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PubMed2006

Quantitative membrane electrostatics with the atomic force microscope.

The atomic force microscope (AFM) is sensitive to electric double layer interactions in electrolyte solutions, but provides only a qualitative view of interfacial electrostatics. We have fully characterized silicon nitride probe tips and other experimental parameters to allow a quantitative electrostatic analysis by AFM, and we have tested the validity of a simple analytical force expression through numerical simulations. As a test sample, we have measured the effective surface charge density of supported zwitterionic dioleoylphosphatidylcholine membranes with a variable fraction of anionic dioleoylphosphatidylserine. The resulting surface charge density and surface potential values are in quantitative agreement with those predicted by the Gouy-Chapman-Stern model of membrane charge regulation, but only when the numerical analysis is employed. In addition, we demonstrate that the AFM can detect double layer forces at a separation of several screening lengths, and that the probe only perturbs the membrane surface potential by <2%. Finally, we demonstrate 50-nm resolution electrostatic mapping on heterogeneous model membranes with the AFM. This novel combination of capabilities demonstrates that the AFM is a unique and powerful probe of membrane electrostatics.

Algorithms↗
PubMedDate not supplied

Buonocore memorial lecture. Adhesion to enamel and dentin: current status and future challenges.

Bonding to tooth tissue can be achieved through an "etch&rinse," "self-etch" or "glass-ionomer" approach. In this paper, the basic bonding mechanism to enamel and dentin of these three approaches is demonstrated by means of ultramorphological and chemical characterization of tooth-biomaterial interfacial interactions. Furthermore, bond-strength testing and measurement of marginal-sealing effectiveness (the two most commonly employed methodologies to determine "bonding effectiveness" in the laboratory) are evaluated upon their value and relevance in predicting clinical performance. A new dynamic methodology to test biomaterial-tooth bonds in a fatigue mode is introduced with a recently developed micro-rotary fatigue-testing device. Eventually, today's adhesives will be critically weighted upon their performance in diverse laboratory studies and clinical trials. Special attention has been given to the benefits/drawbacks of an etch&rinse versus a self-etch approach and the long-term performance of these adhesives. Correlating data gathered in the laboratory with clinical results clearly showed that laboratory research CAN predict clinical effectiveness. Although there is a tendency to simplify bonding procedures, the data presented confirm that conventional three-step etch&rinse adhesives still perform most favorably and are most reliable in the long-term. Nevertheless, a self-etch approach may have the best future perspective. Clinically, when adhesives no longer require an "etch&rinse" step, the application time, and probably more importantly, the technique-sensitivity are substantially reduced. Especially "mild," two-step self-etch adhesives that bond through a combined micromechanical and chemical interaction with tooth tissue closely approach conventional three-step systems in bonding performance.

Acid Etching, Dental↗
PubMed2006

Importance of surface tension characterization for food, pharmaceutical and packaging products: a review.

This article reviews the various theoretical approaches that have been developed for determination of the surface tension of solids, and the applications to food industrial products. The surface tension of a solid is a characteristic of surface properties and interfacial interactions such as adsorption, wetting or adhesion. The knowledge of surface tension is thus of great interest for every domain involved in understanding these mechanisms, which recover a lot of industrial investigations. Indeed, it is the case for the packaging industry, the food materials science, the biomedical applications and the pharmaceutical products, cleaning, adhesive technology, painting, coating and more generally all fields in relation with wettability of their systems. There is however no direct method for measurements of surface tension of solids, except the contact angle measurements combined with an appropriate theoretical approach are indirect methods for estimation of surface tension of solids. Moreover, since the publication by Young (1805) who developed the basis of the theory of contact angle some two hundred years ago, measurements and interpretations are still discussed in scientific literature, pointing out the need to better understand the fundamental mechanisms of solid-liquid interfacial interactions. Applications of surface tension characterization in the field of food materials science are detailed, especially for packaging and coating applications, which recover different actual orientations in order to improve process and quality.

Biodegradation, Environmental↗
PubMedDate not supplied

Physico-chemical characterization and in vivo evaluation of indomethacin ethyl ester-loaded nanocapsules by PCS, TEM, SAXS, interfacial alkaline hydrolysis and antiedematogenic activity.

Nanocapsules are vesicular drug carriers constituted of an oil core, a polymeric wall, and surfactants. A general understanding about the influence of the polymeric wall of nanocapsules on the release profiles of drugs is not known. So, this work was devoted to characterize formulations prepared without polymer or containing it at different concentrations. The indomethacin ethyl ester was used as model and the strategy was based on its interfacial alkaline hydrolysis simulating a sink condition for the release. The antiedematogenic activity in rats for ester-loaded-nanocarriers was also evaluated. The nanocapsules (NC) and nanoemulsion (NE) presented particle sizes below 300 nm, polydispersity lower than 1.2 and pH around 5. SAXS analyses showed that the sorbitan monostearate is dissolved in the oil and the polymer presents regions of crystallinity independently on the PCL concentration. TEM analyses showed droplets (NE) and spherical particles (NC). The time for the total disappearance of the ester varied from 12 h to 24 h depending on the polymer concentration. The biexponential model showed that the indomethacin ester was essentially entrapped within the nanocarriers in an extension of 85 to 95%. The half-lives varied from 147 to 289 min for the sustained phases and from 3 to 6 min for the burst phases. The ester-loaded-NC showed significant antiedematogenic activity, while the ester-loaded-NE did not inhibit the carrageenin-induced paw edema. The nanocapsules promoted the absorption of the indomethacin ethyl ester and the presence of the polymer is important to achieve the pharmacological effect.

Alkalies↗
PubMed2005

Film formation of Ag nanoparticles at the organic-aqueous liquid interface.

We report a wet-chemical method to make films by spontaneous assembly of passivated Ag nanoparticles at the organic-aqueous liquid interface. The interfacial films exhibit a blue opalescence and are characterized with transmission electron microscopy and UV-vis spectrophotometry. Measurements indicate that nanoparticles in the interfacial film can form superlattices and in some cases nanostructures.

Fatty Acids↗
PubMed1999

Effect of metal surface topography on mechanical bonding at simulated total hip stem-cement interfaces.

Bonding and loosening mechanisms between bone cement and joint prostheses have not been well identified. In this study, the effects of simulated hip stem surface topography on the interfacial shear strength were examined. Six different surface topographies were used. They were described by several surface characterization parameters that may directly relate to the interfacial bonding strength: average surface roughness R(a), root mean square slope R(Deltaq), correlation length beta, and fluid retention index R(ri). The shear strengths between Palacos E bone cement and stainless steel rods were measured using an Instron materials testing machine. We found that cement can "flow" into the surface microtopography and establish good contact with the metal surface. The results show that the interfacial strength increases monotonically with the increase of R(Deltaq) instead of with R(a). The relationship between interfacial strength and surface parameters shows that a metal stem with an isotropic surface texture, higher R(Deltaq), and greater R(ri) gives a higher interfacial strength.

Biocompatible Materials↗
PubMed2006

Development of quantitative structure-binding affinity relationship models based on novel geometrical chemical descriptors of the protein-ligand interfaces.

Novel geometrical chemical descriptors have been derived on the basis of the computational geometry of protein-ligand interfaces and Pauling atomic electronegativities (EN). Delaunay tessellation has been applied to a diverse set of 517 X-ray characterized protein-ligand complexes yielding a unique collection of interfacial nearest neighbor atomic quadruplets for each complex. Each quadruplet composition was characterized by a single descriptor calculated as the sum of the EN values for the four participating atom types. We termed these simple descriptors generated from atomic EN values and derived with the Delaunay Tessellation the ENTess descriptors and used them in the variable selection k-nearest neighbor quantitative structure-binding affinity relationship (QSBR) studies of 264 diverse protein-ligand complexes with known binding constants. Twenty-four complexes with chemically dissimilar ligands were set aside as an independent validation set, and the remaining dataset of 240 complexes was divided into multiple training and test sets. The best models were characterized by the leave-one-out cross-validated correlation coefficient q(2) as high as 0.66 for the training set and the correlation coefficient R(2) as high as 0.83 for the test set. The high predictive power of these models was confirmed independently by applying them to the validation set of 24 complexes yielding R(2) as high as 0.85. We conclude that QSBR models built with the ENTess descriptors can be instrumental for predicting the binding affinity of receptor-ligand complexes.

Computer Simulation↗
PubMed1999

Diversity of bacterial strains degrading hexadecane in relation to the mode of substrate uptake.

The relative distribution of the modes of hydrocarbon uptake, used by bacteria of the environment for the degradation of long-chain alkanes, has been evaluated. The first mode of uptake, direct interfacial accession, involves contact of cells with hydrocarbon droplets. In the second mode, biosurfactant-mediated transfer, cell contact takes place with hydrocarbons emulsified or solubilized by biosurfactants. Sixty-one strains growing on hexadecane were isolated from polluted and non-polluted soils and identified. The majority (61%) belonged to the Corynebacterium-Mycobacterium-Nocardia group. Criteria selected for characterizing hexadecane uptake were cell hydrophobicity, interfacial and surface tensions and production of glycolipidic extracellular biosurfactants. These properties were determined in flask cultures on an insoluble (hexadecane) and on a soluble (glycerol or succinate) carbon source for a subset of 23 representative strains. Exclusive direct interfacial uptake was utilized by 47% of studied strains. A large proportion of strains (53%) produced biosurfactants. The data on cellular hydrophobicity suggested the existence of two distinct alkane transfer mechanisms in this group. Accordingly, tentative assignments of biosurfactant-mediated micellar transfer were made for 11% of the isolated strains, and of biosurfactant-enhanced interfacial uptake for 42%.

Alkanes↗
PubMed1997

Structural aspects of interfacial adsorption. A crystallographic and site-directed mutagenesis study of the phospholipase A2 from the venom of Agkistrodon piscivorus piscivorus.

Recent genetic and structural studies have shed considerable light on the mechanism by which secretory phospholipases A2 interact with substrate aggregates. Electrostatic forces play an essential role in optimizing interfacial catalysis. Efficient and productive adsorption of the Class I bovine pancreatic phospholipase A2 to anionic interfaces is dependent upon the presence of two nonconserved lysine residues at sequence positions 56 and 116, implying that critical components of the adsorption surface differ among enzyme species (Dua, R., Wu, S.-K., and Cho, W. (1995) J. Biol. Chem. 270, 263-268). In an effort to further characterize the protein residues involved in interfacial catalysis, we have determined the high resolution (1.7 A) x-ray structure of the Class II Asp-49 phospholipase A2 from the venom of Agkistrodon piscivorus piscivorus. Correlation of the three-dimensional coordinates with kinetic data derived from site-directed mutations near the amino terminus (E6R, K7E, K10E, K11E, and K16E) and the active site (K54E and K69Y) defines much of the interface topography. Lysine residues at sequence positions 7 and 10 mediate the adsorption of A. p. piscivorus phospholipase A2 to anionic interfaces but play little role in the enzyme's interaction with electrically neutral surfaces or in substrate binding. Compared to the native enzyme, the mutant proteins K7E and K10E demonstrate comparable (20-fold) decreases in affinity and catalysis on polymerized mixed liposomes of 1-hexadecanoyl-2-(1-pyrenedecanoyl)-sn-glycero-3-phosphocholine and 1,2-bis[12-(lipoyloxy)dodecanoyl]-sn-glycero-3-phosphoglycerol, while the double mutant, K7E/K10E, shows a more dramatic 500-fold decrease in catalysis and interfacial adsorption. The calculated contributions of Lys-7 and Lys-10 to the free energy of binding of A. p. piscivorus phospholipase A2 to anionic liposomes (-1.8 kcal/mol at 25 degrees C per lysine) are additive (i.e. -3.7 kcal/mol) and together represent nearly half of the total binding energy. Although both lysine side chains lie exposed at the edge of the proposed interfacial adsorption surface, they are geographically remote from the corresponding interfacial determinants for the bovine enzyme. Our results confirm that interfacial adsorption is largely driven by electrostatic forces and demonstrate that the arrangement of the critical charges (e.g. lysines) is species-specific. This variability in the topography of the adsorption surface suggests a corresponding flexibility in the orientation of the active enzyme at the substrate interface.

Adsorption↗
PubMed2006

Investigation and characterization of liquid two-phase systems for the separation of crystal mixtures by interfacial partitioning.

The interfacial partitioning behavior of ampicillin and phenylglycine crystals in different two-phase systems has been investigated. The two-phase systems employed are water/dodecane, water/1-butanol, and water/pentane/methanol. By means of partition experiments and microscopic imaging, it has been shown that the mechanism of separation strongly depends on the choice of the two-phase system. While water/dodecane features a mechanism of sheer competitive adsorption at the interface, separation in water/1-butanol is mainly due to partitioning into both liquid phases, leading to a higher degree of separation. Experiments with water/pentane/methanol have illustrated the large potential of three-component systems, as slight variations in the composition can have large effects on the separation.

1-Butanol↗
PubMed2003

In vivo histological response to anodized and anodized/hydrothermally treated titanium implants.

In the study, characterization of the anodized titanium surface was performed. In addition, histological evaluation and interfacial strength at the bone-implant interface of the characterized surfaces were then evaluated with the use of a rabbit model at 6 and 12 weeks after implantation. Surface treatments consisted of either anodization or anodization followed by hydrothermal treatments. Nontreated titanium surfaces were used as controls in this study. Using scanning-electron microscopy, porous oxide layers were observed on surfaces of anodized titanium implants, whereas porous oxide layers and HA needles were observed on anodized titanium implants following hydrothermal treatments. X-ray diffraction analysis showed the oxide layers were consisted mainly of anatase and a little of rutile. By the hydrothermal treatment on the anodizing surface, HA peaks, as well as the peaks of anatase and trace amounts of rutile peaks were observed. In EPMA analysis, the Ca/P ratio for the anodic oxide was 1.54 for anodized surfaces, whereas the Ca/P ratios for HA needles and the anodic oxide were 1.64 and 0.57, respectively, for anodized surfaces following hydrothermal treatments. Although no significant difference was observed for the percent bone contact on all implants evaluated in the in vivo study, the removal torque strength was significantly higher for anodized implants (48.02+/-5.92 N/cm) than the untreated implants (controls) (27.83+/-1.78 N/cm) at 6 weeks after implantation. As such, it was concluded that the surface anodized implants resulted in a high interfacial strength at an early implantation period as compared to the nontreated titanium implants.

Animals↗
PubMed2003

Stabilizing bolaform amphiphile interfacial assemblies by introducing mesogenic groups.

We describe the synthesis and characterization of the mesogen-bearing bolaform amphiphile 4,4'-dihydroxybiphenylbis(11-pyridinium-N-yl-undecanoic ester) dibromide (BP-10) and its solid/liquid interfacial self-assembly. Cylindrical micelles are directly observed by atomic force microscopy (AFM) at the interface between mica and the aqueous solution above the critical micelle concentration (cmc). In situ and ex situ AFM studies indicate that the cylindrical micelles are stable both at the mica/solution interface and in the dry state. The enhanced stability of the micellar structures enables a detailed investigation of their self-assembly behavior and supramolecular structures at the interface. The adsorption model proposed here is supported by the variation of the interfacial self-assemblies on changing the solution concentration and substrate temperature.

Journal Article↗
PubMed2004

Nonanalytic curvature contributions to solvation free energies: influence of drying.

We investigate the solvation of a hard spherical cavity, of radius R, immersed in a fluid for which the interparticle forces are short ranged. For thermodynamic states lying close to the liquid binodal, where the chemical potential deviation deltamu is identical with mu-muco(T) is very small and positive, complete wetting by gas (drying) occurs and two regimes of interfacial behavior can be identified. These are characterized by the length scale Rc=2gamma(gl)infinity/(Deltarhodeltamu), where gamma(gl)infinity is the planar gas-liquid surface tension and Deltarho is the difference in coexisting densities at temperature T. For R>Rc, the interfacial free energy and the density profile of the fluid near the hard wall can be expanded in powers of the curvature R(-1), in keeping with the analysis of Stillinger and Cotter [J. Chem. Phys. 55, 3449 (1971)]. In the other regime, R 0, of the work of formation of a hard spherical cavity and of the Gibbs adsorption and the fluid density at contact with the wall. Our analysis, which is based on an effective interfacial Hamiltonian combined with exact statistical mechanical sum rules, is confirmed fully by the results of microscopic density functional calculations for a square-well fluid. We discuss the repercussions of our results for solvation phenomena, emphasizing that nonanalytic behavior equivalent to that we find for complete drying in solvophobic systems will also arise in the case of complete wetting, i.e. when liquid films are adsorbed on the surface of large (colloidal) particles or at curved substrates. We reassess various results in the important but neglected Stillinger-Cotter paper, where drying was not considered explicitly, in the light of our present analysis.

Journal Article↗
PubMed1996

The role of scanning probe microscopy in drug delivery research.

The success of a drug delivery system is often dependent on the surface properties of the device. These surface properties will determine the complex dynamic interfacial events that occur when the system is introduced into the aqueous environment of a patient. Development of the scanning probe microscopes has provided a number of very powerful new surface analytical techniques that are making a significant contribution to the characterization of drug delivery systems and the interfacial processes that occur when such systems are exposed to aqueous living environments. In this review, we describe the design and attributes of these instruments and discuss the impact of the techniques on a wide range of drug delivery research. The scanning probe microscopes are providing new insights into important problems concerning drug delivery, including the molecular structure of polymeric biomaterial surfaces, the conformation of target biomolecules, the influence of morphology on biodegradation, the adsorption of proteins to synthetic surfaces, and the structure and interactions of colloidal particles. As the whole field of scanning probe microscopy continues to advance, drug delivery research is set to benefit; in the final section of the review, the future potential derived from the ability to characterize new surface properties under aqueous conditions is discussed.

Drug Delivery Systems↗
PubMed1988

Technique for preparing cross-section transmission electron microscopy specimens from ceramic oxide braze joints.

A method for preparing cross-section transmission electron microscopy specimens from alumina and partially stabilized zirconia braze joints is described. The technique relies on masking a mechanically dimpled 3-mm disc in order to avoid preferential thinning of the metallic braze filler alloy during ion milling. The results presented show that specimens made by this technique are suitable for characterizing the fine microstructural details of interfacial reactions at oxide surfaces that occur during brazing.

Ceramics↗
PubMed1999

Chaotic Dynamics in a Percolation Model for Evaporation of a Solid Body: A Description of Solid/Gas Reactions with Consumption Based on Thermodiffusive Nonlinearity at the Solid/Gas Interface.

A nonlinear truncated model, concerning thermodiffusive chaos in gaseous media, has been employed to represent evaporation of a solid body on the basis of nonlinearity at the solid/gas interface. Solid/gas consumption has been described in the cell which is characterized by the wavenumber of the interfacial convective motion. The solid molecule/atom evaporates according to a Boltzmann law that is ruled by temperature profiles coming from the truncated model. This allows the interpretation of the evaporative mechanism as depending on a Poincaré map related to the interfacial dynamics and suggests a possible correspondence between kinetics and nonlinear cooperative regimes. Percolative properties (k-th moments, critical threshold and exponents, fractal dimension) of the evaporating solid path have been derived for different thermal levels (i.e., reactivity), namely, for different values of the reduced Rayleigh number (r), which in the model accounts for the temperature contribution. The achieved descriptions generally agree with microstructural and theoretical observations concerning gasification of reacting solid/fluid systems. Moreover, previously proposed kinetic data (i.e., gasification rate versus fractional conversion) of char/air reactions have been interpreted in terms of a percolation theory that involves the solid/gas reactivity and the order of the convective mode (i.e., wavenumber). This result resembles the so-called finite amplitude cellular convection in gaseous and liquid layers working in nonlinear regimes. Copyright 1999 Academic Press.

Journal Article↗
PubMed1976

The effect of cholesterol on the viscosity of protein-lipid monolayers.

The addition of cholesterol to a layer of lipids in a membrane structure is generally believed to result in an increase in the viscosity of the layer. We have shown that cholesterol and two other monolayer-forming lipids markedly decrease the viscosity of a serum albumin monolayer at the decane-water interface, a model membrane system. However, when the protein monolayer already has a surface active lipid component present, the effect of added cholesterol depends upon the other substance. When the albumin monolayer contains tristearin, added cholesterol increases the viscosity. When the lipid is octadecanol, cholesterol decreases the viscosity. The dependence of the change in interfacial viscosity due to cholesterol upon the original composition of the interfacial layer may be useful for characterizing the composition of layers of unknown composition, e.g. some natural membranes.

Cholesterol↗
PubMed1999

Surface-induced polymerization of actin.

Living cells contain a very large amount of membrane surface area, which potentially influences the direction, the kinetics, and the localization of biochemical reactions. This paper quantitatively evaluates the possibility that a lipid monolayer can adsorb actin from a nonpolymerizing solution, induce its polymerization, and form a 2D network of individual actin filaments, in conditions that forbid bulk polymerization. G- and F-actin solutions were studied beneath saturated Langmuir monolayers containing phosphatidylcholine (PC, neutral) and stearylamine (SA, a positively charged surfactant) at PC:SA = 3:1 molar ratio. Ellipsometry, tensiometry, shear elastic measurements, electron microscopy, and dark-field light microscopy were used to characterize the adsorption kinetics and the interfacial polymerization of actin. In all cases studied, actin follows a monoexponential reaction-limited adsorption with similar time constants (approximately 10(3) s). At a longer time scale the shear elasticity of the monomeric actin adsorbate increases only in the presence of lipids, to a 2D shear elastic modulus of mu approximately 30 mN/m, indicating the formation of a structure coupled to the monolayer. Electron microscopy shows the formation of a 2D network of actin filaments at the PC:SA surface, and several arguments strongly suggest that this network is indeed causing the observed elasticity. Adsorption of F-actin to PC:SA leads more quickly to a slightly more rigid interface with a modulus of mu approximately 50 mN/m.

Actins↗