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Physico-chemical parameters of new nitrate esters were carried out in order to contribute to the choice of a drug candidate for preclinical development. Thermal analysis (DSC), wettability and solubility of the compounds were investigated in this study.
Hydrophobic soils display resistance to wetting and frequently do not hold water to support good plant growth. A laboratory investigation was conducted to study moisture movement through hydrophobic soils. Test results indicated that hydrophobic soils have a critical moisture content beyond which they behave as wettable or hydrophilic soils. Soil hydrophobicity decreased and water infiltration increased when the soil was subjected to an increasing number of wetting and drying cycles. The effect of diluting hydrophobic soil with hydrophilic soil on water infiltration was also studied. The results indicated that water infiltration into soil becomes more rapid and uniform as the mass fraction of hydrophilic soil is increased in the mix. Water infiltration was observed even in hydrophobic-hydrophilic soil mixtures classified as severely water-repellent by commonly used arbitrary ordinal scales.
OBJECTIVES: To evaluate the dentin wetting by four adhesive systems and to relate the wetting properties with the adhesive efficiency. METHODS: Scotch Bond Multipurpose Plus (3M), Syntac Single-Component (Vivadent), One-Step (Bisco) and Heliobond (Vivadent) were used. The substrate was superficial and deep human dentin. Roughness and water contact angle were measured before and after acid etching. Dentin wetting by resins was studied by contact angle measurements as a function of time to evaluate the spreading time. The shear bond strength was evaluated following a single plane method, and the microleakage was evaluated in Class V cavities. RESULTS: Acid etching increased dentin roughness and wettability and no differences were found between acids tested. Dentin wetting and roughness was higher on deep dentin. Dentin wetting and shear bond strength of resins was similar except for Heliobond that displayed the lowest value. Microleakage was higher on the gingival wall, and the leaking was lowest for Scotch Bond Multipurpose Plus, and maximum for Heliobond. The spreading time exceeded 30s with water-based and hydrophobic adhesives, and was lower with an acetone-based adhesive. Dentin depth had some influence on contact angle and shear bond strength: contact angles obtained with SBMP and One-Step were higher on superficial dentin, and shear bond strength for One-Step was higher on superficial dentin. Dentin wetting by resins could be correlated to shear bond strength and microleakage. SIGNIFICANCE: Dentin acid etching with different conditioners promotes similar roughness and wetting changes. On a similar substrate, the adhesion depends on the chemical and wetting characteristics of resins.
OBJECTIVES: This study was designed to assess: 1) the ability of several commercially available and laboratory-made acid etchants to penetrate occlusal fissures when used for pit and fissure sealing, and 2) the influence of adding a surfactant to the etchant on penetration of the sealer. Viscosity, surface tension and contact angle to enamel of the etchants were determined for each treatment, and these properties were related to the etchant's ability to penetrate fissures. METHODS: Penetration was assessed in an acrylic fissure model having a deep-narrow fissure using a microscope and a chronometer. Penetration depth was expressed as percentage of total fissure depth and was measured in intervals up to 90 s. Commercially available etching agents with different viscosities and two solutions of phosphoric acid (37%), one with and one without a surfactant, were tested. The etch pattern obtained on the fissure wall enamel of extracted teeth with some of these products was evaluated using scanning electron microscopy. Eventually, the penetration depths of a composite sealer in fissures treated with a conventional etchant were compared to those after application of a surfactant-containing etchant on sections of extracted teeth. RESULTS: None of the commercially available etchants studied were able to penetrate farther than 17% of the total fissure depth in the fissure model. The surfactant-containing etchant showed complete penetration within about 1 min and had a significantly lower surface tension and contact angle than the other products tested. Only the surfactant-containing etchant could produce a retentive pattern on the entire wall enamel of the fissure with the exception of locations blocked by debris and plaque. Fissures treated with this product prior to sealing showed a significantly deeper penetration of the sealer in deep-marrow fissures. SIGNIFICANCE: Surfactant-containing etchants with a low viscosity can penetrate completely into fissures and can produce an increased retentive and wettable surface which significantly increased sealant penetration into deep fissures.
In bioartificial organs using isolated cells, polymeric semipermeable membranes are used as immunoselective barriers as a means for cell oxygenation and also as substrata for adhesion of anchorage-dependent cells. The capacity of the membrane to perform its functions and to provide a cytocompatible support for cell culture depends in particular on its surface properties. In this study we investigated the physico-chemical aspects of the interaction between the membrane and mammalian cells in order to provide guidelines to the selection of cytocompatible membranes. We evaluated the adhesion and metabolic behaviour of isolated liver cells cultured on various polymeric membranes such as those modified by protein adsorption. The physico-chemical properties of the membranes were characterised by contact angle measurements. The different parameters such as acid (gamma+), base (gamma-) and Lifshitz-van der Waals (gammaLW) of the surface free energy were calculated according to Good-van Oss's model. The adsorption of protein modified markedly both contact angle and components of membrane surface tension. In particular, base parameter of surface tension decreased drastically with increased water contact angle. For each investigated membrane we observed that cell adhesion increased with increasing base parameter of membrane surface tension. The absolute value of cell adhesion is higher in the presence of serum proteins adsorbed on the membrane surface, which change the wettability by increasing the base parameter of surface tension. Also, the metabolic functions improve on hydrophilic membranes. Liver cells synthesised urea with a rate that increased with increasing base parameter value of membrane surface tension. The metabolic activity is particularly expressed at high levels when cells were cultured on polycarbonate and cellulose acetate membranes.
Polyethylene (PE) foils were implanted with 40 and 150 keV Ar+ ions to the fluences from 1 x 10(13) to 1 x 10(15) cm(-2). Production of conjugated double bonds, characterizing degradation of the PE surface layer, was studied using UV-VIS spectroscopy. Wettability of the PE surface, determined by conventional goniometric techniques, was shown to be an increasing function of both ion energy and fluence. It was also increased after exposure of PE to serum-supplemented cell culture media. Cell culture experiments showed that the ion irradiation significantly increased the adherence of vascular smooth muscle cells (VSMC) and their subsequent growth on the PE surface. On day 1 after seeding, the number of initially adhered VSMC exhibited two maxima. On day 3 after seeding. these maxima disappeared, which was partially due to a significantly shorter doubling time of VSMC. On the other ion-modified samples. the doubling time did not differ significantly from that on the unmodified PE. Enzyme-linked immunosorbent assay revealed increased concentration of talin, a protein of focal adhesion plaques, and alpha-actin, a marker of VSMC differentiation, in cells on ion-implanted surfaces. It can be concluded that the ion irradiation supports the adhesion and differentiation of VSMC without excessive proliferation of these cells.
The role of surface microtopography in combination with different surface wettability for rat calvaria cell differentiation was examined. Mineralization and alkaline phosphatase (ALP) activity of rat calvaria cells on flat polydimethylsiloxane (PDMS) or PDMS contained pyramids which were either hydrophilic or hydrophobic were compared. ALP expressing cells were more frequent on hydrophilic PDMS contained pyramids. ALP activity, peaked at day 9, was highest for hydrophilic pyramids followed by hydrophobic pyramids and flat hydrophilic PDMS surfaces. A similar pattern was obtained with respect to mineralized nodules. These observations showed that micro-sized surface features promote differentiation of rat calvaria cells. Further, hydrophilic surfaces are more prone to stimulate differentiation in comparison with hydrophobic surfaces. The results suggest that both material surface chemistry and topography affect osteoblast differentiation.
Amorphous carbon films have attracted much attention recently due to their good biocompatibility. Diamond-like carbon (DLC), one form of amorphous carbon that is widely used in many kinds of industries, has been proposed for use in blood contacting medical devices. However, the blood coagulation mechanism on DLC in a biological environment is not well understood. Platelet adhesion and activation are crucial events in the interactions between blood and the materials as they influence the subsequent formation of thrombus. In this work, the behavior of platelets adhered onto hydrogenated amorphous carbon films (a-C:H) is investigated. Hydrogenated amorphous carbon films with different hydrogen contents, structures, and chemical bonds were fabricated at room temperature using plasma immersion ion implantation-deposition (PIII-D). The wettability of the films was investigated by contact angle measurements using several common liquids. Platelet adhesion experiments were conducted to examine the interaction of blood with the films in vitro and the activation of adherent platelets. The results show that the behavior of the platelets adhered on the a-C:H films is influenced by their structure and chemical bond, and it appears that protein interaction plays a key role in the activation of the adherent platelets.
The aim of this work was to investigate the effect of the sterilization processes on the mineralization of titanium implants induced by incubation in various biological model fluids. Titanium samples were submitted to the following sterilization processes used for implant materials: steam autoclaving, glow discharge Ar plasma treatment and gamma-irradiation. The modification of the treated surfaces was evaluated by contact angle determinations, X-ray photoelectron spectroscopy (XPS), laser profilometry and X-ray diffraction. The most significant modifications were detected on the wettability: while the samples treated with Ar plasma became highly hydrophilic (water contact angle approximately 0 degrees), gamma-irradiation and steam sterilization induced an increase in the hydrophobicity. After being sterilized, the samples were incubated for one week in three biological model fluids: Hanks' Balanced Salt Solution, Kokubo's simulated body fluid (SBF) and a fluid, designated by SBF0, with the same composition of SBF but without buffer TRIS. The level of mineralization of the incubated Ti samples, assessed by dynamic contact angle analysis, scanning electron microscopy, electron dispersive spectroscopy and XPS, indicated that the early stages of mineralization are essentially independent of the sterilization method. In contrast, the incubating fluid plays a determinant role, SBFO being the most efficient medium for biomineralization of titanium.
Coumarin-endcapped tetrabranched liquid copolymers composed of epsilon-caprolactone and trimethylene carbonate (TMC), prepared using pentaerythritol or four-branched poly(ethylene glycol) (PEG) as an initiator, were ultraviolet irradiated to produce photocured solid biodegradable copolymers. The hydrolytic degradation behaviors of photocured films were determined from the weight loss of the films. The initial hydrolysis rate (determined for up to 24 h using a quartz crystal microbalance) was enhanced with aqueous solutions of higher pH. The hydrolysis rate in the early period of immersion was increased with an increase in TMC content, whereas that in the later period (week order) decreased with a increase in TMC content. This inverse relation of composition dependence on the hydrolysis rate between the early and late periods was discussed. Topological measurements using scanning electron microscopy and atomic force microscopy as well as depth profiles of the fluorescein-stained hydrolyzed layer showed that for the pentaerythritol-initiated copolymer, irrespective of copolymer composition, hydrolysis occurred at surface regions and surface erosion proceeded with immersion time. For PEG-based copolymers, both surface erosion and bulk degradation occurred simultaneously. The hydrolyzed surfaces became highly wettable with water and exhibited noncell adhesivity.
The aim of this study was to compare the initial adhesion forces of the uropathogen Enterococcus faecalis with the medical-grade polymers polyurethane (PU), polyamide (PA), and poly(tetrafluoroethylene) (PTFE). To quantify the cell-substrate adhesion forces, a method was developed using atomic force microscopy (AFM) in liquid that allows for the detachment of individual live cells from a polymeric surface through the application of increasing force using unmodified cantilever tips. Results show that the lateral force required to detach E. faecalis cells from a substrate differed depending on the nature of the polymeric surface: a force of 19 +/- 4 nN was required to detach cells from PU, 6 +/- 4 nN from PA, and 0.7 +/- 0.3 nN from PTFE. Among the unfluorinated polymers (PU and PA), surface wettability was inversely proportional to the strength of adhesion. AFM images also demonstrated qualitative differences in bacterial adhesion; PU was covered by clusters of cells with few cell singlets present, whereas PA was predominantly covered by individual cells. Moreover, extracellular material could be observed on some clusters of PU-adhered cells as well as in the adjacent region surrounding cells adhered on PA. E. faecalis adhesion to the fluorinated polymer (PTFE) showed different characteristics; only a few individual cells were found, and bacteria were easily damaged, and thus detached, by the tip. This work demonstrates the utility of AFM for measurement of cell-substrate lateral adhesion forces and the contribution these forces make toward understanding the initial stages of bacterial adhesion. Further, it suggests that initial adhesion can be controlled, through appropriate biomaterial design, to prevent subsequent formation of aggregates and biofilms.
This paper reports on the structural characteristics of microcontact printed oligo(ethylene glycol)-terminated alkanethiol layers, HS(CH2)15CONH-(CH2CH2O)6-H (hereafter EG6), on gold. Microwetting, contact angle goniometry, imaging null ellipsometry, and infrared reflection-absorption spectroscopy (IRAS) are used to characterize the printed EG6 layers, and the quality of these layers in terms of layer thickness and the crystallinity of the alkyl and ethylene glycol portions is compared with data obtained from analogous layers prepared by solution self-assembly. The outcome of the printing process is critically dependent on the experimental parameters used to prepare the patterns. It is found that high quality layers, consisting of densely packed all-trans alkyl chains terminated with relatively helical hexa(ethylene glycol) tails, are formed by inking the poly(dimethylsiloxane) (PDMS) stamp with a 1 mM EG6 solution and contacting it with gold for 15 min. The homogeneity of printed layers is not as good as the homogeneity of those prepared from solution under similar conditions, most likely because of simultaneous transfer of low molecular weight residues from the PDMS stamp. These residues, however, can be easily removed upon ultrasonication in ethanol without affecting the quality of the printed layer. Further on, the microscopic square-shaped bare gold patterns formed after microcontact printing (muCP) are subsequently filled with 16-hexadecanoic acid (hereafter THA) or HS(CH2)15CONH-(CH2CH2O)6-COOH (hereafter EG6COOH) to provide a microarray platform for further covalent attachment of biomolecules. Well-defined structures in terms of wettability contrast, sharpness, and height differences between the printed and back-filled areas are confirmed by imaging null ellipsometry and microscopic wetting.
Microfluidic devices are well suited for the miniaturization of biological assays, in particular when only small volumes of samples and reagents are available, short time to results is desirable, and multiple analytes are to be detected. Microfluidic networks (MFNs), which fill by means of capillary forces, have already been used to detect important biological analytes with high sensitivity and in a combinatorial fashion. These MFNs were coated with Au, onto which a hydrophilic, protein-repellent monolayer of thiolated poly(ethyleneglycol) (HS-PEG) was self-assembled, and the binding sites for analytes were present on a poly(dimethylsiloxane) (PDMS) sealing cover. We report here a set of simple methods to extend previous work on MFNs by integrating binding sites for analytes inside the microstructures of MFNs using microcontact printing (muCP). First, fluorescently labeled antibodies (Abs) were microcontact-printed from stamps onto planar model surfaces such as glass, Si, Si/SiO2, Au, and Au derivatized with HS-PEG to investigate how much candidate materials for MFNs would quench the fluorescence of printed, labeled Abs. Au coated with HS-PEG led to a fluorescence signal that was approximately 65% weaker than that of glass but provided a convenient surface for printing Abs and for rendering the microstructures of the MFNs wettable. Then, proteins were inked from solution onto the surface of PDMS (Sylgard 184) stamps having continuous or discontinuous micropatterns or locally inked onto planar stamps to investigate how the aspect ratio (depth:width) of microstructures and the printing conditions affected the transfer of protein and the accuracy of the resulting patterns. By applying a controlled pressure to the back of the stamp, Abs were accurately microcontact-printed into the recessed regions of MFNs if the aspect ratio of the MFN microstructures was lower than approximately 1:6. Finally, the realization of a simple assay between Abs (used as antigens) microcontact-printed in microchannels and Abs from solution suggests that this method could become useful to pattern proteins in microstructures for advanced bioanalytical purposes.
Staphylococcus epidermidis is among the most commonly isolated microbes from medical implant infections, particularly in the colonization of blood-contacting devices. We explored the relationships between surface wettability and root-mean-square roughness (Rq) on microbial adhesive strength to a substrate. Molecular-level interactions between S. epidermidis and a variety of chemically and texturally distinct model substrata were characterized using a cellular probe and atomic force microscopy (AFM). Substrata included gold, aliphatic and aromatic self-assembled monolayers, and polymeric and proteinaceous materials. Substrate hydrophobicity, described in terms of the water contact angle, was an insufficient parameter to explain the adhesive force of the bacterium for any of the surfaces. Correlations between adhesion forces and Rq showed weak relationships for most surfaces. We used an alternate methodology to characterize the texture of the surface that is based on a fractal tiling algorithm applied to images of each surface. The relative area as a function of the scale of observation was calculated. The discrete bonding model (DBM) was applied, which describes the area available for bonding interactions over the full range of observational scales contained in the measured substrate texture. Weak negative correlations were obtained between the adhesion forces and the area available for interaction, suggesting that increased roughness decreases bacterial adhesion when nano- to micrometer scales are considered. We suggest that modification of the DBM is needed in order to include discontinuous bonding. The adhesive strength is still related to the area available for bonding on a particular scale, but on some very fine scales, the bacteria may not be able to conform to the valleys or pits of the substrate. Therefore, the bonding between the bacterium and substrate becomes discontinuous, occurring only on the tops of ridges or asperities.
Viscous flow is familiar and useful, yet the underlying physics is surprisingly subtle and complex. Recent experiments and simulations show that the textbook assumption of 'no slip at the boundary' can fail greatly when walls are sufficiently smooth. The reasons for this seem to involve materials chemistry interactions that can be controlled--especially wettability and the presence of trace impurities, even of dissolved gases. To discover what boundary condition is appropriate for solving continuum equations requires investigation of microscopic particulars. Here, we draw attention to unresolved topics of investigation and to the potential to capitalize on 'slip at the wall' for purposes of materials engineering.
Wettability and hydration are determined for aircraft combustor and laboratory-made soots which are used as surrogates for the insoluble part of aircraft-generated black carbon particles in the upper troposphere (UT). The measured water/ice contact angles on the soot surfaces are in the range 60-80 degrees. Factors influencing the soot wetting show a tremendous dependence on the surface chemical composition and microstructure. Wetting characteristics of soots are directly related to its hydrophilicity. The inverse Kelvin effect is considered as a mechanism of ice nucleation which is facilitated by the soot agglomerated structure with interparticle cavities in which condensation takes place on the insoluble surface with a high water contact angle. Estimations of the critical supersaturations needed for the ice condensation growth of particles are provided to determine which of the wetting characteristics are required for cirrus cloud formation in ice saturated regions of the UT.
STATEMENT OF PROBLEM: Maximum wetting of ceramic by adhesive resin is required to achieve optimal adhesion of the resin to ceramic. It is unknown whether the adhesion of the resin to the ceramic is affected by the surface topography and wetting by water or the adhesive resin. PURPOSE: This study was designed to characterize the effect of surface topography on the wetting of ceramics by water and adhesive resin. MATERIALS AND METHODS: Three materials, a veneering ceramic, Eris (ERV), and 2 core ceramics, Empress 1 core ceramic (E1C) and an experimental core ceramic (EXC), were used. Four surface-roughening procedures were used. They included polishing through 1200-grit SiC paper (P), air abrasion with 50 microm Al(2)O(3) (A), etching with 5% hydrofluoric acid gel (E), and a combination of airborne particle abrasion and etching (A/E). Forty bar specimens (15 x 10 x 1.5 mm) were prepared from each material (N=120). Twelve groups of 10 specimens each were prepared for the 4 surface-roughening procedures. Advancing (theta(A)) and receding (theta(R)) contact angles were measured with a CAHN Dynamic Contact Analyzer, on the basis of the Wilhelmy plate technique, with water and adhesive resin. The work of adhesion (W(A)) by the probing media was calculated by use of advancing contact angle data. The data were analyzed by t testing, analysis of variance, and Duncan's tests (alpha=0.05) to determine the statistical significance of differences in the contact angles between ceramic and water or resin as a function of surface roughening. RESULTS: In general, the mean theta(A) values were higher than the mean theta(R) values except for groups of E or A/E specimens with water used as a probing medium. E and A/E treatments yielded the lowest contact angle values, followed by A and P treatments (P<.001). The E1C exhibited the highest mean contact angles, whereas EXC exhibited the lowest mean contact angle except for the theta(R) with resin. The corresponding values for ERV were between those of E1C and EXC except for theta(R) values with resin. The resin medium yielded higher mean contact angles than the water medium for the same surfaces. W(A) ranged from 62.9 to 145.2 mJ/m(2). CONCLUSIONS: Within the limitations of this study, etching or a combination of air abrasion and etching were comparably effective in increasing the surface area for bonding. The most wettable surface as measured by the resin medium was EXC, followed by ERV and E1C.
The objective of our study was to find mechanisms responsible for solubility enhancement of nifedipine in solid dispersions of vitamin E TPGS and/or solutol HS-15. Solid dispersions of nifedipine with selected polymers such as vitamin E TPGS, solutol HS-15, PEG(1,000), and lipocol C-10 of varying drug/polymer ratios were prepared by a fusion method. The solubility enhancement was found to be in the order of vitamin E TPGS > solutol HS-15 > lipocol C-10 > PEG(1,000). Lipocol C-10, with a similar hydrophilic-lipophilic value as vitamin E TPGS, showed a comparable retained solubility enhancement during saturation solubility studies but had lower dissolution profile. Overall, vitamin E TPGS showed the best solubility and dissolution performance, while solutol HS-15 and lipocol C-10 demonstrated moderate solubility enhancements. Solid dispersions of vitamin E TPGS as prepared by microfluidization technique initially showed slightly higher solubility compared with samples prepared by fusion method, but eventually it became the same as the study progressed. However, solid dispersion of solutol HS-15 as prepared by microfluidization demonstrated a significant, sustained increased in solubility over its sample when prepared by fusion method. Based on these results, we concluded that enhanced solubility using vitamin E TPGS and solutol HS-15 resulted from a partial conversion of crystalline drug to the amorphous form, increase in wettability of the drug by water soluble polymers, better separation of drug particles, micellar solubilization of drug by high concentrations of surfactant polymers, and interaction between polymer and drug at the molecular level.