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PubMed2002

Discovery of highly potent Src SH2 binders: structure-activity studies and X-ray structures.

Optimization of the hydrophobic moiety of caprolactam/thiazepinone based compounds led to the identification of potent Src SH2 binders in two different series incorporating a phosphotyrosine group (RU 81843) or a phosphobenzoic group (RU 79181). The X-ray co-structures with the Src SH2 domain revealed different binding modes for RU 81843 and RU 79181, and an excellent fit between RU81843 and the Src SH2 protein thus explaining its high potency (9 nM, 15-fold more potent than pYEEI reference peptide).

Benzoates↗
PubMedDate not supplied

New polymers forming aqueous two-phase polymer systems.

A new type of polymer, starch-modified by acrylamide, has been developed for application in aqueous two-phase systems (ATPS) for protein separation. Partial hydrolysis and acrylamide modification of starch to different degrees make it suitable for forming ATPS with poly(ethylene glycol) in a moderate concentration range. The potential of the polymer to form ATPS with the thermoprecipitating copolymer of 1-vinylimidazole with N-vinylcaprolactam (poly-VI/VCL) has been evaluated. The thermoprecipitation properties of poly-VI/VCL and Cu(II)-loaded poly-VI/VCL have been studied for application in metal affinity partitioning. The formation of ATPS with Cu(II)-loaded thermoprecipitating copolymer was critically achieved for poly-VI/VCL (10/90) copolymer in under-loaded metal concentrations. With the Cu(II)-loaded copolymer, poly-VI/VCL in the top phase and modified starch in the bottom phase, the ATPS formed was used for the purification of alpha-amylase inhibitor from wheat meal. The protein partitioned in the top phase and phase-separated polymer-protein complex could be precipitated by salt. The protein inhibitor was recovered with a yield of 75%.

Acrylamide↗
PubMed2007

High-yield activation of scaffold polymer surfaces to attach cell adhesion molecules.

Zirconium tetra(tert-butoxide) reacts with surface amide groups of polyamide nylon 6/6 to give (eta(2)-amidate)zirconium complexes in high yield. These surface complexes react to bond the cell-adhesive peptide arginine-glycine-aspartic acid (RGD) to the polymer surface. A surface loading of 0.18 nmol/cm(2) of RGD is achieved, which is 20-1000 times higher than previously reported attainable on natural or synthetic polymers by other strategies. Approximately 40% of the nylon surface is covered by the RGD, which gives a surface that is both stable to hydrolysis and highly active for cell adhesion and spreading in vitro.

Animals↗
PubMed2005

Selective measurement of heteronuclear 1H-13C dipolar couplings in motionally heterogeneous semicrystalline polymer systems.

A pulse sequence for the selective recoupling of heteronuclear dipolar interactions in mobile amorphous phase of powdered semicrystalline polymers is described. 1H-13C dipolar interactions are selectively measured by PISEMA-type sequence. Selection of 13C magnetization originating from amorphous phase is achieved by a train of saturation pulses followed by a short delay and a direct excitation pulse on 13C spins. The development of undesired net 13C magnetization during the recoupling sequence is prevented by the efficient "reverse" 13C --> 1H cross-polarization. The efficacy of the 2D method to measure 1H-13C dipolar couplings selectively for mobile components is demonstrated on powdered crystalline L-alanine, semicrystalline polyethylene, and nanocomposite polyamide-6/montmorillonite.

Alanine↗
PubMed2004

Neutron reflectivity and external reflection FTIR studies of DL-aspartic acid crystallization beneath nylon 6 spread films.

The crystallization of DL-aspartic acid beneath nylon 6 spread films has been studied for 150% supersaturated systems using neutron reflectivity and external reflection FTIR. The neutron reflectivity data showed the gradual incorporation of DL-aspartic acid within a nylon 6 spread film layer over a period of 6-8 h, culminating in over 50 vol % of the "film" layer comprising DL-aspartic acid. Accumulation of further DL-aspartic acid material to produce microscopic/macroscopic surface crystals occurred, but on a more limited scale, resulting in approximately 1-5% surface coverage of crystals over the same period. External reflection FTIR studies revealed very weak bands attributable to DL-aspartic acid in surface regions devoid of visible crystals, in agreement with the neutron reflectivity studies. In regions with visible crystals, much larger and sharper DL-aspartic acid bands were seen. Changes in the intensity of the nylon 6 NH stretch band were often observed during the visible crystallization and dissolution of DL-aspartic acid and were consistent with the reversible accumulation of nylon 6 around the growing crystals.

Aspartic Acid↗
PubMed2005

Core-shell nanostructures from single poly(N-vinylcaprolactam) macromolecules: stabilization and visualization.

Formation of core-shell poly(N-vinylcaprolactam) (PVCL) single-molecule nanostructures due to interaction of PVCL with metal ions was studied using transmission electron microscopy, 13C NMR, and light scattering. This study demonstrates that addition of CoCl2 to PVCL in its globular conformation yields unimolecular core-shell polymer particles with the core decorated with Co(II) ions. The crucial condition for formation of well-defined unimolecular nanostructures is the presence of stable globular aggregates in aqueous solution. Moreover, the metal ions should have a sufficiently high coordination number (higher than 2) to provide a cross-linking and stabilization of the core.

Caprolactam↗
PubMed2003

Characterization of the thermal properties of powder particles using microthermal analysis.

PURPOSE: Microthermal analysis is a recently introduced thermoanalytical technique whereby discrete regions of complex samples may be scrutinized at micron or submicron resolution. In this investigation, the novel use of the technique to study individual powder particles is described. METHODS: A TA Instruments microthermal analyzer was used in local thermal analysis mode using a heating rate of 10 degrees C/s. Powder samples of crystalline ibuprofen, spray-dried salbutamol sulphate, spray-dried and crystalline trehalose, and two polymorphic forms of indometacin were studied using differential scanning calorimetry as a supportive technique as appropriate. RESULTS: The ibuprofen showed a probe position discontinuity corresponding to the melting point of the material. Spray-dried salbutamol sulphate showed a discontinuity corresponding to decomposition but not to the glass transition, whereas both crystalline and amorphous trehalose showed a single discontinuity corresponding to physical collapse of the material. Studies using the alpha and gamma forms of indometacin showed that the technique was able to distinguish between the two polymorphic forms. CONCLUSION: The study suggests that micro-TA may be used to assess interparticulate composition and homogeneity.

Albuterol↗
PubMed2003

Electrostatic self-assembly of macroscopic crystals using contact electrification.

Self-assembly of components larger than molecules into ordered arrays is an efficient way of preparing microstructured materials with interesting mechanical and optical properties. Although crystallization of identical particles or particles of different sizes or shapes can be readily achieved, the repertoire of methods to assemble binary lattices of particles of the same sizes but with different properties is very limited. This paper describes electrostatic self-assembly of two types of macroscopic components of identical dimensions using interactions that are generated by contact electrification. The systems we have examined comprise two kinds of objects (usually spheres) made of different polymeric materials that charge with opposite electrical polarities when agitated on flat, metallic surfaces. The interplay of repulsive interactions between like-charged objects and attractive interactions between unlike-charged ones results in the self-assembly of these objects into highly ordered, closed arrays. Remarkably, some of the assemblies that form are not electroneutral-that is, they possess a net charge. We suggest that the stability of these unusual structures can be explained by accounting for the interactions between electric dipoles that the particles in the aggregates induce in their neighbours.

Caprolactam↗
PubMed1997

The antihypertensive effect of orally administered nifedipine-loaded nanoparticles in spontaneously hypertensive rats.

1. The therapeutic use of nifedipine is limited by the rapidity of the onset of its action and its short biological half-life. In order to produce a form devoid of these disadvantages we made nanoparticles of nifedipine from three different polymers, poly-epsilon-caprolactone (PCL), polylactic and glycolic acid (1:1) copolymers (PLAGA), and Eudragit RL/RS (Eudragit). Nifedipine in polyethylene glycol 400 (PEG) solution was used as a control. 2. The average diameters of the nanoparticles ranged from 0.12 to 0.21 micron; the encapsulation ratio was 82% to 88%. 3. In spontaneously hypertensive rats (SHR), the initial rapid fall in systolic arterial blood pressure following oral administration of nifedipine in PEG solution (from 193 +/- 3 to 102 +/- 2 mmHg) was not seen following administration of the same dose in Eudragit nanoparticles (from 189 +/- 2 to 156 +/- 2 mmHg); with PCL and PLAGA nanoparticles the initial fall in blood pressure was significantly reduced (nadirs PCL 124 +/- 2 and PLAGA 113 +/- 2 mmHg). Ten hours following administration, blood pressure in rats administered the nifedipine/PEG preparation had returned to normal (183 +/- 3 mmHg) whereas that of animals given nifedipine in nanoparticles (PCL 170 +/- 3, PLAGA 168 +/- 2, Eudragit 160 +/- 3 mmHg) was still significantly reduced. 4. All of the nanoparticle dosage forms decreased Cmax and increased Tmax and the mean residence time (MRT) values. Relative bioavailability was significantly increased with Eudragit nanoparticles compared to the nifedipine/PEG solution. 5. There was an inverse linear correlation between the fall in blood pressure and plasma nifedipine concentration with all preparations. 6. The nanoparticle nifedipine preparations represent sustained release forms with increased bioavailability, a less pronounced initial antihypertensive effect and a long-lasting action.

Acrylic Resins↗
PubMed2000

Nitrilase of Rhodococcus rhodochrous J1. Conversion into the active form by subunit association.

Nitrilase-containing resting cells of Rhodococcus rhodochrous J1 converted acrylonitrile and benzonitrile to the corresponding acids, but the purified nitrilase hydrolyzed only benzonitrile, and not acrylonitrile. The activity of the purified enzyme towards acrylonitrile was recovered by preincubation with 10 mM benzonitrile, but not by preincubation with aliphatic nitriles such as acrylonitrile. It was shown by light-scattering experiments, that preincubation with benzonitrile led to the assembly of the inactive, purified and homodimeric 80-kDa enzyme to its active 410-kDa aggregate, which was proposed to be a decamer. Furthermore, the association concomitant with the activation was reached after dialysis of the enzyme against various salts and organic solvents, with the highest recovery reached at 10% saturated ammonium sulfate and 50% (v/v) glycerol, and by preincubation at increased temperatures or enzyme concentrations.

Acrylonitrile↗
PubMedDate not supplied

[Osseontegration of trial implants of carbon fiber reinforced plastics].

PROBLEM: To what extent are carbon fibre-reinforced plastics (CFRP) suitable as an osseous integration surface for implants? METHOD: CFRP test implants having a plexus-structured, rhombus-structured, and plexus-structured, hydroxyapatite surface were implanted in the femura of mini-plgs. Exposure time lasted 12 weeks. The implants were subjected to a macroradiological, a histological-histomorphometrical, and a fluorescence-microscopical evaluation. RESULTS: One half of the uncoated, plexus-structured implants were not osteointegrated, the other half displayed an osteointegration rate of 11.8% in the spongy area and 29.8% in the cortex layer. The HA-coated test implants showed an osteointegration of 29.5% in the spongiosa and 56.8% in the cortex layer. The rhombus-structured test implants had an osteointegration of 29.2% (spongiosa) and 46.2% (cortex layer). CONCLUSION: Compared to the osteointegration of metallic, especially titanium surfaces the CFRP surfaces tested by us fared worse, especially the uncoated, plexus-structured surfaces. For this reason we view very critically the use of carbon-fibre reinforced plastics together with the surfaces tested by us as osteointegrating surfaces.

Animals↗
PubMed2005

Feasibility study for the development of certified reference materials for specific migration testing. Part 2: estimation of diffusion parameters and comparison of experimental and predicted data.

This paper describes the second part of a project whose main objective was to develop the know-how to produce certified reference materials (CRMs) for specific migration testing. Certification parameters discussed are the diffusion coefficient, D(P), the respective polymer-specific coefficient, A(P), of the migrant polymer combinations and the partitioning coefficient, K(P,F), describing the partitioning of the migrant between the polymer and a food simulant. The parameters were determined for 16 preliminary candidate CRMs. Each parameter was determined by one laboratory. The six materials most suitable as reference materials were selected and the parameters then determined by four laboratories. The coefficients resulting from this small-scale interlaboratory comparison study can be regarded as the most reliable values available to date. These coefficients were applied for a comparison of experimental and predicted migration data. The experimental migration data arose from the same project and were determined by one laboratory for the first 16 materials and subsequently by four laboratories for the six materials selected in the second phase. Overall, experimental and predicted migration data fit together quite well. Roughly half of the predicted data were within +/-10%; almost all predicted data were within +/-40% compared with the experimental data.

Benzophenones↗
PubMedDate not supplied

The effect of solvent removal conditions on performance and release property of protein-loaded microparticles.

This study was designed to investigate the influence of solvent removal conditions on the performance and release properties of protein-loaded poly(epsilon-caprolactone) microparticles. The microparticles were prepared by the coacervation method in three different conditions. The effects of vacuum pressure, fabrication temperature and evaporation time on the crystallinity, surface morphology, particle size as well as the yield of microparticles, encapsulation efficiency of BSA and in vitro release property were investigated. There was no significant difference in the size of microparticles prepared by varying the vacuum pressure and temperature. Similar results were obtained for the production yield of microparticles and the loading efficiency of protein in these microparticles. However, accelerating the evaporation rate of solvent significantly reduced the crystallinity of polymer from 54.13 +/- 2.67% down to 44.64 +/- 2.17% (p < 0.05). The release of protein from the resulting microparticles was rapid, within 6 h, after which BSA was continuously and slowly released for up to 7 days. The protein release rate and polymer crystallinity possessed a good correlation (r = -0.951). This result indicated that the higher the crystallinity, the slower the release rate. In other words, change in vacuum pressure and temperature reduced the crystallinity of polymer, which was feasible for protein to release from amorphous domain in microparticles.

Caprolactam↗
PubMed2006

Temperature limit values for touching cold surfaces with the fingertip.

OBJECTIVES: At the request of the European Commission and in the framework of the European Machinery Directive, research was performed in five different laboratories to develop specifications for surface temperature limit values for the short-term accidental touching of the fingertip with cold surfaces. METHODS: Data were collected in four laboratories with a total of 20 males and 20 females performing a grand total of 1655 exposures. Each touched polished blocks of aluminium, stainless steel, nylon-6 and wood using the distal phalanx of the index finger with a contact force of 1.0, 2.9 and 9.8 N, at surface temperatures from +2 to -40 degrees C for a maximum duration of 120 s. Conditions were selected in order to elicit varying rates of skin cooling upon contact. Contact temperature (TC) of the fingertip was measured over time using a T-type thermocouple. RESULTS: A database obtained from the experiments was collated and analysed to characterize fingertip contact cooling across a range of materials and surface temperatures. The database was subsequently used to develop a predictive model to describe the contact duration required for skin contact temperature to reach the physiological criteria of onset of pain (15 degrees C), onset of numbness (7 degrees C) and onset of frostbite risk (0 degrees C). CONCLUSIONS: The data reflect the strong link between the risk of skin damage and the thermal properties of the material touched. For aluminium and steel, skin temperatures of 0 degrees C occurs within 2-6 s at surface temperatures of -15 degrees C. For non-metallic surfaces, onset of numbness occurs within 15-65 s of contact at -35 degrees C and onset of cold pain occurs within 5 s of contact at -20 degrees C. The predictive model subsequently developed was a non-linear exponential expression also reflecting the effects of material thermal properties and initial temperature. This model provides information for the protection of workers against the risk of cold injury by establishing the temperature limits of cold touchable surfaces for a broad range of materials, and it is now proposed as guidance values in a new international standard.

Adolescent↗
PubMed1993

Humidity-conditioned gravimetric method to measure the water content of hydrogel contact lens materials.

A method to determine the humidity-conditioned gravimetric water content of hydrogel contact lens materials has been developed, in which errors due to blotting have been eliminated by conditioning the lens in a series of relative humidity (RH) environments before measuring the water content gravimetrically, and then extrapolating the water content to 100% RH. This method has been used to determine the water contents of representative materials from each of the four FDA lens groups, which were compared with their labeled values, as well as with values obtained from refractive index measurements. The deviation of the water content of soft contact lenses as measured by refractive index from that obtained gravimetrically increased as the water content decreased. The humidity-conditioned gravimetric method to determine water content of hydrophilic contact lenses is being proposed as an International Organization for Standardization (ISO) standard, as an improvement over the gravimetric and refractive index methods.

Caprolactam↗
PubMed1997

Critical effects and exposure limits.

The use of critical effects in the determination of occupational exposure limits (OELs) in Sweden is subjected to a statistical study. Many of the present OELs are high in relation to known no-effect levels and effect levels, and the degree of protection has a surprisingly weak correlation with the seriousness of the adverse effect. Several proposals for improved procedures are put forward. One of these is to supplement the concept of critical effects with that of dominant effects. A dominant effect of a substance is a health effect that is at some concentration the most serious health effect.

Acetone↗