtained by skin application of tea catechins (Camellia sinensis) since they have high ultraviolet (UV)-protection activity. In this study, the skin permeation of catechin (C), epicatechin (EC), epigallocatechin (EGC), epicatechin gallate (ECg) and epigallocatechin gallate (EGCg) was determined and compared, and the effect of emulsification on the skin permeation of C was measured. The UV-protective effect of C was also determined. The in vitro skin permeability of each catechin derivative was determined using side-by-side diffusion of cells. The UV-protective effect of C was determined by applying different concentrations of C to the solution or emulsion on a three-dimensional cultured human skin model or normal human epidermal keratinocytes with UV-irradiation. ECg and EGCg with gallate groups showed lower skin permeability than C, EC and EGC without gallate groups, suggesting that the skin permeability of catechin derivatives may be dependent on the existence of a gallate group. Interestingly, the skin permeation of C was increased by an o/w emulsification. In addition, the C emulsion showed a significantly higher UV-protective effect by C than that with its aqueous solution. These results suggest that the o/w emulsion of catechin derivatives is probably useful as a cosmetic formulation with anti-aging efficacy.

Biodegradable microparticles based on poly(D,L-lactide) as a protective transport system in ruminant digestion.

PubMed

Jay, Steven M; Peevy, Nolan J; Jenkins, Thomas C; Burg, Karen J L

2006-01-01

Despite its abundance in their diet, cattle are unable to directly digest cellulose. The bovine digestive tract overcomes this problem via the rumen, a portion of the stomach containing mixed anaerobic bacteria. These microbes, while breaking down foodstuffs, also perform undesirable processes such as biohydrogenation, in which unsaturated fatty acids become saturated, with deleterious cardiovascular effects. An approach to preventing this saturation entailing the use of polymeric microspheres to encapsulate feed supplements is proposed, with a single emulsion, solvent evaporation method used to formulate poly(D,L-lactide) microparticles for delivery of unsaturated fatty acids to ruminant abomasum.

Human Health Concenrs of the Metalworking Fluid Components

NASA Astrophysics Data System (ADS)

Gerulová, Kristína; Buranská, Eva; Soldán, Maroš

2017-06-01

The exploration of 209 available Material safety data sheets of 85 straight oils, 46 emulsions, 51 semi-synthetics and 27 synthetics was carried out to provide a report on the most used components defined as dangerous substances. As many as 217 of different substances of which 15 were identified as biocides, 17 as corrosion inhibitors or neutralizing agent, 17 were lubricity improvers and 38 different base fluids, lubricity solvents or surfactants, while 93 substances were not identified specifically and 37 substances occurred only once. This article is focused on the list of biocides, neutralizing agents and corrosion inhibitors identified in all types of MWFs and their possible health effects.

Solvent extraction system for plutonium colloids and other oxide nano-particles

DOEpatents

Soderholm, Lynda; Wilson, Richard E; Chiarizia, Renato; Skanthakumar, Suntharalingam

2014-06-03

The invention provides a method for extracting plutonium from spent nuclear fuel, the method comprising supplying plutonium in a first aqueous phase; contacting the plutonium aqueous phase with a mixture of a dielectric and a moiety having a first acidity so as to allow the plutonium to substantially extract into the mixture; and contacting the extracted plutonium with second a aqueous phase, wherein the second aqueous phase has a second acidity higher than the first acidity, so as to allow the extracted plutonium to extract into the second aqueous phase. The invented method facilitates isolation of plutonium polymer without the formation of crud or unwanted emulsions.

BASIC STUDIES IN PERCUTANEOUS ABSORPTION.

DTIC Science & Technology

FATTY ACIDS, *SKIN(ANATOMY), ABSORPTION, ALKYL RADICALS, AMIDES, DIFFUSION, ELECTRON MICROSCOPY, HUMIDITY, LABORATORY ANIMALS, LIPIDS, ORGANIC SOLVENTS, PENETRATION, PRIVATION, PROTEINS, RATS, TEMPERATURE, WATER

Solvent evaporation induced graphene powder with high volumetric capacitance and outstanding rate capability for supercapacitors

NASA Astrophysics Data System (ADS)

Zhang, Xiaozhe; Raj, Devaraj Vasanth; Zhou, Xufeng; Liu, Zhaoping

2018-04-01

Graphene-based electrode materials for supercapacitors usually suffer from poor volumetric performance due to the low density. The enhancement of volumetric capacitance by densification of graphene materials, however, is usually accompanied by deterioration of rate capability, as the huge contraction of pore size hinders rapid diffusion of electrolytes. Thus, it is important to develop suitable pore size in graphene materials, which can sustain fast ion diffusion and avoid excessive voids to acquire high density simultaneously for supercapacitor applications. Accordingly, we propose a simple solvent evaporation method to control the pore size of graphene powders by adjusting the surface tension of solvents. Ethanol is used instead of water to reduce the shrinkage degree of graphene powder during solvent evaporation process, due to its lower surface tension comparing with water. Followed by the assistance of mechanical compression, graphene powder having high compaction density of 1.30 g cm-3 and a large proportion of mesopores in the pore size range of 2-30 nm is obtained, which delivers high volumetric capacitance of 162 F cm-3 and exhibits outstanding rate performance of 76% capacity retention at a high current density of 100 A g-1 simultaneously.

Absorption of ethanol, acetone, benzene and 1,2-dichloroethane through human skin in vitro: a test of diffusion model predictions

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

Gajjar, Rachna M.; Kasting, Gerald B., E-mail: Gerald.Kasting@uc.edu

The overall goal of this research was to further develop and improve an existing skin diffusion model by experimentally confirming the predicted absorption rates of topically-applied volatile organic compounds (VOCs) based on their physicochemical properties, the skin surface temperature, and the wind velocity. In vitro human skin permeation of two hydrophilic solvents (acetone and ethanol) and two lipophilic solvents (benzene and 1,2-dichloroethane) was studied in Franz cells placed in a fume hood. Four doses of each {sup 14}C-radiolabed compound were tested — 5, 10, 20, and 40 μL cm{sup −2}, corresponding to specific doses ranging in mass from 5.0 tomore » 63 mg cm{sup −2}. The maximum percentage of radiolabel absorbed into the receptor solutions for all test conditions was 0.3%. Although the absolute absorption of each solvent increased with dose, percentage absorption decreased. This decrease was consistent with the concept of a stratum corneum deposition region, which traps small amounts of solvent in the upper skin layers, decreasing the evaporation rate. The diffusion model satisfactorily described the cumulative absorption of ethanol; however, values for the other VOCs were underpredicted in a manner related to their ability to disrupt or solubilize skin lipids. In order to more closely describe the permeation data, significant increases in the stratum corneum/water partition coefficients, K{sub sc}, and modest changes to the diffusion coefficients, D{sub sc}, were required. The analysis provided strong evidence for both skin swelling and barrier disruption by VOCs, even by the minute amounts absorbed under these in vitro test conditions. - Highlights: • Human skin absorption of small doses of VOCs was measured in vitro in a fume hood. • The VOCs tested were ethanol, acetone, benzene and 1,2-dichloroethane. • Fraction of dose absorbed for all compounds at all doses tested was less than 0.3%. • The more aggressive VOCs absorbed at higher levels than diffusion model predictions. • We conclude that even small exposures to VOCs temporarily alter skin permeability.« less

Water-induced nanochannel networks in self-assembled block ionomers

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

Mineart, Kenneth P.; Al-Mohsin, Heba A.; Lee, Byeongdu

2016-03-07

Block ionomers cast from solution exhibit solvent-templated morphologies that can be altered by solvent-vapor annealing. When cast from a mixed solvent, a midblock-sulfonated pentablock ion- omer self-assembles into spherical ionic microdomains that are loosely connected. Upon exposure to liquid water, nanoscale channels irreversibly develop between the microdomains due to swelling and form a continuous mesoscale network. We use electron tomography and real-time X-ray scat- tering to follow this transformation and show that the resultant morphology provides a highly effec- tive diffusive pathway.

Carbon nanotube balls and their application in supercapacitors.

PubMed

Kang, Da-Young; Moon, Jun Hyuk

2014-01-08

We have provided a design of the macroscopic morphology of carbon nanotubes (CNTs) using emulsion droplet confinement. The evaporation of CNT-dispersed aqueous emulsion droplets in oil produces spherical CNT assemblies, i.e., CNT balls. In this emulsion-assisted method, compact packing of CNT was obtained by the presence of capillary pressure during droplet evaporation. The size of the CNT balls could be controlled by changing the concentration of the CNT dispersion solution; typically, CNT balls with an average size in the range of 8-12 μm were obtained with a Brunauer-Emmett-Teller (BET) specific area of 200 m(2)/g. Heat treatment of the CNT balls, which was required to remove residual solvent, and cement CNTs was followed, and their effect has been characterized; the heat treatment at high temperature desorbed surface oxygenated groups of CNTs and created defective carbon structures, but did not change pore structure. The dispersion of CNT balls was applied to form CNT ball-assembled film for a supercapacitor electrode. The specific capacitance of 80 F/g was obtained at 500 °C heat treatment, but the CNT balls prepared at a higher temperature actually decreased the capacitance, because of the removal of surface oxygenated groups, thereby decreasing the pseudo-capacitance. The capacitive properties of CNT ball-assembled electrodes were compared to CNT films; the CNT ball electrodes showed 40% higher specific electrochemical capacitance and higher rate performance, which is attributed to the compact packing of CNTs in the CNT ball and the hierarchical porous structures in the ball assemblies.

Deposition of Methylammonium Lead Triiodide by Resonant Infrared Matrix-Assisted Pulsed Laser Evaporation

NASA Astrophysics Data System (ADS)

Barraza, E. Tomas; Dunlap-Shohl, Wiley A.; Mitzi, David B.; Stiff-Roberts, Adrienne D.

2018-02-01

Resonant infrared matrix-assisted pulsed laser evaporation (RIR-MAPLE) was used to deposit the metal-halide perovskite (MHP) CH3NH3PbI3 (methylammonium lead triiodide, or MAPbI), creating phase-pure films. Given the moisture sensitivity of these crystalline, multi-component organic-inorganic hybrid materials, deposition of MAPbI by RIR-MAPLE required a departure from the use of water-based emulsions as deposition targets. Different chemistries were explored to create targets that properly dissolved MAPbI components, were stable under vacuum conditions, and enabled resonant laser energy absorption. Secondary phases and solvent contamination in the resulting films were studied through Fourier transform infrared (FTIR) absorbance and x-ray diffraction (XRD) measurements, suggesting that lingering excess methylammonium iodide (MAI) and low-vapor pressure solvents can distort the microstructure, creating crystalline and amorphous non-perovskite phases. Thermal annealing of films deposited by RIR-MAPLE allowed for excess solvent to be evaporated from films without degrading the MAPbI structure. Further, it was demonstrated that RIR-MAPLE does not require excess MAI to create stoichiometric films with optoelectronic properties, crystal structure, and film morphology comparable to films created using more established spin-coating methods for processing MHPs. This work marks the first time a MAPLE-related technique was used to deposit MHPs.

Innovative approach to produce submicron drug particles by vibrational atomization spray drying: influence of the type of solvent and surfactant.

PubMed

Durli, T L; Dimer, F A; Fontana, M C; Pohlmann, A R; Beck, R C R; Guterres, S S

2014-08-01

Spray drying is a technique used to produce solid particles from liquid solutions, emulsions or suspensions. Buchi Labortechnik developed the latest generation of spray dryers, Nano Spray Dryer B-90. This study aims to obtain, directly, submicron drug particles from an organic solution, employing this equipment and using dexamethasone as a model drug. In addition, we evaluated the influence of both the type of solvent and surfactant on the properties of the powders using a 3(2) full factorial analysis. The particles were obtained with high yields (above 60%), low water content (below 2%) and high drug content (above 80%). The surface tension and the viscosity were strongly influenced by the type of solvent. The highest powder yields were obtained for the highest surface tension and the lowest viscosity of the drug solutions. The use of ionic surfactants led to higher process yields. The laser diffraction technique revealed that the particles deagglomerate into small ones with submicrometric size, (around 1 µm) that was also observed by scanning electron microscopy. Interaction between the raw materials in the spray-dried powders was verified by calorimetric analysis. Thus, it was possible to obtain dexamethasone submicrometric particles by vibrational atomization from organic solution.

Effect of Solvents on the Behavior of Lithium and Superoxide Ions in Lithium-Oxygen Battery Electrolytes.

PubMed

Smirnov, Vladimir S; Kislenko, Sergey A

2018-01-05

The molecular life of intermediates, namely, O 2 - and Li + , produced during the discharge of aprotic Li-O 2 batteries was investigated by molecular dynamics simulation. This work is of potential interest in the development of new electrolytes for Li-air batteries. We present the results on the structure and stability of the Li + and O 2 - solvation shells and the thermodynamics and kinetics of the ion-association reaction in solvents such as dimethyl sulfoxide (DMSO), dimethoxyethane (DME), and acetonitrile (ACN). The residence time of solvent molecules in the Li + solvation shell increases with the solvent donor number and is 100 times larger in DMSO than in ACN. In DMSO and DME, the Li + ion diffuses with its solvation shell as a whole. On the contrary, in ACN it diffuses as a "bare" ion because of weak solvation. The rate constant for the association of the lithium ion with the superoxide anion in DMSO is two orders of magnitude slower than that in ACN due to fact that the free-energy barrier is 2.5 times larger in DMSO than in ACN. In addition, we show that despite the strong dependence of the Li + shell stability on donor number, the rate of association does not necessarily correlate with this solvent property. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Direct measurement for organic solvents diffusion using ultra-sensitive optical resonator

NASA Astrophysics Data System (ADS)

Ali, Amir R.; Elias, Catherine M.

2017-06-01

In this paper, novel techniques using ultra-sensitive chemical optical sensor based on whispering gallery modes (WGM) are proposed through two different configurations. The first one will use a composite micro-sphere, when the solvent interacts with the polymeric optical sensors through diffusion the sphere start to swallow that solvent. In turn, that leads to change the morphology and mechanical properties of the polymeric spheres. Also, these changes could be measured by tracking the WGM shifts. Several experiments were carried out to study the solvent induced WGM shift using microsphere immersed in a solvent atmosphere. It can be potentially used for sensing the trace organic solvents like ethanol and methanol. The second configuration will use a composite beam nitrocellulose composite (NC) structure that acts as a sensing element. In this configuration, a beam is anchored to a substrate in one end, and the other end is compressing the polymeric sphere causing a shift in its WGM. When a chemical molecule is attached to the beam, the resonant frequency of the cantilever will be changed for a certain amount. By sensing this certain resonant frequency change, the existence of a single chemical molecule can be detected. A preliminary experimental model is developed to describe the vibration of the beam structure. The resonant frequency change of the cantilever due to attached mass is examined imperially using acetone as an example. Breath diagnosis can use this configuration in diabetic's diagnosis. Since, solvent like acetone concentration in human breath leads to a quick, convenient, accurate and painless breath diagnosis of diabetics. These micro-optical sensors have been examined using preliminary experiments to fully investigate its response. The proposed chemical sensor can achieve extremely high sensitivity in molecular level.

Fabrication, characterization, and thermal property evaluation of silver nanofluids

PubMed Central

2014-01-01

Silver nanoparticles were successfully prepared in two different solvents using a microwave heating technique, with various irradiation times. The silver nanoparticles were dispersed in polar liquids (distilled water and ethylene glycol) without any other reducing agent, in the presence of the stabilizer polyvinylpyrrolidone (PVP). The optical properties, thermal properties, and morphology of the synthesized silver particles were characterized using ultraviolet-visible spectroscopy, photopyroelectric technique, and transmission electron microscopy. It was found that for the both solvents, the effect of microwave irradiation was mainly on the particles distribution, rather than the size, which enabled to make stable and homogeneous silver nanofluids. The individual spherical nanostructure of self-assembled nanoparticles has been formed during microwave irradiation. Ethylene glycol solution, due to its special properties, such as high dielectric loss, high molecular weight, and high boiling point, can serve as a good solvent for microwave heating and is found to be a more suitable medium than the distilled water. A photopyroelectric technique was carried out to measure thermal diffusivity of the samples. The precision and accuracy of this technique was established by comparing the measured thermal diffusivity of the distilled water and ethylene glycol with values reported in the literature. The thermal diffusivity ratio of the silver nanofluids increased up to 1.15 and 1.25 for distilled water and ethylene glycol, respectively. PMID:25489293

Transport equations of electrodiffusion processes in the laboratory reference frame.

PubMed

Garrido, Javier

2006-02-23

The transport equations of electrodiffusion processes use three reference frames for defining the fluxes: Fick's reference in diffusion, solvent-fixed reference in transference numbers, and laboratory fluxes in electric conductivity. The convenience of using only one reference frame is analyzed here from the point of view of the thermodynamics of irreversible processes. A relation between the fluxes of ions and solvent and the electric current density is deduced first from a mass and volume balance. This is then used to show that (i) the laboratory and Fick's diffusion coefficients are identical and (ii) the transference numbers of both the solvent and the ion in the laboratory reference frame are related. Finally, four experimental methods for the measurement of ion transference numbers are analyzed critically. New expressions for evaluating transference numbers for the moving boundary method and the chronopotentiometry technique are deduced. It is concluded that the ion transport equation in the laboratory reference frame plays a key role in the description of electrodiffusion processes.

A review on methods of regeneration of spent pickling solutions from steel processing.

PubMed

Regel-Rosocka, Magdalena

2010-05-15

The review presents various techniques of regeneration of spent pickling solutions, including the methods with acid recovery, such as diffusion dialysis, electrodialysis, membrane electrolysis and membrane distillation, evaporation, precipitation and spray roasting as well as those with acid and metal recovery: ion exchange, retardation, crystallization solvent and membrane extraction. Advantages and disadvantages of the techniques are presented, discussed and confronted with the best available techniques requirements. Most of the methods presented meet the BAT requirements. The best available techniques are electrodialysis, diffusion dialysis and crystallization; however, in practice spray roasting and retardation/ion-exchange are applied most frequently for spent pickling solution regeneration. As "waiting for their chance" solvent extraction, non-dispersive solvent extraction and membrane distillation should be indicated because they are well investigated and developed. Environmental and economic benefits of the methods presented in the review depend on the cost of chemicals and wastewater treatment, legislative regulations and cost of modernization of existing technologies or implementation of new ones. Copyright (c) 2009 Elsevier B.V. All rights reserved.

Molecular and mesoscopic study of ionic liquids and their use as solvents of active agents released by polymeric vehicles

NASA Astrophysics Data System (ADS)

Ramos-Rodríguez, Daniel-Apolinar; Rodríguez-Hidalgo, María-del-Rosario; Soto-Figueroa, César; Vicente, Luis

2010-03-01

This work explores the diffusivity of the drug albendazole contained in a polymeric vehicle, Styrene-Divinylbenzene (ST-DVD), when it is subject to different environments. The environments consist of water and three different ionic liquids. First, the solubility parameters of these ionic liquids, [BMIM][PF6], [HMIM][Br] and [BMIM][BF4], and albendazole were evaluated by means of molecular dynamics employing COMPASS force-field and a NPT ensemble at 298 K. Then a mesoscopic simulation using Dissipative Particle Dynamics (DPD) was used. In the presence of ionic liquids the albendazole exhibits a diffusivity in [BMIM][PF6] around ten times that shown in [BMIM][BF4] or [HMIM][Br]. This is connected with the corresponding solvent power. The results obtained from these molecular and mesoscopic simulations are consistent with reported experimental results and are useful to predict and evaluate the solvent power of ionic liquids applied to drugs of pharmaceutical use.

Atomistic characterization of the active-site solvation dynamics of a model photocatalyst

DOE PAGES

van Driel, Tim B.; Kjær, Kasper S.; Hartsock, Robert W.; ...

2016-11-28

The interactions between the reactive excited state of molecular photocatalysts and surrounding solvent dictate reaction mechanisms and pathways, but are not readily accessible to conventional optical spectroscopic techniques. Here we report an investigation of the structural and solvation dynamics following excitation of a model photocatalytic molecular system [Ir 2(dimen) 4] 2+, where dimen is para-diisocyanomenthane. The time-dependent structural changes in this model photocatalyst, as well as the changes in the solvation shell structure, have been measured with ultrafast diffuse X-ray scattering and simulated with Born-Oppenheimer Molecular Dynamics. Both methods provide direct access to the solute–solvent pair distribution function, enabling themore » solvation dynamics around the catalytically active iridium sites to be robustly characterized. Our results provide evidence for the coordination of the iridium atoms by the acetonitrile solvent and demonstrate the viability of using diffuse X-ray scattering at free-electron laser sources for studying the dynamics of photocatalysis.« less

Behaviour of a solvent trapped in a physical molecular gel

NASA Astrophysics Data System (ADS)

Morfin, I.; Spagnoli, S.; Rambaud, C.; Longeville, S.; Plazanet, M.

2016-03-01

Physical gels formed by amphiphilic molecules, namely in this study Methyl-4,6-O-benzylidene-? -D-mannopyranoside, can be form either in polar and protic liquid-like water or in organic apolar solvent such as toluene. The solvent, that influences the supramolecular organization of the gelators, plays an important role in the stability and formation of the gel phase. Gelator-solvent interactions govern not only the assembly but also the solvent diffusion in the material. We present here measurements of neutron scattering (Time of Flight and Neutron Spin Echo) characterizing this microscopic behaviour. In addition, we show that transient grating spectroscopy provides valuable information through the characterization of the longitudinal acoustic wave propagating in the system. Opposite effects on the speed of sound in the gels are observed for the two solvents investigated, being relevant of the interactions between the gelators and the surrounding liquid.

Adsorption behavior of acetone solvent at the HMX crystal faces: A molecular dynamics study.

PubMed

Liu, Yingzhe; Yu, Tao; Lai, Weipeng; Ma, Yiding; Kang, Ying; Ge, Zhongxue

2017-06-01

Molecular dynamics simulations have been performed to understand the adsorption behavior of acetone (AC) solvent at the three surfaces of 1,3,5,7-tetranitro-1,3,5,7-tetraazacyclooctan (HMX) crystal, i.e. (011), (110), and (020) faces. The simulation results show that the structural features and electrostatic potentials of crystal faces are determined by the HMX molecular packing, inducing distinct mass density distribution, dipole orientation, and diffusion of solvent molecules in the interfacial regions. The solvent adsorption is mainly governed by the van der Waals forces, and the crystal-solvent interaction energies among three systems are ranked as (020)≈(110)>(011). The adsorption sites for solvent incorporation at the crystal surface were found and visualized with the aid of occupancy analysis. A uniform arrangement of adsorption sites is observed at the rough (020) surface as a result of ordered adsorption motif. Copyright © 2017 Elsevier Inc. All rights reserved.

Synchronization Dynamics of Coupled Chemical Oscillators

NASA Astrophysics Data System (ADS)

Tompkins, Nathan

The synchronization dynamics of complex networks have been extensively studied over the past few decades due to their ubiquity in the natural world. Prominent examples include cardiac rhythms, circadian rhythms, the flashing of fireflies, predator/prey population dynamics, mammalian gait, human applause, pendulum clocks, the electrical grid, and of the course the brain. Detailed experiments have been done to map the topology of many of these systems and significant advances have been made to describe the mathematics of these networks. Compared to these bodies of work relatively little has been done to directly test the role of topology in the synchronization dynamics of coupled oscillators. This Dissertation develops technology to examine the dynamics due to topology within networks of discrete oscillatory components. The oscillatory system used here consists of the photo-inhibitable Belousov-Zhabotinsky (BZ) reaction water-in-oil emulsion where the oscillatory drops are diffusively coupled to one another and the topology is defined by the geometry of the diffusive connections. Ring networks are created from a close-packed 2D array of drops using the Programmable Illumination Microscope (PIM) in order to test Turing's theory of morphogenesis directly. Further technology is developed to create custom planar networks of BZ drops in more complicated topologies which can be individually perturbed using illumination from the PIM. The work presented here establishes the validity of using the BZ emulsion system with a PIM to study the topology induced effects on the synchronization dynamics of coupled chemical oscillators, tests the successes and limitations of Turing's theory of morphogenesis, and develops new technology to further probe the effects of network topology on a system of coupled oscillators. Finally, this Dissertation concludes by describing ongoing experiments which utilize this new technology to examine topology induced transitions of synchronization dynamics of diffusively coupled chemical oscillators.

Fabrication of magnetic hydroxypropyl cellulose-g-poly(acrylic acid) porous spheres via Pickering high internal phase emulsion for removal of Cu(2+) and Cd(2.).

PubMed

Zhu, Yongfeng; Zheng, Yian; Zong, Li; Wang, Feng; Wang, Aiqin

2016-09-20

A series of magnetic hydroxypropyl cellulose-g-poly(acrylic acid) porous spheres were prepared via O/W Pickering high internal phase emulsions (HIPEs) integrated precipitation polymerization. The structure and composition of modified Fe3O4 and porous structures were characterized by TEM, XRD, TGA and SEM. The results indicated that the silanized Fe3O4 can influence greatly the pore structure of magnetic porous sphere in addition to non-negligible impacts of the proportion of mixed solvent and co-surfactant. The adsorption experiment demonstrated that the adsorption equilibrium can be reached within 40min and the maximal adsorption capacity was 300.00mg/g for Cd(2+) and 242.72mg/g for Cu(2+), suggesting its fast adsorption kinetics and high adsorption capacity. After five adsorption-desorption cycles, no significant changes in the adsorption capacity were observed, suggesting its excellent reusability. The magnetic porous sphere can be easily separated from the solution and then find its potential as a recyclable material for highly efficient removal of heavy metals. Copyright © 2016 Elsevier Ltd. All rights reserved.

Photocatalytic degradation of commercial phoxim over La-doped TiO2 nanoparticles in aqueous suspension.

PubMed

Dai, Ke; Peng, Tianyou; Chen, Hao; Liu, Juan; Zan, Lin

2009-03-01

Photocatalytic degradation of commercial phoxim emulsion in aqueous suspension was investigated by using La-doped mesoporous TiO2 nanoparticles (m-TiO2) as the photocatalyst under UV irradiation. Effects of La-doping level, calcination temperature, and additional amount of the photocatalyst on the photocatalytic degradation efficiency were investigated in detail. Experimental results indicate that 20 mg L(-1) phoxim in 0.5 g L(-1) La/m-TiO2 suspension (the initial pH 4.43) can be decomposed as prolonging the irradiation time. Almost 100% phoxim was decomposed after 4 h irradiation according to the spectrophotometric analyses, whereas the mineralization rate of phoxim just reached ca. 80% as checked by ion chromatography (IC) analyses. The elimination of the organic solvent in the phoxim emulsion as well as the formation and decomposition of some degradation intermediates were observed by high-performance liquid chromatography-mass spectroscopy (HPLC-MS). On the basis of the analysis results on the photocatalytic degradation intermediates, two possible photocatalytic degradation pathways are proposed under the present experimental conditions, which reveal that both the hydrolysis and adsorption of phoxim under UV light irradiation play important roles during the photocatalytic degradation of phoxim.

No Heat Spray Drying Technology

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

Beetz, Charles

No Heat Spray Drying Technology. ZoomEssence has developed our Zooming™ spray drying technology that atomizes liquids to powders at ambient temperature. The process of drying a liquid into a powder form has been traditionally achieved by mixing a heated gas with an atomized (sprayed) fluid within a vessel (drying chamber) causing the solvent to evaporate. The predominant spray drying process in use today employs air heated up to 400° Fahrenheit to dry an atomized liquid into a powder. Exposing sensitive, volatile liquid ingredients to high temperature causes molecular degradation that negatively impacts solubility, stability and profile of the powder. Inmore » short, heat is detrimental to many liquid ingredients. The completed award focused on several areas in order to advance the prototype dryer to a commercial scale integrated pilot system. Prior to the award, ZoomEssence had developed a prototype ‘no-heat’ dryer that firmly established the feasibility of the Zooming™ process. The award focused on three primary areas to improve the technology: (1) improved ability to formulate emulsions for specific flavor groups and improved understanding of the relationship of emulsion properties to final dry particle properties, (2) a new production atomizer, and (3) a dryer controls system.« less

Conservation of artists' acrylic emulsion paints: XPS, NEXAFS and ATR-FTIR studies of wet cleaning methods

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

Willneff, E. A.; Ormsby, B. A.; Stevens, J. S.

Works of art prepared with acrylic emulsion paints became commercially available in the 1960s. It is increasingly necessary to undertake and optimise cleaning and preventative conservation treatments to ensure their longevity. Model artists' acrylic paint films covered with artificial soiling were thus prepared on a canvas support and exposed to a variety of wet cleaning treatments based on aqueous or hydrocarbon solvent systems. This included some with additives such as chelating agents and/or surfactants, and microemulsion systems made specifically for conservation practice. The impact of cleaning (soiling removal) on the paint film surface was examined visually and correlated with resultsmore » of attenuated total reflection Fourier transform infrared, XPS and near-edge X-ray absorption fine structure analyses – three spectroscopic techniques with increasing surface sensitivity ranging from approximately $-$ 1000, 10 and 5 nm, respectively. Visual analysis established the relative cleaning efficacy of the wet cleaning treatments in line with previous results. X-ray spectroscopy analysis provided significant additional findings, including evidence for (i) surfactant extraction following aqueous swabbing, (ii) modifications to pigment following cleaning and (iii) cleaning system residues.« less

Preparation and in vitro evaluation of heparin-loaded polymeric nanoparticles.

PubMed

Jiao, Y Y; Ubrich, N; Marchand-Arvier, M; Vigneron, C; Hoffman, M; Maincent, P

2001-01-01

Nanoparticles of a highly soluble macromolecular drug, heparin, were formulated with two biodegradable polymers (poly-E-caprolactone [PCL] and poly (D, L-lactic-co-glycolic-acid) 50/50 [PLAGA]) and two nonbiodegradable positively charged polymers (Eudragit RS and RL) by the double emulsion and solvent evaporation method, using a high-pressure homogenization device. The encapsulation efficiency and heparin release profiles were studied as a function of the type of polymers employed (alone or in combination) and the concentration of heparin. Optimal encapsulation efficiency was observed when 5000 IU of heparin were incorporated in the first emulsion. High drug entrapment efficiency was observed in both Eudragit RS and RL nanoparticles (60% and 98%, respectively), compared with PLAGA and PCL nanoparticles (<14%). The use of the two types of Eudragit in combination with PCL and PLAGA increased the encapsulation efficiency compared with these two biodegradable polymers used alone; however, the in vitro drug release was not modified and remained low. On the other hand, the addition of esterase to the dissolution medium resulted in a significant increase in heparin release. The in vitro biological activity of released heparin, evaluated by measuring the anti-Xa activity by a colorimetric assay, was conserved after the encapsulation process.

Nano-based systems for oil spills control and cleanup.

PubMed

Avila, Antonio F; Munhoz, Viviane C; de Oliveira, Aline M; Santos, Mayara C G; Lacerda, Glenda R B S; Gonçalves, Camila P

2014-05-15

This paper reports the development of superhydrophobic nanocomposite systems which are also oleophilic. As hydrophobicity is based on low energy surface and surface roughness, the electrospinning technique was selected as the manufacturing technique. N,N' dimethylformamide (DMF) was employed as the polystyrene (PS) solvent. The "Tea-bag" (T-B) nanocomposite system is based on exfoliated graphite surrounded by PS superhydrophobic membranes. The T-B systems were tested regarding its adsorption and absorption rates. To test these properties, it was employed three different water/oil emulsions, i.e., new and used motor oil, which have physical properties (viscosity and specific gravity) similar to heavy crude oil extracted in Brazil, and vacuum pump oil (which does not form oil/water emulsion). It was observed that oil adsorption rate is dependent on oil surface tension, while the absorption rate is mainly dependent on membrane/exfoliated graphite surface area. Experimental data show that oil absorption rates ranged between 2.5g/g and 40g/g, while the adsorption rate oscillated from 0.32g/g/min to 0.80g/g/min. Furthermore, T-B systems were tested as containment barriers and sorbent materials with good results including its recyclability. Copyright © 2014 Elsevier B.V. All rights reserved.

High- and low-molecular-mass microbial surfactants.

PubMed

Rosenberg, E; Ron, E Z

1999-08-01

Microorganisms synthesize a wide variety of high- and low-molecular-mass bioemulsifiers. The low-molecular-mass bioemulsifiers are generally glycolipids, such as trehalose lipids, sophorolipids and rhamnolipids, or lipopeptides, such as surfactin, gramicidin S and polymyxin. The high-molecular-mass bioemulsifiers are amphipathic polysaccharides, proteins, lipopolysaccharides, lipoproteins or complex mixtures of these biopolymers. The low-molecular-mass bioemulsifiers lower surface and interfacial tensions, whereas the higher-molecular-mass bioemulsifiers are more effective at stabilizing oil-in-water emulsions. Three natural roles for bioemulsifiers have been proposed: (i) increasing the surface area of hydrophobic water-insoluble growth substrates; (ii) increasing the bioavailability of hydrophobic substrates by increasing their apparent solubility or desorbing them from surfaces; (iii) regulating the attachment and detachment of microorganisms to and from surfaces. Bioemulsifiers have several important advantages over chemical surfactants, which should allow them to become prominent in industrial and environmental applications. The potential commercial applications of bioemulsifiers include bioremediation of oil-polluted soil and water, enhanced oil recovery, replacement of chlorinated solvents used in cleaning-up oil-contaminated pipes, vessels and machinery, use in the detergent industry, formulations of herbicides and pesticides and formation of stable oil-in-water emulsions for the food and cosmetic industries.

Conservation of artists' acrylic emulsion paints: XPS, NEXAFS and ATR-FTIR studies of wet cleaning methods

DOE PAGES

Willneff, E. A.; Ormsby, B. A.; Stevens, J. S.; ...

2014-02-17

Works of art prepared with acrylic emulsion paints became commercially available in the 1960s. It is increasingly necessary to undertake and optimise cleaning and preventative conservation treatments to ensure their longevity. Model artists' acrylic paint films covered with artificial soiling were thus prepared on a canvas support and exposed to a variety of wet cleaning treatments based on aqueous or hydrocarbon solvent systems. This included some with additives such as chelating agents and/or surfactants, and microemulsion systems made specifically for conservation practice. The impact of cleaning (soiling removal) on the paint film surface was examined visually and correlated with resultsmore » of attenuated total reflection Fourier transform infrared, XPS and near-edge X-ray absorption fine structure analyses – three spectroscopic techniques with increasing surface sensitivity ranging from approximately $-$ 1000, 10 and 5 nm, respectively. Visual analysis established the relative cleaning efficacy of the wet cleaning treatments in line with previous results. X-ray spectroscopy analysis provided significant additional findings, including evidence for (i) surfactant extraction following aqueous swabbing, (ii) modifications to pigment following cleaning and (iii) cleaning system residues.« less

Nuclear magnetic resonance study of the conformation and dynamics of beta-casein at the oil/water interface in emulsions.

PubMed Central

ter Beek, L C; Ketelaars, M; McCain, D C; Smulders, P E; Walstra, P; Hemminga, M A

1996-01-01

A (13)C and (31)P nuclear magnetic resonance (NMR) study has been carried out on beta-casein adsorbed at the interface of a tetradecane/water emulsion. (13)C NMR spectra show signals from the carbonyl, carboxyl, aromatic, and C alpha carbons in beta-casein, well resolved from solvent resonances. Only a small fraction of all carbon atoms in beta-casein contribute to detectable signals; intensity measurements show that the observable spectrum is derived from about 30 to 40 amino acid residues.(31)P NMR spectra show signals from the five phosphoserines on the hydrophilic N-terminal part of the protein. Analysis of T(1) relaxation times of these nuclei, using the model free approach for the spectral density function and the line shape of the alpha-carbon region, indicates that a large part of the protein is in a random coil conformation with restricted motion and a relatively long internal correlation time. The NMR results show that the conformation and dynamics of the N-terminal part of beta-casein are not strongly altered at the oil/water interface, as compared to beta-casein in micelle-like aggregates in aqueous solution. PMID:9172765

Simple, rapid and, cost-effective fabrication of PDMS electrophoresis microchips using poly(vinyl acetate) as photoresist master.

PubMed

Lobo-Júnior, Eulício O; Gabriel, Ellen F M; Dos Santos, Rodrigo A; de Souza, Fabrício R; Lopes, Wanderson D; Lima, Renato S; Gobbi, Angelo L; Coltro, Wendell K T

2017-01-01

This study describes a simple, rapid, and cost-effective fabrication of PDMS electrophoresis microchips using poly(vinyl acetate) (PVAc) emulsion as photoresist master. High-relief microfluidic structures were defined on poly(vinyl acetate) previously deposited on printed circuit boards surfaces without cleanroom facilities and sophisticated instrumentation. After a UV exposure, channels with heights ranging from 30 to 140 μm were obtained by controlling the emulsion mass deposited on the master surface. The developing stage was performed using water rather than the organic solvents that are applied for conventional masks. The surface morphology was characterized by optical imaging, profilometry, and SEM. Based on the achieved results, the proposed method offers suitable reproducibility for the prototyping of electrophoresis microchips in PDMS. The feasibility of the resulting PDMS electrophoresis chips was successfully demonstrated with the separation of major inorganic cations within 100 s using a contactless conductivity detection system. The separation efficiencies ranged from ca. 67 900 to 125 600 plates/m. Due to the satisfactory performance and simplified instrumentation, we believe this fabrication protocol presents potential to be implemented in any chemical, biochemical, or biological laboratory. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Nonideality in diffusion of ionic and hydrophobic solutes and pair dynamics in water-acetone mixtures of varying composition.

PubMed

Gupta, Rini; Chandra, Amalendu

2007-07-14

We have performed a series of molecular dynamics simulations of water-acetone mixtures containing either an ionic solute or a neutral hydrophobic solute to study the extent of nonideality in the dynamics of these solutes with variation of composition of the mixtures. The diffusion coefficients of the charged solutes, both cationic and anionic, are found to change nonmonotonically with the composition of the mixtures showing strong nonideality of their dynamics. Also, the extent of nonideality in the diffusion of these charged solutes is found to be similar to the nonideality that is observed for the diffusion and orientational relaxation of water and acetone molecules in these mixtures which show a somewhat similar changes in the solvation characteristics of charged and dipolar solutes with changes of composition of water-acetone mixtures. The diffusion of the hydrophobic solute, however, shows a monotonic increase with increase of acetone concentration showing its different solvation characteristics as compared to the charged and dipolar solutes. The links between the nonideality in diffusion and solvation structures are further confirmed through calculations of the relevant solute-solvent and solvent-solvent radial distribution functions for both ionic and hydrophobic solutes. We have also calculated various pair dynamical properties such as the relaxation of water-water and acetone-water hydrogen bonds and residence dynamics of water molecules in water and acetone hydration shells. The lifetimes of both water-water and acetone-water hydrogen bonds and also the residence times of water molecules are found to increase steadily with increase in acetone concentration. No maximum or minimum was found in the composition dependence of these pair dynamical quantities. The lifetimes of water-water hydrogen bonds are always found to be longer than that of acetone-water hydrogen bonds in these mixtures. The residence times of water molecules are also found to follow a similar trend.

Air-assisted liquid-liquid microextraction by solidifying the floating organic droplets for the rapid determination of seven fungicide residues in juice samples.

PubMed

You, Xiangwei; Xing, Zhuokan; Liu, Fengmao; Zhang, Xu

2015-05-22

A novel air assisted liquid-liquid microextraction using the solidification of a floating organic droplet method (AALLME-SFO) was developed for the rapid and simple determination of seven fungicide residues in juice samples, using the gas chromatography with electron capture detector (GC-ECD). This method combines the advantages of AALLME and dispersive liquid-liquid microextraction based on the solidification of floating organic droplets (DLLME-SFO) for the first time. In this method, a low-density solvent with a melting point near room temperature was used as the extraction solvent, and the emulsion was rapidly formed by pulling in and pushing out the mixture of aqueous sample solution and extraction solvent for ten times repeatedly using a 10-mL glass syringe. After centrifugation, the extractant droplet could be easily collected from the top of the aqueous samples by solidifying it at a temperature lower than the melting point. Under the optimized conditions, good linearities with the correlation coefficients (γ) higher than 0.9959 were obtained and the limits of detection (LOD) varied between 0.02 and 0.25 μgL(-1). The proposed method was applied to determine the target fungicides in juice samples and acceptable recoveries ranged from 72.6% to 114.0% with the relative standard deviations (RSDs) of 2.3-13.0% were achieved. Compared with the conventional DLLME method, the newly proposed method will neither require a highly toxic chlorinated solvent for extraction nor an organic dispersive solvent in the application process; hence, it is more environmentally friendly. Copyright © 2015 Elsevier B.V. All rights reserved.

Charactrisation of particle assemblies by 3D cross correlation light scattering and diffusing wave spectroscopy

NASA Astrophysics Data System (ADS)

Scheffold, Frank

2014-08-01

To characterize the structural and dynamic properties of soft materials and small particles, information on the relevant mesoscopic length scales is required. Such information is often obtained from traditional static and dynamic light scattering (SLS/DLS) experiments in the single scattering regime. In many dense systems, however, these powerful techniques frequently fail due to strong multiple scattering of light. Here I will discuss some experimental innovations that have emerged over the last decade. New methods such as 3D static and dynamic light scattering (3D LS) as well as diffusing wave spectroscopy (DWS) can cover a much extended range of experimental parameters ranging from dilute polymer solutions, colloidal suspensions to extremely opaque viscoelastic emulsions.

What's new in the proton transfer reaction from pyranine to water? A femtosecond study of the proton transfer dynamics

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

Prayer, C.; Gustavsson, T.; Tran-Thi, T.-H.

1996-04-01

The proton transfer from excited pyranine to water is studied by the femtosecond fluorescence upconversion technique. It is shown for the first time that the proton transfer reaction in water proceeds by three successive steps: the solvent cage relaxation, the specific solute-solvent hydrogen-bond formation and finally the ion pair dissociation/diffusion.

Single molecule studies of solvent-dependent diffusion and entrapment in poly(dimethylsiloxane) thin films.

PubMed

Lange, Jeffrey J; Culbertson, Christopher T; Higgins, Daniel A

2008-12-15

Single molecule microscopic and spectroscopic methods are employed to probe the mobility and physical entrapment of dye molecules in dry and solvent-loaded poly(dimethylsiloxane) (PDMS) films. PDMS films of approximately 220 nm thickness are prepared by spin casting dilute solutions of Sylgard 184 onto glass coverslips, followed by low temperature curing. A perylene diimide dye (BPPDI) is used to probe diffusion and molecule-matrix interactions. Two classes of dye-loaded samples are investigated: (i) those incorporating dye dispersed throughout the films ("in film" samples) and (ii) those in which the dye is restricted primarily to the PDMS surface ("on film" samples). Experiments are performed under dry nitrogen and at various levels of isopropyl alcohol (IPA) loading from the vapor phase. A PDMS-coated quartz-crystal microbalance is employed to monitor solvent loading and drying of the PDMS and to ensure equilibrium conditions are achieved. Single molecules are shown to be predominantly immobile under dry conditions and mostly mobile under IPA-saturated conditions. Quantitative methods for counting the fluorescent spots produced by immobile single molecules in optical images of the samples demonstrate that the population of mobile molecules increases nonlinearly with IPA loading. Even under IPA saturated conditions, the population of fixed molecules is found to be greater than zero and is greatest for "in film" samples. Fluorescence correlation spectroscopy is used to measure the apparent diffusion coefficient for the mobile molecules, yielding a mean value of D = 1.4(+/-0.4) x 10(-8) cm(2)/s that is virtually independent of IPA loading and sample class. It is concluded that a nonzero population of dye molecules is physically entrapped within the PDMS matrix under all conditions. The increase in the population of mobile molecules under high IPA conditions is attributed to the filling of film micropores with solvent, rather than by incorporation of molecularly dispersed solvent into the PDMS.

Single-Molecule Tracking Study of the Permeability and Transverse Width of Individual Cylindrical Microdomains in Solvent-Swollen Polystyrene-block-poly(ethylene oxide) Films.

PubMed

Sapkota, Dol Raj; Tran-Ba, Khanh-Hoa; Elwell-Cuddy, Trevor; Higgins, Daniel A; Ito, Takashi

2016-12-01

Understanding the properties of solvent-swollen block copolymer (BCP) microdomains is important for better solvent-based control of microdomain morphology, orientation, and permeability. In this study, single-molecule tracking (SMT) was explored to assess the permeability and transverse width of individual cylindrical microdomains in solvent-swollen polystyrene-block-poly(ethylene oxide) (PS-b-PEO) films. PS-b-PEO films comprising shear-elongated cylindrical PEO microdomains were prepared by sandwiching its benzene or tetrahydrofuran (THF) solution between two glass substrates. SMT measurements were performed at different drying times to investigate the effects of solvent evaporation on the microdomain properties. SMT data showed one-dimensional (1D) motions of single fluorescent molecules (sulforhodamine B) based on their diffusion within the cylindrical microdomains. Microdomain permeability and transverse width were assessed from the single-molecule diffusion coefficients (D SMT ) and transverse variance of the 1D trajectories (σ δ 2 ), respectively. The D SMT and σ δ 2 values from individual 1D trajectories were widely distributed with no evidence of correlation on a single molecule basis, possibly because the individual microdomains in a film were swollen to different extents. On average, microdomain permeability (D) and effective radius (r) gradually decreased within the first 3 days of drying due to solvent evaporation, and changed negligibly thereafter. PS-b-PEO films prepared from THF solutions exhibited larger changes in D and r as compared with those from benzene solutions due to the better swelling of the PEO microdomains by THF. Importantly, changes in D were more prominent than those in r, suggesting that the permeability of the PEO microdomains is very susceptible to the presence of solvent. These results reveal the unique capability of SMT to assess the properties of individual cylindrical microdomains in a solvent-swollen BCP film.

Single-molecule tracking study of the permeability and transverse width of individual cylindrical microdomains in solvent-swollen polystyrene- block-poly(ethylene oxide) films

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

Sapkota, Dol Raj; Tran-Ba, Khanh-Hoa; Elwell-Cuddy, Trevor

Understanding the properties of solvent-swollen block copolymer (BCP) microdomains is important for better solvent-based control of microdomain morphology, orientation, and permeability. In this study, single-molecule tracking (SMT) was explored to assess the permeability and transverse width of individual cylindrical microdomains in solvent-swollen polystyrene- block-poly(ethylene oxide) (PS-b-PEO) films. PS-b-PEO films comprising shear-elongated cylindrical PEO microdomains were prepared by sandwiching its benzene or tetrahydrofuran (THF) solution between two glass substrates. In this paper, SMT measurements were performed at different drying times to investigate the effects of solvent evaporation on the microdomain properties. SMT data showed one-dimensional (1D) motions of single fluorescent moleculesmore » (sulforhodamine B) based on their diffusion within the cylindrical microdomains. Microdomain permeability and transverse width were assessed from the single-molecule diffusion coefficients (D SMT) and transverse variance of the 1D trajectories (σ δ 2), respectively. The D SMT and σ δ 2 values from individual 1D trajectories were widely distributed with no evidence of correlation on a single molecule basis, possibly because the individual microdomains in a film were swollen to different extents. On average, microdomain permeability (D) and effective radius (r) gradually decreased within the first 3 days of drying due to solvent evaporation, and changed negligibly thereafter. PS-b-PEO films prepared from THF solutions exhibited larger changes in D and r as compared with those from benzene solutions due to the better swelling of the PEO microdomains by THF. Importantly, changes in D were more prominent than those in r, suggesting that the permeability of the PEO microdomains is very susceptible to the presence of solvent. Finally, these results reveal the unique capability of SMT to assess the properties of individual cylindrical microdomains in a solvent-swollen BCP film.« less

Single-molecule tracking study of the permeability and transverse width of individual cylindrical microdomains in solvent-swollen polystyrene- block-poly(ethylene oxide) films

DOE PAGES

Sapkota, Dol Raj; Tran-Ba, Khanh-Hoa; Elwell-Cuddy, Trevor; ...

2016-11-04

Understanding the properties of solvent-swollen block copolymer (BCP) microdomains is important for better solvent-based control of microdomain morphology, orientation, and permeability. In this study, single-molecule tracking (SMT) was explored to assess the permeability and transverse width of individual cylindrical microdomains in solvent-swollen polystyrene- block-poly(ethylene oxide) (PS-b-PEO) films. PS-b-PEO films comprising shear-elongated cylindrical PEO microdomains were prepared by sandwiching its benzene or tetrahydrofuran (THF) solution between two glass substrates. In this paper, SMT measurements were performed at different drying times to investigate the effects of solvent evaporation on the microdomain properties. SMT data showed one-dimensional (1D) motions of single fluorescent moleculesmore » (sulforhodamine B) based on their diffusion within the cylindrical microdomains. Microdomain permeability and transverse width were assessed from the single-molecule diffusion coefficients (D SMT) and transverse variance of the 1D trajectories (σ δ 2), respectively. The D SMT and σ δ 2 values from individual 1D trajectories were widely distributed with no evidence of correlation on a single molecule basis, possibly because the individual microdomains in a film were swollen to different extents. On average, microdomain permeability (D) and effective radius (r) gradually decreased within the first 3 days of drying due to solvent evaporation, and changed negligibly thereafter. PS-b-PEO films prepared from THF solutions exhibited larger changes in D and r as compared with those from benzene solutions due to the better swelling of the PEO microdomains by THF. Importantly, changes in D were more prominent than those in r, suggesting that the permeability of the PEO microdomains is very susceptible to the presence of solvent. Finally, these results reveal the unique capability of SMT to assess the properties of individual cylindrical microdomains in a solvent-swollen BCP film.« less

Production, deformation and mechanical investigation of magnetic alginate capsules

NASA Astrophysics Data System (ADS)

Zwar, Elena; Kemna, Andre; Richter, Lena; Degen, Patrick; Rehage, Heinz

2018-02-01

In this article we investigated the deformation of alginate capsules in magnetic fields. The sensitivity to magnetic forces was realised by encapsulating an oil in water emulsion, where the oil droplets contained dispersed magnetic nanoparticles. We solved calcium ions in the aqueous emulsion phase, which act as crosslinking compounds for forming thin layers of alginate membranes. This encapsulating technique allows the production of flexible capsules with an emulsion as the capsule core. It is important to mention that the magnetic nanoparticles were stable and dispersed throughout the complete process, which is an important difference to most magnetic alginate-based materials. In a series of experiments, we used spinning drop techniques, capsule squeezing experiments and interfacial shear rheology in order to determine the surface Young moduli, the surface Poisson ratios and the surface shear moduli of the magnetically sensitive alginate capsules. In additional experiments, we analysed the capsule deformation in magnetic fields. In spinning drop and capsule squeezing experiments, water droplets were pressed out of the capsules at elevated values of the mechanical load. This phenomenon might be used for the mechanically triggered release of water-soluble ingredients. After drying the emulsion-filled capsules, we produced capsules, which only contained a homogeneous oil phase with stable suspended magnetic nanoparticles (organic ferrofluid). In the dried state, the thin alginate membranes of these particles were rather rigid. These dehydrated capsules could be stored at ambient conditions for several months without changing their properties. After exposure to water, the alginate membranes rehydrated and became flexible and deformable again. During this swelling process, water diffused back in the capsule. This long-term stability and rehydration offers a great spectrum of different applications as sensors, soft actuators, artificial muscles or drug delivery systems.

Kinetic Monte Carlo simulation of nanoparticle film formation via nanocolloid drying

NASA Astrophysics Data System (ADS)

Kameya, Yuki

2017-06-01

A kinetic Monte Carlo simulation of nanoparticle film formation via nanocolloid drying is presented. The proposed two-dimensional model addresses the dynamics of nanoparticles in the vertical plane of a drying nanocolloid film. The gas-liquid interface movement due to solvent evaporation was controlled by a time-dependent chemical potential, and the resultant particle dynamics including Brownian diffusion and aggregate growth were calculated. Simulations were performed at various Peclet numbers defined based on the rate ratio of solvent evaporation and nanoparticle diffusion. At high Peclet numbers, nanoparticles accumulated at the top layer of the liquid film and eventually formed a skin layer, causing the formation of a particulate film with a densely packed structure. At low Peclet numbers, enhanced particle diffusion led to significant particle aggregation in the bulk colloid, and the resulting film structure became highly porous. The simulated results showed some typical characteristics of a drying nanocolloid that had been reported experimentally. Finally, the potential of the model as well as the remaining challenges are discussed.

Solid lipid nanoparticles as carrier for sunscreens: in vitro release and in vivo skin penetration.

PubMed

Wissing, S A; Müller, R H

2002-06-17

The aim of this study was the comparison of two different formulations (solid lipid nanoparticles (SLN) and conventional o/w emulsion) as carrier systems for the molecular sunscreen oxybenzone. The influence of the carrier on the rate of release was studied in vitro with a membrane-free model. The release rate could be decreased by up to 50% with the SLN formulation. Further in vitro measurements with static Franz diffusion cells were performed. In vivo, penetration of oxybenzone into stratum corneum on the forearm was investigated by the tape stripping method. It was shown that the rate of release is strongly dependent upon the formulation and could be decreased by 30-60% in SLN formulations. In all test models, oxybenzone was released and penetrated into human skin more quickly and to a greater extent from the emulsions. The rate of release also depends upon the total concentration of oxybenzone in the formulation. In vitro-in vivo correlations could be made qualitatively.

The tetrapeptide N-acetyl-Pro-Pro-Tyr-Leu in skin care formulations-Physicochemical and release studies.

PubMed

Olejnik, Anna; Schroeder, Grzegorz; Nowak, Izabela

2015-08-15

Recently there has been a growth of interest in the novel skin care formulations containing active ingredients such as low molecular weight peptides. In this paper we present new skincare formulations such as hydrogels, oil-in-water emulsions and water-in-oil emulsion containing a tetrapeptide (N-acetyl-Pro-Pro-Tyr-Leu). These formulations were characterized in terms of physicochemical parameters (pH, viscosity), stability and particle size distribution. Additionally, the diffusion parameters of the peptide in the obtained formulations were calculated based on the Einstein-Smoluchowski equation. Furthermore, in order to determine the penetration of the tetrapeptide through membranes its release kinetics were investigated. On the basis of release curves, the release rate constants were determined. The results proved that the properties of the formulations strongly determined the release rate of the tetrapeptide. The higher viscosity of the semisolid, the slower was the permeation through the membrane. Copyright © 2015 Elsevier B.V. All rights reserved.

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

Ghosh, Soumya; Soudackov, Alexander V.; Hammes-Schiffer, Sharon

Electron transfer and proton coupled electron transfer (PCET) reactions at electrochemical interfaces play an essential role in a broad range of energy conversion processes. The reorganization energy, which is a measure of the free energy change associated with solute and solvent rearrangements, is a key quantity for calculating rate constants for these reactions. We present a computational method for including the effects of the double layer and ionic environment of the diffuse layer in calculations of electrochemical solvent reorganization energies. This approach incorporates an accurate electronic charge distribution of the solute within a molecular-shaped cavity in conjunction with a dielectricmore » continuum treatment of the solvent, ions, and electrode using the integral equations formalism polarizable continuum model. The molecule-solvent boundary is treated explicitly, but the effects of the electrode-double layer and double layer-diffuse layer boundaries, as well as the effects of the ionic strength of the solvent, are included through an external Green’s function. The calculated total reorganization energies agree well with experimentally measured values for a series of electrochemical systems, and the effects of including both the double layer and ionic environment are found to be very small. This general approach was also extended to electrochemical PCET and produced total reorganization energies in close agreement with experimental values for two experimentally studied PCET systems. This research was supported as part of the Center for Molecular Electrocatalysis, an Energy Frontier Research Center, funded by the U.S. Department of Energy, Office of Science, Office of Basic Energy Sciences.« less

Anion exchange membranes composed of a poly(2,6-dimethyl-1,4-phenylene oxide) random copolymer functionalized with a bulky phosphonium cation

DOE PAGES

Liu, Ye; Zhang, Bingzi; Kinsinger, Corey L.; ...

2016-01-22

A random copolymer, tris(2,4,6-trimethoxyphenyl) phosphonium functionalized poly(2,6-dimethyl-1,4-phenylene oxide) (PPO-TPQP) was cast from three different solvents: dimethyl sulfoxide (DMSO), ethyl lactate, or a 41:59 vol% mixture of DMSO and ethyl lactate. Solvents were selected via analysis of the Hansen solubility parameters to vary the phase separation of the polymer in the films. An optimized mixture of DMSO and ethyl lactate chosen for film fabrication and this film was contrasted with films cast from the neat constituent solvents. Atomic force microscopy identified domains from nanometer to tens of nanometer sizes, while the light microscopy showed features on the order of micron. SAXSmore » revealed a cation scattering peak with a d-spacing from 7 to 15 Å. Trends in conductivity and water diffusion for the membranes vary depending on the solvent from which they are cast. The mixed solvent cast membrane shows a linear Arrhenius behavior indicating fully dissociated cationic/anionic groups, and has the highest bromide conductivity of 3 mS/cm at 95% RH, 90 °C. The ethyl lactate cast membrane shows a linear Arrhenius relation in conductivity, but a Vogel-Tamman-Fulcher behavior in its water self-diffusion. While water increases bromide dissociation, water and bromide transport in these films seems to be decoupled. Lastly, this is particularly true for the film cast from ethyl lactate.« less

Anion exchange membranes composed of a poly(2,6-dimethyl-1,4-phenylene oxide) random copolymer functionalized with a bulky phosphonium cation

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

Liu, Ye; Zhang, Bingzi; Kinsinger, Corey L.

A random copolymer, tris(2,4,6-trimethoxyphenyl) phosphonium functionalized poly(2,6-dimethyl-1,4-phenylene oxide) (PPO-TPQP) was cast from three different solvents: dimethyl sulfoxide (DMSO), ethyl lactate, or a 41:59 vol% mixture of DMSO and ethyl lactate. Solvents were selected via analysis of the Hansen solubility parameters to vary the phase separation of the polymer in the films. An optimized mixture of DMSO and ethyl lactate chosen for film fabrication and this film was contrasted with films cast from the neat constituent solvents. Atomic force microscopy identified domains from nanometer to tens of nanometer sizes, while the light microscopy showed features on the order of micron. SAXSmore » revealed a cation scattering peak with a d-spacing from 7 to 15 A. Trends in conductivity and water diffusion for the membranes vary depending on the solvent from which they are cast. The mixed solvent cast membrane shows a linear Arrhenius behavior indicating fully dissociated cationic/anionic groups, and has the highest bromide conductivity of 3 mS/cm at 95% RH, 90 degrees C. The ethyl lactate cast membrane shows a linear Arrhenius relation in conductivity, but a Vogel-Tamman-Fulcher behavior in its water self-diffusion. While water increases bromide dissociation, water and bromide transport in these films seems to be decoupled. This is particularly true for the film cast from ethyl lactate.« less

Anion exchange membranes composed of a poly(2,6-dimethyl-1,4-phenylene oxide) random copolymer functionalized with a bulky phosphonium cation

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

Liu, Ye; Zhang, Bingzi; Kinsinger, Corey L.

A random copolymer, tris(2,4,6-trimethoxyphenyl) phosphonium functionalized poly(2,6-dimethyl-1,4-phenylene oxide) (PPO-TPQP) was cast from three different solvents: dimethyl sulfoxide (DMSO), ethyl lactate, or a 41:59 vol% mixture of DMSO and ethyl lactate. Solvents were selected via analysis of the Hansen solubility parameters to vary the phase separation of the polymer in the films. An optimized mixture of DMSO and ethyl lactate chosen for film fabrication and this film was contrasted with films cast from the neat constituent solvents. Atomic force microscopy identified domains from nanometer to tens of nanometer sizes, while the light microscopy showed features on the order of micron. SAXSmore » revealed a cation scattering peak with a d-spacing from 7 to 15 Å. Trends in conductivity and water diffusion for the membranes vary depending on the solvent from which they are cast. The mixed solvent cast membrane shows a linear Arrhenius behavior indicating fully dissociated cationic/anionic groups, and has the highest bromide conductivity of 3 mS/cm at 95% RH, 90 °C. The ethyl lactate cast membrane shows a linear Arrhenius relation in conductivity, but a Vogel-Tamman-Fulcher behavior in its water self-diffusion. While water increases bromide dissociation, water and bromide transport in these films seems to be decoupled. Lastly, this is particularly true for the film cast from ethyl lactate.« less

Oral insulin delivery by means of solid lipid nanoparticles

PubMed Central

Sarmento, Bruno; Martins, Susana; Ferreira, Domingos; Souto, Eliana B

2007-01-01

The aim of this work was to produce and characterize cetyl palmitate-based solid lipid nanoparticles (SLN) containing insulin, and to evaluate the potential of these colloidal carriers for oral administration. SLN were prepared by a modified solvent emulsification-evaporation method based on a w/o/w double emulsion. The particle size, zeta potential and association efficiency of unloaded and insulin-loaded SLN were determined and were found to be around 350 nm, negatively charged and the insulin association efficiency was over 43%. After oral administration of insulin-loaded SLN to diabetic rats, a considerable hypoglycemic effect was observed during 24 hours. These results demonstrated that SLN promote the oral absorption of insulin. PMID:18203440

Pharmacokinetics of intramuscular microparticle depot of valdecoxib in an experimental model.

PubMed

Agnihotri, Sagar M; Vavia, Pradeep R

2009-09-01

We did a prospective study to investigate pharmacokinetics of a single intramuscularly (i.m.) administered Valdecoxib (VC) polymeric microparticles in New Zealand white rabbits. Poly[lac(glc-leu)] microparticles encapsulating a potent cyclooxygenase-2- selective inhibitor, VC, were prepared by emulsion and solvent evaporation technique and administered i.m. to rabbits for pharmacokinetic study. A single i.m. dose of drug-loaded poly[lac(glc-leu)] microparticles resulted in sustained therapeutic drug levels in the plasma for 49 days. The relative bioavailability was increased severalfold as compared with unencapsulated drug. Injectable poly[lac(glc-leu)] microparticles hold promise for increasing drug bioavailability and reducing dosing frequency for better management of rheumatoid arthritis.

One-step fabrication of multifunctional micromotors.

PubMed

Gao, Wenlong; Liu, Mei; Liu, Limei; Zhang, Hui; Dong, Bin; Li, Christopher Y

2015-09-07

Although artificial micromotors have undergone tremendous progress in recent years, their fabrication normally requires complex steps or expensive equipment. In this paper, we report a facile one-step method based on an emulsion solvent evaporation process to fabricate multifunctional micromotors. By simultaneously incorporating various components into an oil-in-water droplet, upon emulsification and solidification, a sphere-shaped, asymmetric, and multifunctional micromotor is formed. Some of the attractive functions of this model micromotor include autonomous movement in high ionic strength solution, remote control, enzymatic disassembly and sustained release. This one-step, versatile fabrication method can be easily scaled up and therefore may have great potential in mass production of multifunctional micromotors for a wide range of practical applications.

Demulsification. [branched polyalkylene polyamines

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

Dickson, W.J.; Jenkins, F.W.

1966-07-05

A method of demulsification uses branched polyalkylene polyamines or their derivatives as demulsifiers for water-in-oil and oil-in-water emulsions. In addition to demulsification these products have a broad spectrum of uses. Among other uses are the following: (1) as corrosion inhibitors; (2) as fuel oil or lubricating oil additives; (3) as scale preventatives; (4) as acidizing additives; (5) as water-treating agents in waterflooding operations; (6) as mud additives; (7) as agents for the removal of mud filter cake from the walls of newly drilled wells; (8) as agents in paraffin solvents; (9) as additives in fracturing fluids; and (10) as agentsmore » in bactericides and fungicides. (8 claims)« less

Study on the disparate transition behaviors of the electrical/physical properties in PEDOT:PSS film depending on solvent species under a follow-up solution-treatment process

NASA Astrophysics Data System (ADS)

Yun, Dong-Jin; Kim, Jung-Hwa; Kim, Seong Heon; Seol, Minsu; Yu, DaEun; Kwon, Hyukju; Ham, Yongnam; Chung, JaeGwan; Kim, Yongsu; Heo, Sung

2016-04-01

In most solution-processed organic devices, a poly(3,4-ethylenedioxythiophene) (PEDOT) polymerized with poly(4-styrenesulfonate) (PSS) film is inevitably affected by various conditions during the subsequent solution-coating processes. To investigate the effects of direct solvent exposure on the properties of PEDOT polymerized with PSS (PEDOT:PSS) films, photoemission spectroscopy-based analytical methods were used before and after solvent-coating processes. Our results clearly indicate that PEDOT:PSS films undergo a different transition mechanism depending on the solubility of the solvent in water. The water-miscible solvents induce the solvation of hydrophilic PSS chains. As a result, this process allows the solvent to diffuse into the PEDOT:PSS film, and a conformational change between PEDOT and PSS occurs. On the other hand, the water-immiscible organic solvents cause the partial adsorption of solvent molecules at the PE surface, which leads to changes in the surface properties, including work function. Based on our finding, we demonstrate that the energy-level alignments at the organic semiconductor/electrode interface for the PEDOT:PSS films can be controlled by simple solvent treatments.

Frost Grape Polysaccharide (FGP), an Emulsion-Forming Arabinogalactan Gum from the Stems of Native North American Grape Species Vitis riparia Michx.

PubMed

Price, Neil P J; Vermillion, Karl E; Eller, Fred J; Vaughn, Steven F

2015-08-19

A new arabinogalactan is described that is produced in large quantity from the cut stems of the North American grape species Vitis riparia (Frost grape). The sugar composition consists of l-arabinofuranose (l-Araf, 55.2%) and d-galactopyranose (d-Galp 30.1%), with smaller components of d-xylose (11.2%), d-mannose (3.5%), and glucuronic acid (GlcA, ∼2%), the latter linked via a galactosyl residue. Permethylation identified 3-linked Galp residues, some substituted at the 2-position with Galp or Manp, terminal Araf and Xylp, and an internal 3-substituted Araf. NMR (HSQC, TOCSY, HMBC, DOSY) identified βGalp and three αAraf spin systems, in an Araf-α1,3-Araf-α1,2-Araf-α1,2-Galp structural motif. Diffusion-ordered NMR showed that the FGP has a molecular weight of 1-10 MDa. Unlike gum arabic, the FGP does not contain a hydroxyproline-rich protein (HPRP). FGP forms stable gels at >15% w/v and at 1-12% solutions are viscous and are excellent emulsifiers of flavoring oils (grapefruit, clove, and lemongrass), giving stable emulsions for ≥72 h. Lower concentrations (0.1% w/v) were less viscous, yet still gave stable grapefruit oil/water emulsions. Hence, FGP is a β1,3-linked arabinogalactan with potential as a gum arabic replacement in the food and beverage industries.

Addition of perfluorocarbons to alginate hydrogels significantly impacts molecular transport and fracture stress.

PubMed

White, Joseph C; Stoppel, Whitney L; Roberts, Susan C; Bhatia, Surita R

2013-02-01

Perfluorocarbons (PFCs) are used in biomaterial formulations to increase oxygen (O(2) ) tension and create a homogeneous O(2) environment in three-dimensional tissue constructs. It is unclear how PFCs affect mechanical and transport properties of the scaffold, which are critical for robustness, intracellular signaling, protein transport, and overall device efficacy. In this study, we investigate composite alginate hydrogels containing a perfluorooctyl bromide (PFOB) emulsion stabilized with Pluronic(®) F68 (F68). We demonstrate that PFC addition significantly affects biomaterial properties and performance. Solution and hydrogel mechanical properties and transport of representative hydrophilic (riboflavin), hydrophobic (methyl and ethyl paraben), and protein (bovine serum albumin, BSA) solutes were compared in alginate/F68 composite hydrogels with or without PFOB. Our results indicate that mechanical properties of the alginate/F68/PFOB hydrogels are not significantly affected under small strains, but a significant decrease fracture stress is observed. The effective diffusivity D(eff) of hydrophobic small molecules decreases with PFOB emulsion addition, yet the D(eff) of hydrophilic small molecules remained unaffected. For BSA, the D(eff) increased and the loading capacity decreased with PFOB emulsion addition. Thus, a trade-off between the desired increased O(2) supply provided by PFCs and the mechanical weakening and change in transport of cellular signals must be carefully considered in the design of biomaterials containing PFCs. Copyright © 2012 Wiley Periodicals, Inc.

Flexible continuous manufacturing platforms for solid dispersion formulations

NASA Astrophysics Data System (ADS)

Karry-Rivera, Krizia Marie

In 2013 16,000 people died in the US due to overdose from prescription drugs and synthetic narcotics. As of that same year, 90% of new molecular entities in the pharmaceutical drug pipeline are classified as poor water-soluble. The work in this dissertation aims to design, develop and validate platforms that solubilize weak acids and can potentially deter drug abuse. These platforms are based on processing solid dispersions via solvent-casting and hot-melt extrusion methods to produce oral transmucosal films and melt tablets. To develop these platforms, nanocrystalline suspensions and glassy solutions were solvent-casted in the form of films after physicochemical characterizations of drug-excipient interactions and design of experiment approaches. A second order model was fitted to the emulsion diffusion process to predict average nanoparticle size and for process optimization. To further validate the manufacturing flexibility of the formulations, glassy solutions were also extruded and molded into tablets. This process included a systematic quality-by-design (QbD) approach that served to identify the factors affecting the critical quality attributes (CQAs) of the melt tablets. These products, due to their novelty, lack discriminatory performance tests that serve as predictors to their compliance and stability. Consequently, Process Analytical Technology (PAT) tools were integrated into the continuous manufacturing platform for films. Near-infrared (NIR) spectroscopy, including chemical imaging, combined with deconvolution algorithms were utilized for a holistic assessment of the effect of formulation and process variables on the product's CQAs. Biorelevant dissolution protocols were then established to improve the in-vivo in-vitro correlation of the oral transmucosal films. In conclusion, the work in this dissertation supports the delivery of poor-water soluble drugs in products that may deter abuse. Drug nanocrystals ensured high bioavailability, while glassy solutions enabled drug solubilization in polymer matrices. PAT tools helped in characterizing the micro and macro structure of the product while also used as a control strategy for manufacturing. The systematic QbD assessment enabled identification of the variables that significantly affected melt tablet performance and their potential as an abuse deterrent product. Being that these glassy products are novel systems, biorelevant protocols for testing dissolution performance of films were also developed.

The effect of additives on release and in vitro skin retention of flavonoids from emulsion and gel semisolid formulations.

PubMed

Dyja, R; Jankowski, A

2017-08-01

To assess the effect of two different additives (propylene glycol (PG) and polyethylene glycol 400 (PEG 400)) on release and in vitro skin retention of quercetin and chrysin from semisolid bases (amphiphilic creams and acidic carbomer gels). For obtaining semisolid formulations, flavonoids were pre-dissolved in the liquid (PG or PEG 400) or directly suspended in the semisolid base. Three chrysin formulations ('cream 0', 'PG-cream' and 'PEG 400-cream') and five quercetin formulations ('cream 0', 'PG cream', 'PEG 400 cream', 'gel 0' and 'PG gel') were prepared. The release studies were carried out in Franz diffusion cells by means of a cellulose membrane. The porcine ear skin was used in in vitro skin retention studies. The dissolution was a prerequisite to increase the release rates of tested flavonoids from obtained semisolid formulations. The cumulative amount of chrysin released after 6 h from 'PEG 400 cream' containing partly dissolved form of that flavonoid was higher than that from 'cream 0' or 'PG cream' containing its suspended form. The formulations containing quercetin dissolved in PG ('PG cream', 'PG gel') or PEG 400 ('PEG 400 cream') exhibited higher release rates of that flavonoid than corresponding semisolid suspensions ('cream 0' or 'gel 0'). The effects of both liquid additives (PG and PEG 400) on the cumulative amount of quercetin released after 6 h were comparable. However, there was no correlation between the release rate and the skin retention. The amounts of the flavonoids found in the skin were strongly affected by the type of the used solvent. While PG increased the skin retention of both flavonoids, PEG 400 had no effect on chrysin skin retention and delayed quercetin skin absorption. The proper choice of the solvent added to the semisolid base is crucial for enhanced skin delivery of the tested flavonoids. PG is more efficient absorption promoter than PEG 400 of both chrysin and quercetin. © 2017 Society of Cosmetic Scientists and the Société Française de Cosmétologie.

Management of the diffusion of 4-methylumbelliferone across phases in microdroplet-based systems for in vitro protein evolution.

PubMed

Wu, Nan; Courtois, Fabienne; Zhu, Yonggang; Oakeshott, John; Easton, Chris; Abell, Chris

2010-09-01

Fluorongenic reagents based on 4-methylumbelliferone (4-MU) have been widely used for the detection of phosphatase, sulfatase, esterase, lipase and glycosidase activities in conventionally formatted enzyme assay systems. However, the sensitivity of assays based on these substrates is also potentially very useful in the microdroplet formats now being developed for high throughput in vitro evolution experiments. In this article, we report the investigation of diffusion of 4-MU as a model dye from water-in-oil droplets and the internal aqueous phase of water-in-oil-in-water droplets in microfluidics. The effect of BSA in the aqueous phase on the diffusion of 4-MU is also discussed. Based on these results, we provided here proof-of-concept of the reaction of the enzyme OpdA with the substrate coumaphos in water-in-oil-in-water droplets. In this double-emulsion system, the reaction of OpdA and coumaphos was achieved by allowing coumaphos to diffuse from the continuous aqueous phase across the oil phase into the internal aqueous droplets.

Application of liquid-liquid interactions with single-walled carbon nanotubes

NASA Astrophysics Data System (ADS)

Wang, Randy Kai-Wei

This study covers three important research topics related to the application of liquid-liquid interaction with single-walled carbon nanotubes (SWNTs). The first topic describes the removal of SWNT bundles from liquid suspensions of nanotubes. The key to this work includes the use of liquid-liquid interfaces to trap the SWNT bundles due to the free energy change of the system during the process. SWNTs pack into crystalline ropes that form bundles due to strong van der Waals attraction. Bundling diminishes mechanical and electronic properties because it could interrupt the electronic structure of the nanotubes. Also, the electronic devices based on as-grown nanotubes, which contains a mixture of individual nanotubes and nanotube bundles, make the electrical response unpredictable. We developed a new simple process to remove bundles by liquid-liquid interaction. SWNTs bundles are trapped at the interface because bundles stabilize the emulsions. Eliminating the use of ultracentrifugation to remove SWNT bundles enables large-scale production with reduced production costs and time savings. The second topic presented the swelling effect of the surfactant layer surrounding SWNTs with nonpolar solvents. Solvatochromic shifts in the absorbance and fluorescence spectra are observed when surfactant-stabilized aqueous SWNT suspensions are mixed with immiscible organic solvents. When aqueous surfactant-suspended SWNTs are mixed with certain solvents, the spectra closely match the peaks for SWNTs dispersed in only that solvent. These spectral changes suggest the hydrophobic region of the micelle surrounding SWNTs swells with the organic solvent when mixed. The solvatochromic shifts of the aqueous SWNT suspensions are reversible once the solvent evaporates. However, some surfactant-solvent systems show permanent changes to the fluorescence emission intensity after exposure to the organic solvent. The intensity of some large diameter SWNT (n, m) types increase by more than 175%. These differences are attributed to surfactant reorganization, which can improve nanotube coverage, resulting in decreased exposure to quenching mechanisms from the aqueous phase. The third topic describes the further study of the solvatochromism of the SWNTs. Since SWNTs are encapsulated with microenvironments of nonpolar solvents, it provides a new method to measure the photophysical properties of nanotubes in environments with known properties. Fluorescence and absorbance spectra of SWNTs show solvatochromic shifts in 16 nonpolar solvents, which are proportional to the solvent induction polarization. The photophysical properties of SWNTs were used to determine the relationship between the longitudinal polarizability and other nanotube properties, alpha11,|| ∝ 1/(R2E11 3). (Full text of this dissertation may be available via the University of Florida Libraries web site. Please check http://www.uflib.ufl.edu/etd.html)

A review: fabrication of porous polyurethane scaffolds.

PubMed

Janik, H; Marzec, M

2015-03-01

The aim of tissue engineering is the fabrication of three-dimensional scaffolds that can be used for the reconstruction and regeneration of damaged or deformed tissues and organs. A wide variety of techniques have been developed to create either fibrous or porous scaffolds from polymers, metals, composite materials and ceramics. However, the most promising materials are biodegradable polymers due to their comprehensive mechanical properties, ability to control the rate of degradation and similarities to natural tissue structures. Polyurethanes (PUs) are attractive candidates for scaffold fabrication, since they are biocompatible, and have excellent mechanical properties and mechanical flexibility. PU can be applied to various methods of porous scaffold fabrication, among which are solvent casting/particulate leaching, thermally induced phase separation, gas foaming, emulsion freeze-drying and melt moulding. Scaffold properties obtained by these techniques, including pore size, interconnectivity and total porosity, all depend on the thermal processing parameters, and the porogen agent and solvents used. In this review, various polyurethane systems for scaffolds are discussed, as well as methods of fabrication, including the latest developments, and their advantages and disadvantages. Copyright © 2014. Published by Elsevier B.V.

Light-responsive polymer microcapsules as delivery systems for natural active agents

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

Bizzarro, Valentina; Carfagna, Cosimo; Cerruti, Pierfrancesco

2016-05-18

In this work we report the preparation and the release behavior of UV-responsive polymeric microcapsules containing essential oils as a core. The oil acted also as a monomer solvent during polymerization. Accordingly, the potentially toxic organic solvent traditionally used was replaced with a natural active substance, resulting in a more sustainable functional system. Polymer shell was based on a lightly cross-linked polyamide containing UV-sensitive azobenzene moieties in the main chain. The micro-sized capsules were obtained via interfacial polycondensation in o/w emulsion, and their mean size was measured via Dynamic Light Scattering. Shape and morphology were analyzed through Scanning Electron andmore » Optical Microscopy. UV-responsive behavior was evaluated via spectrofluorimetry, by assessing the release kinetics of a fluorescent probe molecule upon UV light irradiation (λ{sub max}=360 nm). The irradiated samples showed an increase in fluorescence intensity, in accordance with the increase of the probe molecule concentration in the release medium. As for the un-irradiated sample, no changes could be detected demonstrating the effectiveness of the obtained releasing system.« less

Self-assembly of block copolymers into sieve-like particles with arrayed switchable channels and as scaffolds to guide the arrangement of gold nanoparticles.

PubMed

He, Yun; Zhang, Yan; Yan, Nan; Zhu, Yutian; Jiang, Wei; Shi, Dean

2017-10-12

Well-defined polymeric particles with not only a controllable shape and internal nanostructures but also stimuli-responsive functions have attracted intensive attention because of their great potential in various fields. Herein, we created unique sieve-like particles with lattice arrayed switchable channels via the confined self-assembly of poly(4-vinylpyridine)-b-polystyrene-b-poly(4-vinylpyridine) (P4VP-b-PS-b-P4VP) triblock copolymers within the emulsion droplets and the subsequent swelling treatment in ethanol. It is worth noting that the hexagonally packed P4VP channels in the sieve-like particles are switched on and off by changing the solvent type, i.e., P4VP channels are switched on in ethanol and switched off in water, which can operate as a solvent-controlled chemical gate. Moreover, the well-defined sieve-like particles can be further used as scaffolds to guide the spatial arrangement of gold nanoparticles, which generates hybrid nanomaterials with controllable morphology and ordered spatial arrangement of AuNPs.

Simultaneous microencapsulation of hydrophilic and lipophilic bioactives in liposomes produced by an ecofriendly supercritical fluid process.

PubMed

Tsai, Wen-Chyan; Rizvi, Syed S H

2017-09-01

Organic solvent residues are always a concern with the liposomes produced by traditional techniques. Our objectives were to encapsulate hydrophilic and lipophilic compounds in liposomes using a newly designed supercritical fluid process coupled with vacuum-driven cargo loading. Supercritical carbon dioxide was chosen as the phospholipid-dissolving medium and an ecofriendly substitute for organic solvents. Liposomal microencapsulation was conducted via a 1000-μm expansion nozzle at 12.41MPa, 90°C, and aqueous cargo loading rate of 0.25ml/s. Vitamins C and E were selected as model hydrophilic and lipophilic compounds encapsulated in the integrated liposomes. The average vesicle size was 951.02nm with a zeta potential of -51.87mV. The encapsulation efficiency attained was 32.97% for vitamin C and 99.32% for vitamin E. Good emulsion stability was maintained during storage at 4°C for 20days. Simultaneous microencapsulation in the liposomes was successfully achieved with this supercritical fluid process. Copyright © 2017 Elsevier Ltd. All rights reserved.

Cabazitaxel-loaded human serum albumin nanoparticles as a therapeutic agent against prostate cancer

PubMed Central

Qu, Na; Lee, Robert J; Sun, Yating; Cai, Guangsheng; Wang, Junyang; Wang, Mengqiao; Lu, Jiahui; Meng, Qingfan; Teng, Lirong; Wang, Di; Teng, Lesheng

2016-01-01

Cabazitaxel-loaded human serum albumin nanoparticles (Cbz-NPs) were synthesized to overcome vehicle-related toxicity of current clinical formulation of the drug based on Tween-80 (Cbz-Tween). A salting-out method was used for NP synthesis that avoids the use of chlorinated organic solvent and is simpler compared to the methods based on emulsion-solvent evaporation. Cbz-NPs had a narrow particle size distribution, suitable drug loading content (4.9%), and superior blood biocompatibility based on in vitro hemolysis assay. Blood circulation, tumor uptake, and antitumor activity of Cbz-NPs were assessed in prostatic cancer xenograft-bearing nude mice. Cbz-NPs exhibited prolonged blood circulation and greater accumulation of Cbz in tumors along with reduced toxicity compared to Cbz-Tween. Moreover, hematoxylin and eosin histopathological staining of organs revealed consistent results. The levels of blood urea nitrogen and serum creatinine in drug-treated mice showed that Cbz-NPs were less toxic than Cbz-Tween to the kidneys. In conclusion, Cbz-NPs provide a promising therapeutic for prostate cancer. PMID:27555767

A fully automated liquid–liquid extraction system utilizing interface detection

PubMed Central

Maslana, Eugene; Schmitt, Robert; Pan, Jeffrey

2000-01-01

The development of the Abbott Liquid-Liquid Extraction Station was a result of the need for an automated system to perform aqueous extraction on large sets of newly synthesized organic compounds used for drug discovery. The system utilizes a cylindrical laboratory robot to shuttle sample vials between two loading racks, two identical extraction stations, and a centrifuge. Extraction is performed by detecting the phase interface (by difference in refractive index) of the moving column of fluid drawn from the bottom of each vial containing a biphasic mixture. The integration of interface detection with fluid extraction maximizes sample throughput. Abbott-developed electronics process the detector signals. Sample mixing is performed by high-speed solvent injection. Centrifuging of the samples reduces interface emulsions. Operating software permits the user to program wash protocols with any one of six solvents per wash cycle with as many cycle repeats as necessary. Station capacity is eighty, 15 ml vials. This system has proven successful with a broad spectrum of both ethyl acetate and methylene chloride based chemistries. The development and characterization of this automated extraction system will be presented. PMID:18924693

Characterization and tailoring of porous sol-gel dielectrics for interlayer dielectric applications

NASA Astrophysics Data System (ADS)

Rogojevic, Svetlana

A new, better insulator is needed to replace SiO2 in the next generation of microelectronic devices. The dielectric constant of porous materials can be tailored by adjusting the porosity, so that their use can be extended to more than one generation of devices. Silica xerogel films with wide range of porosities (25 90%) are fabricated by varying the rate of solvent evaporation during spin-coating. Even better porosity control is achieved by using mixtures of high and low boiling point solvents, and allowing one solvent to evaporate completely during spin-coating. The quartz crystal microbalance method was employed to measure the traces of moisture adsorbed in xerogel films of varying porosities. By employing two different surface modifiers, it is demonstrated that the level of hydrophobicity is a function of surface chemistry, and can be tailored by using a suitable surface modifier. To investigate the interaction of xerogels with other materials, metallic layers were deposited on xerogel films, and subsequently annealed. When annealed in the ambient with trace amount of oxygen, Ta and Cu films undergo morphological instabilities. These morphological changes may lead to the erroneous interpretation of the Rutherford backscattering spectra as metal diffusion. When the samples are capped with a Si3N4 layer, Cu and Ta do not show diffusion through xerogel when annealed up to 650°C. Bias-temperature stressing was conducted in order to assess Cu drift through xerogel in the presence of an electric field. Contrary to what is normally observed with other dielectrics, the leakage current and C-V curve shifts were larger with an Al electrode than with a Cu electrode. This indicates that the surface modification of xerogel can contribute to the smaller charge injection from the Cu/xerogel interface, or to the inhibition of Cu diffusion, thus offering a possibility of designing future monolayer diffusion barriers for porous materials. Two possible paths of mass transfer in porous solids are identified: bulk and surface diffusion. Three driving forces are also analyzed: concentration gradient, electric field, and curvature gradient. The model of diffusion through porous solids shows the effects of the electric field, the solid network thickness, porosity, surface and bulk diffusivity. The model is a useful tool for designing and interpreting the experiments, in order to assess the role of surface diffusion in porous materials.

Uncovering Implicit Assumptions: A Large-Scale Study on Students' Mental Models of Diffusion

ERIC Educational Resources Information Center

Stains, Marilyne; Sevian, Hannah

2015-01-01

Students' mental models of diffusion in a gas phase solution were studied through the use of the Structure and Motion of Matter (SAMM) survey. This survey permits identification of categories of ways students think about the structure of the gaseous solute and solvent, the origin of motion of gas particles, and trajectories of solute particles in…

Chemical approach to solvent removal during nanoencapsulation: its application to preparation of PLGA nanoparticles with non-halogenated solvent

NASA Astrophysics Data System (ADS)

Lee, Youngme; Sah, Eric; Sah, Hongkee

2015-11-01

The objective of this study was to develop a new oil-in-water emulsion-based nanoencapsulation method for the preparation of PLGA nanoparticles using a non-halogenated solvent. PLGA (60-150 mg) was dissolved in 3 ml of methyl propionate, which was vortexed with 4 ml of a 0.5-4 % polyvinyl alcohol solution. This premix was sonicated for 2 min, added into 30 ml of the aqueous polyvinyl alcohol solution, and reacted with 3 ml of 10 N NaOH. Solvent removal was achieved by the alkaline hydrolysis of methyl propionate dissolved in an aqueous phase into water-soluble methanol and sodium propionate. It was a simple but effective technique to quickly harden nanoemulsion droplets into nanoparticles. The appearing PLGA nanoparticles were recovered by ultracentrifugation and/or dialysis, lyophilized with trehalose, and redispersed by water. This nanoencapsulation technique permitted a control of their mean diameters over 151.7 ± 3.8 to 440.2 ± 22.2 nm at mild processing conditions. When the aqueous polyvinyl alcohol concentration was set at ≥1 %, nanoparticles showed uniform distributions with polydispersity indices below 0.1. There were no significant changes in their mean diameters and size distribution patterns before and after lyophilization. When mestranol was encapsulated into nanoparticles, the drug was completely nanoencapsulated: depending on experimental conditions, their encapsulation efficiencies were determined to be 99.4 ± 7.2 to 105.8 ± 6.3 %. This simple, facile nanoencapsulation technique might have versatile applications for the preparation of polymeric nanoparticulate dosage forms.

Water dynamics in small reverse micelles in two solvents: two-dimensional infrared vibrational echoes with two-dimensional background subtraction.

PubMed

Fenn, Emily E; Wong, Daryl B; Fayer, M D

2011-02-07

Water dynamics as reflected by the spectral diffusion of the water hydroxyl stretch were measured in w(0) = 2 (1.7 nm diameter) Aerosol-OT (AOT)/water reverse micelles in carbon tetrachloride and in isooctane solvents using ultrafast 2D IR vibrational echo spectroscopy. Orientational relaxation and population relaxation are observed for w(0) = 2, 4, and 7.5 in both solvents using IR pump-probe measurements. It is found that the pump-probe observables are sensitive to w(0), but not to the solvent. However, initial analysis of the vibrational echo data from the water nanopool in the reverse micelles in the isooctane solvent seems to yield different dynamics than the CCl(4) system in spite of the fact that the spectra, vibrational lifetimes, and orientational relaxation are the same in the two systems. It is found that there are beat patterns in the interferograms with isooctane as the solvent. The beats are observed from a signal generated by the AOT/isooctane system even when there is no water in the system. A beat subtraction data processing procedure does a reasonable job of removing the distortions in the isooctane data, showing that the reverse micelle dynamics are the same within experimental error regardless of whether isooctane or carbon tetrachloride is used as the organic phase. Two time scales are observed in the vibrational echo data, ~1 and ~10 ps. The slower component contains a significant amount of the total inhomogeneous broadening. Physical arguments indicate that there is a much slower component of spectral diffusion that is too slow to observe within the experimental window, which is limited by the OD stretch vibrational lifetime.

Water dynamics in small reverse micelles in two solvents: Two-dimensional infrared vibrational echoes with two-dimensional background subtraction

NASA Astrophysics Data System (ADS)

Fenn, Emily E.; Wong, Daryl B.; Fayer, M. D.

2011-02-01

Water dynamics as reflected by the spectral diffusion of the water hydroxyl stretch were measured in w0 = 2 (1.7 nm diameter) Aerosol-OT (AOT)/water reverse micelles in carbon tetrachloride and in isooctane solvents using ultrafast 2D IR vibrational echo spectroscopy. Orientational relaxation and population relaxation are observed for w0 = 2, 4, and 7.5 in both solvents using IR pump-probe measurements. It is found that the pump-probe observables are sensitive to w0, but not to the solvent. However, initial analysis of the vibrational echo data from the water nanopool in the reverse micelles in the isooctane solvent seems to yield different dynamics than the CCl4 system in spite of the fact that the spectra, vibrational lifetimes, and orientational relaxation are the same in the two systems. It is found that there are beat patterns in the interferograms with isooctane as the solvent. The beats are observed from a signal generated by the AOT/isooctane system even when there is no water in the system. A beat subtraction data processing procedure does a reasonable job of removing the distortions in the isooctane data, showing that the reverse micelle dynamics are the same within experimental error regardless of whether isooctane or carbon tetrachloride is used as the organic phase. Two time scales are observed in the vibrational echo data, ~1 and ~10 ps. The slower component contains a significant amount of the total inhomogeneous broadening. Physical arguments indicate that there is a much slower component of spectral diffusion that is too slow to observe within the experimental window, which is limited by the OD stretch vibrational lifetime.

Probing Ion Transfer across Liquid-Liquid Interfaces by Monitoring Collisions of Single Femtoliter Oil Droplets on Ultramicroelectrodes.

PubMed

Deng, Haiqiang; Dick, Jeffrey E; Kummer, Sina; Kragl, Udo; Strauss, Steven H; Bard, Allen J

2016-08-02

We describe a method of observing collisions of single femtoliter (fL) oil (i.e., toluene) droplets that are dispersed in water on an ultramicroelectrode (UME) to probe the ion transfer across the oil/water interface. The oil-in-water emulsion was stabilized by an ionic liquid, in which the oil droplet trapped a highly hydrophobic redox probe, rubrene. The ionic liquid also functions as the supporting electrolyte in toluene. When the potential of the UME was biased such that rubrene oxidation would be possible when a droplet collided with the electrode, no current spikes were observed. This implies that the rubrene radical cation is not hydrophilic enough to transfer into the aqueous phase. We show that current spikes are observed when tetrabutylammonium trifluoromethanesulfonate or tetrahexylammonium hexafluorophosphate are introduced into the toluene phase and when tetrabutylammonium perchlorate is introduced into the water phase, implying that the ion transfer facilitates electron transfer in the droplet collisions. The current (i)-time (t) behavior was evaluated quantitatively, which indicated the ion transfer is fast and reversible. Furthermore, the size of these emulsion droplets can also be calculated from the electrochemical collision. We further investigated the potential dependence on the electrochemical collision response in the presence of tetrabutylammonium trifluoromethanesulfonate in toluene to obtain the formal ion transfer potential of tetrabutylammonium across the toluene/water interface, which was determined to be 0.754 V in the inner potential scale. The results yield new physical insights into the charge balance mechanism in emulsion droplet collisions and indicate that the electrochemical collision technique can be used to probe formal ion transfer potentials between water and solvents with very low (ε < 5) dielectric constants.

Employing photoacoustic spectroscopy in the evaluation of the skin permeation profile of emulsion containing antioxidant phenolic-rich extract of Melochia arenosa.

PubMed

Tunin, Luana Magri; Borghi, Fernanda Belincanta; Nogueira, Ana Claudia; Higachi, Luciana; Barbosa, Décio Sabbatini; Baesso, Mauro Luciano; Hernandes, Luzmarina; Diniz, Andréa; Truiti, Maria da Conceição Torrado

2016-01-01

Oxidative stress is an important factor modulating skin alterations. Melochia arenosa Benth. (Malvaceae) is a Brazilian plant with antimicrobial activity and antioxidant potential. The objective of this study is to develop a topical formulation containing antioxidant phenolic-rich extract of M. arenosa and to evaluate its skin permeation profile. Response surface methodology was used to maximize the total phenolic (TP) content of the extract and its antioxidant activity was evaluated by 2,2-diphenyl-1-picryl-hydrazyl (DPPH), 2,2'-azinobis (3-ethylbenzothiazoline-6-sulfonic acid) (ABTS), and respiratory burst methods. An emulsion containing 1% optimized extract (OE) was developed and employed photoacoustic spectroscopy (PAS) for the determination of its skin permeation profile. The morphology of the skin was studied in histological sections stained with hematoxylin-eosin. The optimum conditions predicted for the major extractive efficiency of the phenolics with 100% ethanol led extraction time 101 h and plant:solvent proportion 1:13.5 (w/v). OE presented TP = 724.6 ± 8.2 mg GAE/g extract and scavenging capacity of DPPH (IC50 value = 11.43 ± 0.14 µg/mL) and ABTS radicals (IC50 value = 35.42 ± 0.48 µg/mL). The production of ROS by neutrophils after stimulation with phorbol miristate acetate was lower when the OE was present in the reaction medium, endorsing its high antioxidant capacity. The data obtained by PAS indicated that the OE present in the emulsion has permeated and was distributed in the whole skin. No histopathological alterations were observed in the histological analysis. The formulation developed is a promising tool for skin care and could prevent the damage caused by oxidative stress.

High loading efficiency and sustained release of siRNA encapsulated in PLGA nanoparticles: quality by design optimization and characterization.

PubMed

Cun, Dongmei; Jensen, Ditte Krohn; Maltesen, Morten Jonas; Bunker, Matthew; Whiteside, Paul; Scurr, David; Foged, Camilla; Nielsen, Hanne Mørck

2011-01-01

Poly(DL-lactide-co-glycolide acid) (PLGA) is an attractive polymer for delivery of biopharmaceuticals owing to its biocompatibility, biodegradability and outstanding controlled release characteristics. The purpose of this study was to understand and define optimal parameters for preparation of small interfering RNA (siRNA)-loaded PLGA nanoparticles by the double emulsion solvent evaporation method and characterize their properties. The experiments were performed according to a 2(5-1) fractional factorial design based on five independent variables: The volume ratio between the inner water phase and the oil phase, the PLGA concentration, the sonication time, the siRNA load and the amount of acetylated bovine serum albumin (Ac-BSA) in the inner water phase added to stabilize the primary emulsion. The effects on the siRNA encapsulation efficiency and the particle size were investigated. The most important factors for obtaining an encapsulation efficiency as high as 70% were the PLGA concentration and the volume ratio whereas the size was mainly affected by the PLGA concentration. The viscosity of the oil phase was increased at high PLGA concentration, which explains the improved encapsulation by stabilization of the primary emulsion and reduction of siRNA leakage to the outer water phase. Addition of Ac-BSA increased the encapsulation efficiency at low PLGA concentrations. The PLGA matrix protected siRNA against nuclease degradation, provided a burst release of surface-localized siRNA followed by a triphasic sustained release for two months. These results enable careful understanding and definition of optimal process parameters for preparation of PLGA nanoparticles encapsulating high amounts of siRNA with immediate and long-term sustained release properties. Copyright © 2010 Elsevier B.V. All rights reserved.

Alternative Bio-Based Solvents for Extraction of Fat and Oils: Solubility Prediction, Global Yield, Extraction Kinetics, Chemical Composition and Cost of Manufacturing

PubMed Central

Sicaire, Anne-Gaëlle; Vian, Maryline; Fine, Frédéric; Joffre, Florent; Carré, Patrick; Tostain, Sylvain; Chemat, Farid

2015-01-01

The present study was designed to evaluate the performance of alternative bio-based solvents, more especially 2-methyltetrahydrofuran, obtained from crop’s byproducts for the substitution of petroleum solvents such as hexane in the extraction of fat and oils for food (edible oil) and non-food (bio fuel) applications. First a solvent selection as well as an evaluation of the performance was made with Hansen Solubility Parameters and the COnductor-like Screening MOdel for Realistic Solvation (COSMO-RS) simulations. Experiments were performed on rapeseed oil extraction at laboratory and pilot plant scale for the determination of lipid yields, extraction kinetics, diffusion modeling, and complete lipid composition in term of fatty acids and micronutrients (sterols, tocopherols and tocotrienols). Finally, economic and energetic evaluations of the process were conducted to estimate the cost of manufacturing using 2-methyltetrahydrofuran (MeTHF) as alternative solvent compared to hexane as petroleum solvent. PMID:25884332

A modified spontaneous emulsification solvent diffusion method for the preparation of curcumin-loaded PLGA nanoparticles with enhanced in vitro anti-tumor activity

NASA Astrophysics Data System (ADS)

Chen, Cen; Yang, Wei; Wang, Dan-Tong; Chen, Chao-Long; Zhuang, Qing-Ye; Kong, Xiang-Dong

2014-12-01

To improve the anti-tumor activity of hydrophobic drug curcumin, we prepared curcumin-loaded PLGA nanoparticles (PLGA-Cur NPs) through a modified spontaneous emulsification solvent diffusion (modified-SESD) method. The influence of main preparation parameters was investigated, such as the volume ratio of binary organic solvents and the concentration of surfactant. Results indicated that the synthesized regular spherical PLGA NPs with the average diameter of 189.7 nm exhibited relatively higher yield (58.9%), drug loading (11.0% (w/w)) and encapsulation efficiency (33.5%), and also a controllable drug release profile. In order to evaluate the in vitro cytotoxicity of the prepared NPs, MTT assay was conducted, and results showed that the NPs could effectively inhibit HL60 and HepG2 cells with lower IC50 values compared with free curcumin. Furthermore, confocal microscopy together with flow cytometry analysis proved the enhanced apoptosis-inducing ability of PLGA-Cur NPs. Polymeric NP formulations are potential to be used for hydrophobic drug delivery systems in cancer therapy.

Novel nanometer-level uniform amorphous carbon coating for boron powders by direct pyrolysis of coronene without solvent.

PubMed

Ye, ShuJun; Song, MingHui; Kumakura, Hiroaki

2015-01-30

A 3 nm coronene coating and a 4 nm amorphous carbon coating with a uniform shell-core encapsulation structure for nanosized boron (B) powders are formed by a simple process in which coronene is directly mixed with boron particles without a solvent and heated at 520 °C for 1 h or at 630 °C for 3 h in a vacuum-sealed silica tube. Coronene has a melting point lower than its decomposition temperature, which enables liquid coronene to cover B particles by liquid diffusion and penetration without the need for a solvent. The diffusion and penetration of coronene can extend to the boundaries of particles and to inside the agglomerated nanoparticles to form a complete shell-core encapsulated structure. As the temperature is increased, thermal decomposition of coronene on the B particles results in the formation of a uniform amorphous carbon coating layer. This novel and simple nanometer-level uniform amorphous carbon coating method can possibly be applied to many other powders; thus, it has potential applications in many fields at low cost.

An empirical relation between the limiting ionic molar conductivities and self-diffusion coefficients of pure solvents

NASA Astrophysics Data System (ADS)

Matsuyama, Hisashi; Motoyoshi, Kota

2018-05-01

The limiting ionic molar conductivity (λ∞) of an electrolyte solution depends on the self-diffusion coefficient (Ds) of the pure solvent when the temperature (T) changes. To study the Ds-dependence of λ∞, we proposed a new empirical relation λ∞ ∝(Ds / T) t , with a parameter t. The relation is applied to the λ∞ and Ds of alkali, tetra-alkyl ammonium, and halogen ions in water or methanol. All ions except for tetra-alkyl ammonium ions in water exhibit excellent linear relationships in their λ∞ ∝(Ds / T) t plots, with t in the range from 0.88 to 1.26. This is the first report showing an affirmative linear correlation between λ∞ and Ds.

Ballistic Motion of Enzymes that Catalyze Highly Exothermic Reactions

NASA Astrophysics Data System (ADS)

Tsekouras, Konstantinos; Pressé, Steve

Recently we proposed that the experimentally observed enhanced diffusion of enzymes catalyzing highly exothermic reactions is a consequence of their mechanism for dissipating reaction energy. More specifically, we proposed that reaction energy spreads out from the reaction site in the form of an acoustic wave which causes the enzyme to asymmetrically deform into the solvent. The solvent reaction propels the enzyme. However, it has been noted that in water, high viscosity should reduce enzyme momentum to zero within a few ps, so any diffusion increase should not be observable. Here we provide a model explaining how small volumetric expansions of biomolecules inside water may cause fluid compression that in turn creates regions of low fluid density around the biomolecule. We then investigate the dynamics of the biomolecule in the presence of these perturbations.

Roles of Poly(propylene Glycol) During Solvent-Based Lamination of Ceramic Green Tapes

NASA Technical Reports Server (NTRS)

Suppakarn, Nitinat; Ishida, Hatsuo; Cawley, James D.; Levine, Stanley R. (Technical Monitor)

2000-01-01

Solvent lamination for alumina green tapes is readily accomplished using a mixture of ethanol, toluene and poly(propylene glycol). After lamination, the PPG is clearly present as a discrete film at the interface between the laminated tapes. This condition, however, does not generate delamination during firing. Systematic sets of experiments are undertaken to determine the role of PPG in the lamination process and, specifically, the mechanism by which it is redistributed during subsequent processing. PPG slowly diffuses through the organic binder film at room temperature. The PPG diffusion rapidly increases as temperature is increased to 80 C. The key to the efficiency of adhesives during green-tape lamination is mutual solubility of the nonvolatile component of the glue and the base polymeric binder.

The relevance of light diffusion profiles for interstitial PDT using light-diffusing optical fibers

NASA Astrophysics Data System (ADS)

Stringasci, Mirian D.; Fortunato, Thereza C.; Moriyama, Lilian T.; Vollet Filho, José Dirceu; Bagnato, Vanderlei S.; Kurachi, Cristina

2017-02-01

Photodynamic therapy (PDT) is a technique used for several tumor types treatment. Light penetration on biological tissue is one limiting factor for PDT applied to large tumors. An alternative is using interstitial PDT, in which optical fibers are inserted into tumors. Cylindrical diffusers have been used in interstitial PDT. Light emission of different diffusers depends on the manufacturing process, size and optical properties of fibers, which make difficult to establish an adequate light dosimetry, since usually light profile is not designed for direct tissue-fiber contact. This study discusses the relevance of light distribution by a cylindrical diffuser into a turbid lipid emulsion solution, and how parts of a single diffuser contribute to illumination. A 2 cm-long cylindrical diffuser optical fiber was connected to a diode laser (630 nm), and the light spatial distribution was measured by scanning the solution with a collection probe. From the light field profile generated by a 1 mm-long intermediary element of a 20 mm-long cylindrical diffuser, recovery of light distribution for the entire diffuser was obtained. PDT was performed in rat healthy liver for a real treatment outcome analysis. By using computational tools, a typical necrosis profile generated by the irradiation with such a diffuser fiber was reconstructed. The results showed that it was possible predicting theoretically the shape of a necrosis profile in a healthy, homogeneous tissue with reasonable accuracy. The ability to predict the necrosis profile obtained from an interstitial illumination by optical diffusers has the potential improve light dosimetry for interstitial PDT.

Design and formulation of nano-sized spray dried efavirenz-part I: influence of formulation parameters

NASA Astrophysics Data System (ADS)

Katata, Lebogang; Tshweu, Lesego; Naidoo, Saloshnee; Kalombo, Lonji; Swai, Hulda

2012-11-01

Efavirenz (EFV) is one of the first-line antiretroviral drugs recommended by the World Health Organisation for treating HIV. It is a hydrophobic drug that suffers from low aqueous solubility (4 μg/mL), which leads to a limited oral absorption and low bioavailability. In order to improve its oral bioavailability, nano-sized polymeric delivery systems are suggested. Spray dried polycaprolactone-efavirenz (PCL-EFV) nanoparticles were prepared by the double emulsion method. The Taguchi method, a statistical design with an L8 orthogonal array, was implemented to optimise the formulation parameters of PCL-EFV nanoparticles. The types of sugar (lactose or trehalose), surfactant concentration and solvent (dichloromethane and ethyl acetate) were chosen as significant parameters affecting the particle size and polydispersity index (PDI). Small nanoparticles with an average particle size of less than 254 ± 0.95 nm in the case of ethyl acetate as organic solvent were obtained as compared to more than 360 ± 19.96 nm for dichloromethane. In this study, the type of solvent and sugar were the most influencing parameters of the particle size and PDI. Taguchi method proved to be a quick, valuable tool in optimising the particle size and PDI of PCL-EFV nanoparticles. The optimised experimental values for the nanoparticle size and PDI were 217 ± 2.48 nm and 0.093 ± 0.02.

Mesophase and size manipulation of itraconazole liquid crystalline nanoparticles produced via quasi nanoemulsion precipitation.

PubMed

Mugheirbi, Naila A; Tajber, Lidia

2015-10-01

The fabrication of drug nanoparticles (NPs) with process-mediated tunable properties and performances continues to grow rapidly during the last decades. This study investigates the synthesis and phase tuning of nanoparticulate itraconazole (ITR) mesophases using quasi nanoemulsion precipitation from acetone/water systems to seek out an alternative pathway to the nucleation-based NP formation. ITR liquid crystalline (LC) phases were formed and nematic-smectic mesomorphism was achieved via controlling solvent:antisolvent temperature difference (ΔTS:AS). The use of ΔTS:AS=49.5°C was associated with a nematic assembly, while intercalated smectic A layering was observed at ΔTS:AS=0°C, with both phases confined in the nanospheres at room temperature. The quasi emulsion system has not been investigated at the nanoscale to date and in contrary to the microscale, quasi nanoemulsion was observed over the solvent:antisolvent viscosity ratios of 1:7-1:1.4. Poly(acrylic acid) in the solvent phase exhibited a concentration dependent interaction when ITR formed NPs. This nanodroplet-based approach enabled the preparation of a stable ITR nanodispersion using Poloxamer 407 at 80°C, which was unachievable before using precipitation via nucleation. Findings of this work lay groundwork in terms of rationalised molecular assembly as a tool in designing pharmaceutical LC NPs with tailored properties. Copyright © 2015 Elsevier B.V. All rights reserved.

Electrophoretic and Electrolytic Deposition of Ceramic Particles on Porous Substrates

DTIC Science & Technology

1990-08-30

hydrodynamic drag force exerted on the particle due to the electroosmotic flow of the solvent inside the pore, the electrophoretic force exerted on the...8217 - electrophoretic velocity UN - electroosmotic velocity b - pore mean radius D - diffusion coefficient k - local deposition rate Large Peclet numbers and small...experimentally as the charge is acquired spontaneously on mixing the particles with the solvent and it may be reversed upon addition ot ionic compounds. The

Solvent friction changes the folding pathway of the tryptophan zipper TZ2.

PubMed

Narayanan, Ranjani; Pelakh, Leslie; Hagen, Stephen J

2009-07-17

Because the rate of a diffusional process such as protein folding is controlled by friction encountered along the reaction pathway, the speed of folding is readily tunable through adjustment of solvent viscosity. The precise relationship between solvent viscosity and the rate of diffusion is complex and even conformation-dependent, however, because both solvent friction and protein internal friction contribute to the total reaction friction. The heterogeneity of the reaction friction along the folding pathway may have subtle consequences. For proteins that fold on a multidimensional free-energy surface, an increase in solvent friction may drive a qualitative change in folding trajectory. Our time-resolved experiments on the rapidly and heterogeneously folding beta-hairpin TZ2 show a shift in the folding pathway as viscosity increases, even though the energetics of folding is unaltered. We also observe a nonlinear or saturating behavior of the folding relaxation time with rising solvent viscosity, potentially an experimental signature of the shifting pathway for unfolding. Our results show that manipulations of solvent viscosity in folding experiments and simulations may have subtle and unexpected consequences on the folding dynamics being studied.

Temperature Dependence of Nonelectrolyte Permeation across Red Cell Membranes

PubMed Central

Galey, W. R.; Owen, J. D.; Solomon, A. K.

1973-01-01

The temperature dependence of permeation across human red cell membranes has been determined for a series of hydrophilic and lipophilic solutes, including urea and two methyl substituted derivatives, all the straight-chain amides from formamide through valeramide and the two isomers, isobutyramide and isovaleramide. The temperature coefficient for permeation by all the hydrophilic solutes is 12 kcal mol-1 or less, whereas that for all the lipophilic solutes is 19 kcal mol-1 or greater. This difference is consonant with the view that hydrophilic molecules cross the membrane by a path different from that taken by the lipophilic ones. The thermodynamic parameters associated with lipophile permeation have been studied in detail. ΔG is negative for adsorption of lipophilic amides onto an oil-water interface, whereas it is positive for transfer of the polar head from the aqueous medium to bulk lipid solvent. Application of absolute reaction rate theory makes it possible to make a clear distinction between diffusion across the water-red cell membrane interface and diffusion within the membrane. Diffusion coefficients and apparent activation enthalpies and entropies have been computed for each process. Transfer of the polar head from the solvent into the interface is characterized by ΔG ‡ = 0 kcal mol-1 and ΔS ‡ negative, whereas both of these parameters have large positive values for diffusion within the membrane. Diffusion within the membrane is similar to what is expected for diffusion through a highly associated viscous fluid. PMID:4708405

Diffusional Transport of Organic Solutes in Subsurface Clay Lenses and Layers

NASA Astrophysics Data System (ADS)

Demond, A. H.; Ayral, D.; Goltz, M. N.

2009-12-01

The storage of organic solvents in clay lenses and layers in the subsurface creates long-term contaminant sources. Because of the low hydraulic conductivities of clay, it is thought that organic movement into clay lenses occurs through the process of diffusion. The ratio of the effective diffusion coefficient in the porous medium and the diffusion coefficient in bulk water is usually given by the tortuosity factor which accounts for the reduced area and the increased path length in the porous medium. However, there is field evidence which suggests that the concentrations in these lenses exceed that which can be accounted for by simple diffusion. There are reports, for example, of tortuosity factors greater than 1.0, which theoretically is not possible. Clays such as montmorillonite or bentonite shrink and swell depending on water content, and similar behavior can occur in the presence of organic solvents. In fact, research has shown that the basal spacing of bentonite can decrease by 50% when permeated with heptane. Such contraction of the clay structure can lead to the formation of cracks and macropores, with a concomitant alteration of the diffusional pathways that solutes follow. Models formulated for diffusional transport in soil are available to calculate the tortuosity factor as a function of water content. In addition, models are available to simulate phenomena in which the diffusion coefficient is concentration dependent. However, calculations of diffusional transport using such models show that they may not adequately reflect the impact of the alteration of the clay structure. However, modeling the transport of organic solutes in clay as a dual-domain system with some minimal advective transport in macropores can yield tortuosity factors greater than 1.0. Thus, it appears the cracking of clay in contact with organic solvents and a resultant advective component to transport of the solute may be an explanation of field observations.

Preliminary evaluation of an aqueous wax emulsion for controlled-release coating.

PubMed

Walia, P S; Stout, P J; Turton, R

1998-02-01

The purpose of this work was to evaluate the use of an aqueous carnauba wax emulsion (Primafresh HS, Johnson Wax) in a spray-coating process. This involved assessing the effectiveness of the wax in sustaining the release of the drug, theophylline. Second, the process by which the drug was released from the wax-coated pellets was modeled. Finally, a method to determine the optimum blend of pellets with different wax thicknesses, in order to yield a zero-order release profile of the drug, was addressed. Nonpareil pellets were loaded with theophylline using a novel powder coating technique. These drug-loaded pellets were then coated with different levels of carnauba wax in a 6-in. diameter Plexiglas fluid bed with a 3.5-in. diameter Wurster partition. Drug release was measured using a spin-filter dissolution device. The study resulted in continuous carnauba wax coatings which showed sustained drug release profile characteristics typical of a barrier-type, diffusion-controlled system. The effect of varying wax thickness on the release profiles was investigated. It was observed that very high wax loadings would be required to achieve long sustained-release times. The diffusion model, developed to predict the release of the drug, showed good agreement with the experimental data. However, the data exhibited an initial lag-time for drug release which could not be predicted a priori based on the wax coating thickness. A method of mixing pellets with different wax thicknesses was proposed as a way to approximate zero-order release.

Fabrication of Polymer Microspheres for Optical Resonator and Laser Applications.

PubMed

Yamamoto, Yohei; Okada, Daichi; Kushida, Soh; Ngara, Zakarias Seba; Oki, Osamu

2017-06-02

This paper describes three methods of preparing fluorescent microspheres comprising π-conjugated or non-conjugated polymers: vapor diffusion, interface precipitation, and mini-emulsion. In all methods, well-defined, micrometer-sized spheres are obtained from a self-assembling process in solution. The vapor diffusion method can result in spheres with the highest sphericity and surface smoothness, yet the types of the polymers able to form these spheres are limited. On the other hand, in the mini-emulsion method, microspheres can be made from various types of polymers, even from highly crystalline polymers with coplanar, π-conjugated backbones. The photoluminescent (PL) properties from single isolated microspheres are unusual: the PL is confined inside the spheres, propagates at the circumference of the spheres via the total internal reflection at the polymer/air interface, and self-interferes to show sharp and periodic resonant PL lines. These resonating modes are so-called "whispering gallery modes" (WGMs). This work demonstrates how to measure WGM PL from single isolated spheres using the micro-photoluminescence (µ-PL) technique. In this technique, a focused laser beam irradiates a single microsphere, and the luminescence is detected by a spectrometer. A micromanipulation technique is then used to connect the microspheres one by one and to demonstrate the intersphere PL propagation and color conversion from coupled microspheres upon excitation at the perimeter of one sphere and detection of PL from the other microsphere. These techniques, µ-PL and micromanipulation, are useful for experiments on micro-optic application using polymer materials.

Improved Treatment of Pancreatic Cancer With Drug Delivery Nanoparticles Loaded With a Novel AKT/PDK1 Inhibitor.

PubMed

Kobes, Joseph E; Daryaei, Iman; Howison, Christine M; Bontrager, Jordan G; Sirianni, Rachael W; Meuillet, Emmanuelle J; Pagel, Mark D

2016-09-01

This research study sought to improve the treatment of pancreatic cancer by improving the drug delivery of a promising AKT/PDK1 inhibitor, PHT-427, in poly(lactic-co-glycolic) acid (PLGA) nanoparticles. PHT-427 was encapsulated in single-emulsion and double-emulsion PLGA nanoparticles (SE-PLGA-427 and DE-PLGA-427). The drug release rate was evaluated to assess the effect of the second PLGA layer of DE-PLGA-427. Ex vivo cryo-imaging and drug extraction from ex vivo organs was used to assess the whole-body biodistribution in an orthotopic model of MIA PaCa-2 pancreatic cancer. Anatomical magnetic resonance imaging (MRI) was used to noninvasively assess the effects of 4 weeks of nanoparticle drug treatment on tumor size, and diffusion-weighted MRI longitudinally assessed changes in tumor cellularity. DE-PLGA-427 showed delayed drug release and longer drug retention in the pancreas relative to SE-PLGA-427. Diffusion-weighted MRI indicated a consistent decrease in cellularity during drug treatment with both types of drug-loaded nanoparticles. Both SE- and DE-PLGA-427 showed a 6-fold and 4-fold reduction in tumor volume relative to untreated tumors and an elimination of primary pancreatic tumor in 68% of the mice. These results indicated that the PLGA nanoparticles improved drug delivery of PHT-427 to pancreatic tumors, which improved the treatment of MIA PaCa-2 pancreatic cancer.

Improved Treatment of Pancreatic Cancer With Drug Delivery Nanoparticles Loaded With a Novel AKT/PDK1 Inhibitor

PubMed Central

Kobes, Joseph E.; Daryaei, Iman; Howison, Christine M.; Bontrager, Jordan G.; Sirianni, Rachael W.; Meuillet, Emmanuelle J.; Pagel, Mark D.

2015-01-01

Objectives This research study sought to improve the treatment of pancreatic cancer by improving the drug delivery of a promising AKT/PDK1 inhibitor, PHT-427, in poly(lactic-co-glycolic) acid (PLGA) nanoparticles. Methods PHT-427 was encapsulated in single-emulsion and double-emulsion PLGA nanoparticles (SE- and DE-PLGA-427). The drug release rate was evaluated to assess the effect of the second PLGA layer of DE-PLGA-427. Ex vivo cryo-imaging and drug extraction from ex vivo organs was used to assess the whole body biodistribution in an orthotopic model of MiaPaCa-2 pancreatic cancer. Anatomical MRI was used to noninvasively assess the effects of four weeks of nanoparticle-drug treatment on tumor size, and diffusion-weighted MRI longitudinally assessed changes in tumor cellularity. Results DE-PLGA-427 showed delayed drug release and longer drug retention in the pancreas relative to SE-PLGA-427. Diffusion-weighted MRI indicated a consistent decrease in cellularity during drug treatment with both types of drug-loaded nanoparticles. Both SE- and DE-PLGA-427 showed a 6-fold and 4-fold reduction in tumor volume relative to untreated tumors, and an elimination of primary pancreatic tumor in 68% of the mice. Conclusions These results indicated that the PLGA nanoparticles improved drug delivery of PHT-427 to pancreatic tumors, which improved the treatment of Mia PaCa-2 pancreatic cancer. PMID:26918875

Percolation characteristics of solvent invasion in rough fractures under miscible conditions

NASA Astrophysics Data System (ADS)

Korfanta, M.; Babadagli, T.; Develi, K.

2017-10-01

Surface roughness and flow rate effects on the solvent transport under miscible conditions in a single fracture are studied. Surface replicas of seven different rocks (marble, granite, and limestone) are used to represent different surface roughness characteristics each described by different mathematical models including three fractal dimensions. Distribution of dyed solvent is investigated at various flow rate conditions to clarify the effect of roughness on convective and diffusive mixing. After a qualitative analysis using comparative images of different rocks, the area covered by solvent with respect to time is determined to conduct a semi-quantitative analysis. In this exercise, two distinct zones are identified, namely the straight lines obtained for convective (early times) and diffusive (late times) flow. The bending point between these two lines is used to point the transition between the two zones. Finally, the slopes of the straight lines and the bending points are correlated to five different roughness parameters and the rate (Peclet number). It is observed that both surface roughness and flow rate have significant effect on solvent spatial distribution. The largest area covered is obtained at moderate flow rates and hence not only the average surface roughness characteristic is important, but coessentially total fracture surface area needs to be considered when evaluating fluid distribution. It is also noted that the rate effect is critically different for the fracture samples of large grain size (marbles and granite) compared to smaller grain sizes (limestones). Variogram fractal dimension exhibits the strongest correlation with the maximum area covered by solvent, and display increasing trend at the moderate flow rates. Equations with variogram surface fractal dimension in combination with any other surface fractal parameter coupled with Peclet number can be used to predict maximum area covered by solvent in a single fracture, which in turn can be utilized to model oil recovery, waste disposal, and groundwater contamination processes in the presence of fractures.

Enhanced encapsulation and bioavailability of breviscapine in PLGA microparticles by nanocrystal and water-soluble polymer template techniques.

PubMed

Wang, Hong; Zhang, Guangxing; Ma, Xueqin; Liu, Yanhua; Feng, Jun; Park, Kinam; Wang, Wenping

2017-06-01

Poly (lactide-co-glycolide) (PLGA) microparticles are widely used for controlled drug delivery. Emulsion methods have been commonly used for preparation of PLGA microparticles, but they usually result in low loading capacity, especially for drugs with poor solubility in organic solvents. In the present study, the nanocrystal technology and a water-soluble polymer template method were used to fabricate nanocrystal-loaded microparticles with improved drug loading and encapsulation efficiency for prolonged delivery of breviscapine. Breviscapine nanocrystals were prepared using a precipitation-ultrasonication method and further loaded into PLGA microparticles by casting in a mold from a water-soluble polymer. The obtained disc-like particles were then characterized and compared with the spherical particles prepared by an emulsion-solvent evaporation method. X-ray powder diffraction (XRPD) and confocal laser scanning microscopy (CLSM) analysis confirmed a highly-dispersed state of breviscapine inside the microparticles. The drug form, loading percentage and fabrication techniques significantly affected the loading capacity and efficiency of breviscapine in PLGA microparticles, and their release performance as well. Drug loading was increased from 2.4% up to 15.3% when both nanocrystal and template methods were applied, and encapsulation efficiency increased from 48.5% to 91.9%. But loading efficiency was reduced as the drug loading was increased. All microparticles showed an initial burst release, and then a slow release period of 28days followed by an erosion-accelerated release phase, which provides a sustained delivery of breviscapine over a month. A relatively stable serum drug level for more than 30days was observed after intramuscular injection of microparticles in rats. Therefore, PLGA microparticles loaded with nanocrystals of poorly soluble drugs provided a promising approach for long-term therapeutic products characterized with preferable in vitro and in vivo performance. Copyright © 2017 Elsevier B.V. All rights reserved.

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

Han, Kee Sung; Rajput, Nav Nidhi; Persson, Kristin A.

Ferrocene (Fc) and N-(ferrocenylmethyl)-N,N-dimethyl-N-ethylammonium bistrifluoromethyl-sulfonimide (Fc1N112-TFSI) were dissolved in carbonate solvents and self-diffusion coefficients (D) of solutes and solvents were measured by {sup 1}H and {sup 19}F pulsed field gradient nuclear magnetic resonance (NMR) spectroscopy. The organic solvents were propylene carbonate (PC), ethyl methyl carbonate (EMC), and a ternary mixture that also includes ethylene carbonate (EC). Results from NMR studies over the temperature range of 0–50 °C and for various concentrations (0.25–1.7 M) of Fc1N112-TFSI are compared to values of D simulated with classical molecular dynamics (MD). The measured self-diffusion coefficients gradually decreased as the Fc1N112-TFSI concentration increased in allmore » solvents. Since TFSI{sup −} has fluoromethyl groups (CF{sub 3}), D{sub TFSI} could be measured separately and the values found are larger than those for D{sub Fc1N112} in all samples measured. The EC, PC, and EMC have the same D in the neat solvent mixture and when Fc is dissolved in EC/PC/EMC at a concentration of 0.2 M, probably due to the interactions between common carbonyl structures within EC, PC, and EMC. A difference in D (D{sub PC} < D{sub EC} < D{sub EMC}), and both a higher E{sub a} for translational motion and higher effective viscosity for PC in the mixture containing Fc1N112-TFSI reflect the interaction between PC and Fc1N112{sup +}, which is a relatively stronger interaction than that between Fc1N112{sup +} and other solvent species. In the EC/PC/EMC solution that is saturated with Fc1N112-TFSI, we find that D{sub PC} = D{sub EC} = D{sub EMC} and Fc1N112{sup +} and all components of the EC/PC/EMC solution have the same E{sub a} for translational motion, while the ratio D{sub EC/PC/EMC}/D{sub Fc1N112} is approximately 3. These results reflect the lack of available free volume for independent diffusion in the saturated solution. The Fc1N112{sup +} transference numbers lie around 0.4 and increase slightly as the temperature is increased in the PC and EMC solvents. The trends observed for D from simulations are in good agreement with experimental results and provide molecular level understanding of the solvation structure of Fc1N112-TFSI dissolved in EC/PC/EMC.« less

Environmental stress cracking in gamma-irradiated polycarbonate - A diffusion approach

NASA Astrophysics Data System (ADS)

Silva, Pietro Paolo J. C. de O.; Araújo, Patricia L. B.; da Silveira, Leopoldo B. B.; Araújo, Elmo S.

2017-01-01

Polycarbonate (PC) is an engineering polymer which presents interesting properties. This material has been also used in medical devices, which is frequently exposed to gamma radiosterilization and to chemical agents. This may produce significant changes in polymer structure, leading to failure in service. The present work brings about a new approach on environmental stress cracking (ESC) processes elucidation in 100 kGy gamma-irradiated PC, by evaluating the diffusion process of methanol or 2-propanol in test specimens and determining the diffusion parameters on solvent-irradiated polymer systems. A comparison of diffusion parameters for both solvents indicated that methanol has a considerable ESC action on PC, with diffusion parameter of 7.5×10-14±1% m2 s-1 for non-irradiated PC and 7.8×10-14±2.8% m2 s-1 for PC irradiated at 100 kGy. In contrast, 2-propanol did not act as an ESC agent, as it did promote neither swelling nor cracks in the test specimens. These results were confirmed by visual analysis and optical microscopy. Unexpectedly, structural damages evidenced in tensile strength tests suggested that 2-propanol is as aggressive as methanol chemical for PC. Moreover, although some manufacturers indicate the use of 2-propanol as a cleaning product for PC artifacts, such use should be avoided in parts under mechanical stress.

Diffusion behavior of the fluorescent proteins eGFP and Dreiklang in solvents of different viscosity monitored by fluorescence correlation spectroscopy

NASA Astrophysics Data System (ADS)

Junghans, Cornelia; Schmitt, Franz-Josef; Vukojević, Vladana; Friedrich, Thomas

2016-12-01

Fluorescence correlation spectroscopy relies on temporal autocorrelation analysis of fluorescence intensity fluctuations that spontaneously arise in systems at equilibrium due to molecular motion and changes of state that cause changes in fluorescence, such as triplet state transition, photoisomerization and other photophysical transformations, to determine the rates of these processes. The stability of a fluorescent molecule against dark state conversion is of particular concern for chromophores intended to be used as reference tags for comparing diffusion processes on multiple time scales. In this work, we analyzed properties of two fluorescent proteins, the photoswitchable Dreiklang and its parental eGFP, in solvents of different viscosity to vary the diffusion time through the observation volume element by several orders of magnitude. In contrast to eGFP, Dreiklang undergoes a dark-state conversion on the time scale of tens to hundreds of microseconds under conditions of intense fluorescence excitation, which results in artificially shortened diffusion times if the diffusional motion through the observation volume is sufficiently slowed down. Such photophysical quenching processes have also been observed in FCS studies on other photoswitchable fluorescent proteins including Citrine, from which Dreiklang was derived by genetic engineering. This property readily explains the discrepancies observed previously between the diffusion times of eGFP- and Dreiklang-labeled plasma membrane protein complexes.

Effect of hydro-oleophobic perfluorocarbon chain on interfacial behavior and mechanism of perfluorooctane sulfonate in oil-water mixture

PubMed Central

Meng, Pingping; Deng, Shubo; Du, Ziwen; Wang, Bin; Huang, Jun; Wang, Yujue; Yu, Gang; Xing, Baoshan

2017-01-01

Perfluorocarbon chain of perfluorooctane sulfonate (PFOS) is not only hydrophobic but also oleophobic, and its effect on PFOS distribution in oil-water mixture and underlying mechanism are unclear. For the first time, we propose that PFOS can emulsify oil-water mixture only in the presence of air, completely different from hydrocarbon surfactants. The perfluorocarbon chain repels hydrophobic compounds and its oleophobicity increases with decreasing polarity of organic solvents. The formed emulsion in oil phase contains high concentrations of PFOS, resulting in PFOS decrease in water. The increase of shaking speed and time as well as oil and air volume all increase the emulsification and decrease PFOS concentrations in water. During the settling process, the emulsion gradually disappears and the concentrated PFOS is released into water. The emulsification mechanism of PFOS based on air bubbles is proposed, and PFOS partitions to the interfaces of air bubbles with the hydro-oleophobic perfluorocarbon chain stretching into air bubbles and the polar head in water. This study clarifies the ambiguous understanding of the oleophobicity of perfluorocarbon chain in PFOS, and it is helpful for the understanding of the transport and fate of PFOS at oil-water interfaces in aquatic environments as well as the enhanced removal of PFOS from wastewater. PMID:28300199

Effect of PLGA as a polymeric emulsifier on preparation of hydrophilic protein-loaded solid lipid nanoparticles.

PubMed

Xie, ShuYu; Wang, SiLiang; Zhao, BaoKai; Han, Chao; Wang, Ming; Zhou, WenZhong

2008-12-01

Most proteins are hydrophilic and poorly encapsulated into the hydrophobic matrix of solid lipid nanoparticles (SLN). To solve this problem, poly (lactic-co-glycolic acid) (PLGA) was utilized as a lipophilic polymeric emulsifier to prepare hydrophilic protein-loaded SLN by w/o/w double emulsion and solvent evaporation techniques. Hydrogenated castor oil (HCO) was used as a lipid matrix and bovine serum albumin (BSA), lysozyme and insulin were used as model proteins to investigate the effect of PLGA on the formulation of the SLN. The results showed that PLGA was essential for the primary w/o emulsification. In addition, the stability of the w/o emulsion, the encapsulation efficiency and loading capacity of the nanoparticles were enhanced with the increase of PLGA concentration. Furthermore, increasing PLGA concentration decreased zeta potential significantly but had no influence on particle size of the SLN. In vitro release study showed that PLGA significantly affected the initial burst release, i.e. the higher the content of PLGA, the lower the burst release. The released proteins maintained their integrity and bioactivity as confirmed by sodium dodecyl sulphate-polyacrylamide gel electrophoresis (SDS-PAGE) and biological assay. These results demonstrated that PLGA was an effective emulsifier for the preparation of hydrophilic protein-loaded SLN.

Carbon dioxide extraction of residual chloroform from biodegradable polymers.

PubMed

Koegler, Wendy S; Patrick, Carmen; Cima, Michael J; Griffith, Linda G

2002-01-01

Biodegradable polymeric devices for drug delivery and tissue engineering are often fabricated with the use of organic solvents and may still contain significant amounts of solvent (> 1 wt%) even after aggressive vacuum drying. This excess solvent can interfere with tissue response and the mechanical properties of the devices. The aim of this article is to demonstrate that liquid CO(2) extraction can be used to reduce residual solvent in dense poly(L-lactide-co-glycolide) devices to 50 ppm relatively quickly and with minimal changes in architecture under some conditions. Two liquid CO(2) extraction systems were developed to examine the removal of residual solvents from bar-shaped PLGA devices: (1) a low-pressure (1400 psi) batch system, and (2) a high-pressure (5000 psi) continuous-flow system. Eight hours of extraction in the high-pressure system reduced residual chloroform in 3 mm thick bars below the 50-ppm target. A simple Fickian diffusion model was fit to the extraction results. Diffusion coefficients ranged from 1.10 x 10(-6) cm(2)/s to 2.64 x 10(-6) cm(2)/s. The model predicts that approximately 1 h is needed to dry 1-mm bars to chloroform levels below 50 ppm, and 7 h are needed for 3 mm thick bars. The micro- and macroarchitectures of porous PLGA scaffolds created by particulate leaching were not significantly altered by CO(2) drying if the salt used to make the pores was not removed before drying. Copyright 2002 Wiley Periodicals, Inc. J Biomed Mater Res (Appl Biomater) 63: 567-576, 2002

Study of diffusion of indocyanine green as a photodynamic dye into skin using backscattering spectroscopy

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

Genina, E A; Bashkatov, A N; Tuchin, V V

One of the lines of development of modern medicine is theranostics consisting in simultaneous diagnosis and laser treatment with the use of multifunctional agents such as fluorescent indocyanine green that has photodynamic and photothermal properties. Diffusion of indocyanine green dissolved in water and aqueous solutions of alcohols (glycerol, propylene glycol and ethanol) into the dermis is studied by using backscattering spectroscopy. The coefficients of the dye diffusion into the dermis are obtained for the first time by using these solvents. (laser biophotonics)

Proteins as micro viscosimeters: Brownian motion revisited.

PubMed

Lavalette, Daniel; Hink, Mark A; Tourbez, Martine; Tétreau, Catherine; Visser, Antonie J

2006-08-01

Translational and rotational diffusion coefficients of proteins in solution strongly deviate from the Stokes-Einstein laws when the ambient viscosity is induced by macromolecular co-solutes rather than by a solvent of negligible size as was assumed by A. Einstein one century ago for deriving the laws of Brownian motion and diffusion. Rotational and translational motions experience different micro viscosities and both become a function of the size ratio of protein and macromolecular co-solute. Possible consequences upon fluorescence spectroscopy observations of diffusing proteins within living cells are discussed.