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The use of histological techniques for the demonstration of ion exchange resins.

AIM: To establish the staining characteristics of certain ion exchange resins in histological material, with a view to enabling confident differential identification. METHODS: Various histological staining procedures were applied to selected pathological material and prepared agar blocks containing the cation exchange resin calcium polystyrene sulphonate and the anion exchange resin cholestyramine. RESULTS: Calcium polystyrene sulphonate uniquely stained strongly by a direct Schiff's reagent procedure without any preoxidation and by the Ziehl-Neelsen method. Cholestyramine was negative by the former method but stained strongly with a standard Congo red technique. CONCLUSIONS: These staining results are consistent with the known structure and properties of polystyrene sulphonate and cholestyramine resins. Polystyrene sulphonate resins have the virtually pathognomonic feature of direct Schiff positivity, while morphology, location, and strong non-birefringent Congo red positivity facilitate the identification of cholestyramine. It is possible that the intrinsic staining characteristics of cholestyramine may be lost once it has bound to its target.

Anion Exchange Resins↗

Effect of interchanging two composite resin system with a dentine adhesive.

There is a tendency to interchange dentine adhesives and composite resins when using composite resins for restorations. This study used marginal contraction gaps to test the effect of changing composite resins with a dentine adhesive. Cylindrical butt-joint cavities were prepared entirely in dentine using extracted human teeth. Two groups of control cavities (30 cavities per group) were restored with Prisma-Bond/Prisma-Fil and Heliobond/Heliomolar respectively. Two groups of test cavities (30 cavities per group) were restored using the dentine adhesive. Prisma Universal Bond with Prisma-Fil on one group and Prisma Universal Bond and Heliomolar in the other. Following thermocycling the marginal contraction gaps were measured and assessed. The results showed a significant reduction in marginal contraction gaps when using either composite resin with Prisma Universal Bond. This indicates a compatibility of both resins with the adhesive in this instance.

Acrylates↗

Separation of resin acids using cyclodextrin-modified capillary electrophoresis.

A cyclodextrin-modified capillary electrophoretic method has been developed for the analysis of eleven common resin acids using a pH 4.5, 20 mM sodium acetate buffer containing 10% acetonitrile, 20 mM methyl-beta-cyclodextrin (MECD) and 30 mM sulfobutylether-beta-cyclodextrin (SBCD) as buffer modifiers. At pH below their pKa (< 5.7-6.4) the resin acids were virtually unionized and insoluble; however, they formed water-soluble inclusion complexes with MECD (20 mM) or SBCD (30 mM) even at pH 4.5. The analytes were separated in 25 min and, with the exception of two pairs, 12- or 14-chlorodehydroabietic/12,14-dichlorodehydroabietic acid and dehydroabietic/palustric acid, the remaining resin acids were baseline-separated. Analysis time was significantly shortened (< 12 min) at pH 9.25 using 30 mM SBCD and 20 mM MECD in 20 mM sodium borate. Resin acids were baseline-separated with the exception of two pairs, pimaric/sandaracopimaric acid and 12- or 14-chlorodehydroabietic/abietic acid. The addition of 7.5% methanol to the running buffer resolved the abietic acid peak. Both HPLC and micellar capillary electrokinetic chromatography using 20 mM deoxycholic acid, 10% acetonitrile in 20 mM sodium borate, pH 9.25, failed to resolve the resin acids. The simple capillary electrophoretic method developed would be useful for the rapid separation and characterization of several important resin acids in pulp mill effluents and other contaminated samples.

Acetonitriles↗

Effect of silicon carbide whisker-silica heat treatment on the reinforcement of dental resin composites.

The strength and fracture resistance of dental resin composites need to be improved to extend their use to large stress-bearing crown and multiple-unit applications. Recent studies showed that the addition of ceramic whiskers significantly reinforced resin composites. The aim of the present study was to use a silicon carbide whisker-silica particle mixture to reinforce resin composites, and to investigate the effect of whisker-silica mixture heat-treatment on composite properties. The whiskers were blended with silica particles and were thermally fused in an attempt to roughen the whiskers for improved retention in the matrix. The mixtures were heat-treated at temperatures of 500, 650, 800, 950, and 1100 degrees C for 10 min, 30 min, and 3 h. The mixtures were then silanized, incorporated into a dental resin, and the paste was placed into 2 x 2 x 25 mm molds and heat-cured at 140 degrees C for 30 min. A 3-point flexural test was used to measure flexural strength and work-of-fracture. Two commercial indirect composites were tested as controls. Two-way ANOVA showed that there was no significant effect from temperature or time. Therefore, all the whisker-silica mixture samples were combined into one group (n = 96), and compared to composites filled with silica only or whisker only, and the two indirect control composites. The whisker-silica mixture group had a flexural strength (mean +/- SD) of (186 +/- 24) MPa, significantly higher than (99 +/- 29) MPa for silica only, (131 +/- 22) MPa for whisker only, and (109 +/- 23) MPa and (114 +/- 18) MPa for the two indirect composites (Tukey's multiple comparison test; family confidence coefficient = 0.95). Similar results were obtained on work-of-fracture. Scanning electron microscopy revealed rough fracture surfaces for the whisker-silica composites, indicating crack deflection and bridging by whiskers as toughening mechanisms. Whisker-silica mixture minimized whisker entanglement and enhanced whisker-resin bonding, resulting in substantially stronger and tougher dental resin composites.

Carbon Compounds, Inorganic↗

Reinforcement of acrylic denture base resin by incorporation of various fibers.

This study was designed to evaluate improvements in the mechanical properties of acrylic resin following reinforcement with three types of fiber. Polyester fiber (PE), Kevlar fiber (KF), and glass fiber (GF) were cut into 2, 4, and 6 mm lengths and incorporated at concentrations of 1, 2, and 3% (w/w). The mixtures of resin and fiber were cured at 70 degrees C in a water bath for 13 h, then at 90 degrees C for 1 h, in 70 x 25 x 15 mm stone molds, which were enclosed by dental flasks. The cured resin blocks were cut to an appropriate size and tested for impact strength and bending strength following the methods of ASTM Specification No. 256 and ISO Specification No. 1567, respectively. Specimens used in the impact strength test were reused for the Knoop hardness test. The results showed that the impact strength tended to be enhanced with fiber length and concentration, particularly PE at 3% and 6 mm length, which was significantly stronger than other formulations. Bending strength did not change significantly with the various formulations when compared to a control without fiber. The assessment of Knoop hardness revealed a complex pattern for the various formulations. The Knoop hardness of 3%, 6 mm PE-reinforced resin was comparable to that of the other formulations except for the control without fiber, but for clinical usage this did not adversely affect the merit of acrylic denture base resin. It is concluded that, for improved strength the optimum formulation to reinforce acrylic resin is by incorporation of 3%, 6 mm length PE fibers.

Acrylic Resins↗

Fourier Transform-Raman spectroscopic study of natural resins of archaeological interest.

Resins from several different genera are studied using Fourier transform (FT)-Raman spectroscopy. Tree resins can be broadly divided into those that contain diterpenoid components and those that contain triterpenoid components. The diterpenoid resins analyzed are from the genera Pinus, Cedrus, and Agathis (kauri resin) and the triterpenoid resins examined are samples from Pistacia, Boswellia (frankincense), and Commiphora (myrrh) genera. A protocol is developed to nondestructively distinguish diterpenoid and triterpenoid resins and to differentiate the genera within the two types. The effects of oxidation on the discrimination of the FT-Raman spectra are considered.

Archaeology↗

Thermal analysis of dental resins cured with blue light-emitting diodes (LEDs).

Thermal analysis was used to measure the characteristics of dental resins cured with the use of a new light-activation unit equipped with high illuminant blue light-emitting diodes (LEDs). The characteristics were compared with those of resins cured with the use of two conventional halogen lamp units. The prepared base monomer consisted of a mixture of Bis-GMA and TEGDMA (60:40 by weight), with 0.5 wt% CQ/DMPT or CQ/DMAEMA. The two experimental visible-light-cured resins were polymerized for 40 s. Differential scanning calorimetry (DSC) was used to examine the thermal characteristics of the cured resins. The activation energy for the decomposition of the dental resin was calculated from the peaks of the endothermic curves obtained when the specimens were heated at three different rates (5, 10, and 15 C/min) during DSC. The activation energies calculated for the LED-cured specimens were more than 220 kJ/mol; specimens cured with the use of the halogen units had activation energies of less than 192 kJ/mol. The Knoop hardness number (KHN) of the same specimens was measured, and was higher with the blue LED units than with halogen lamp units. Therefore, dental resins cured using blue LEDs have a higher degree of polymerization and more stable three-dimensional structures than those cured with halogen lamps.

Calorimetry, Differential Scanning↗

Accelerated aging studies of UHMWPE. I. Effect of resin, processing, and radiation environment on resistance to mechanical degradation.

The resin and processing route have been identified as potential variables influencing the mechanical behavior, and hence the clinical performance, of ultra-high molecular weight polyethylene (UHMWPE) orthopedic components. Researchers have reported that components fabricated from 1900 resin may oxidize to a lesser extent than components fabricated from GUR resin during shelf aging after gamma sterilization in air. Conflicting reports on the oxidation resistance for 1900 raise the question of whether resin or manufacturing method, or an interaction between resin and manufacturing method, influences the mechanical behavior of UHMWPE. We conducted a series of accelerated aging studies (no aging, aging in oxygen or in nitrogen) to systematically examine the influence of resin (GUR or 1900), manufacturing method (bulk compression molding or extrusion), and sterilization method (none, in air, or in nitrogen) on the mechanical behavior of UHMWPE. The small punch testing technique was used to evaluate the mechanical behavior of the materials, and Fourier transform infrared spectroscopy was used to characterize the oxidation in selected samples. Our study showed that the sterilization environment, aging condition, and specimen location (surface or subsurface) significantly affected the mechanical behavior of UHMWPE. Each of the three polyethylenes evaluated seem to degrade according to a similar pathway after artificial aging in oxygen and gamma irradiation in air. The initial ability of the materials to exhibit post-yield strain hardening was significantly compromised by degradation. In general, there were only minor differences in the aging behavior of molded and extruded GUR 1050, whereas the molded 1900 material seemed to degrade slightly faster than either of the 1050 materials.

Biocompatible Materials↗

Effects of dental resin components on vascular reactivity.

The frequent use of resins in dentistry has raised the question of their compatibility with oral tissues. The present study was undertaken to determine the effects of the resin components methyl methacrylate (MMA), hydroxyethyl methacrylate (HEMA), and triethylene glycol dimethacrylate (TEGDMA) on the reactivity of blood vessels using the isolated rat aorta as a tissue model. MMA, HEMA, and TEGDMA caused endothelium-dependent and -independent relaxation of rat aortic rings in a concentration-related manner. The endothelium-dependent responses of the tissues to all the resins were significantly attenuated by N-nitro-L-arginine methyl ester (L-NAME), indicating the involvement of nitric oxide. The vasorelaxant effects of both MMA and TEGDMA on the intact and denuded aortae were markedly inhibited by indomethacin, providing evidence for the role of prostanoids in these responses. Glybenclamide selectively attenuated TEGDMA-induced relaxation of the tissues with and without endothelium to a similar extent, suggesting the activation of vascular smooth muscle K(ATP) channels by this resin. It is concluded that MMA, HEMA, and TEGDMA interfere with the function of blood vessels by inducing vasorelaxation via different mechanisms, which, depending upon the type of resin, may at least involve the release of nitric oxide and prostanoid(s), and the activation of smooth muscle K(ATP) channels. These phenomena may play a role in tissue homeostasis and certain pathophysiological conditions associated with the application of resin materials to the oral environment.

Animals↗

Microleakage of conventional and microfilled composite restorative resins.

Microfilled composite resins have been introduced in clinical dentistry because of the difficulty in finishing conventional composite resins satisfactorily. Owing to the difference in coefficients of thermal expansion of the two resin systems, the objective of this in vitro study was to evaluate microleakage of a conventional and a microfilled composite resin. Class V cavities with butt cavosurface margins were prepared in the middle third of the facial surfaces of the crowns of 80 noncarious human premolar teeth; they were acid etched within the preparations only. Forty preparations were restored with Concise composite and forty with Silar microfilled resin. Ten teeth from each group were subjected to cyclic temperature changes between 5 and 55 degrees C for 1000, 2500, or 5000 cycles, respectively, and ten teeth from each group were not cycled (controls). After suitable preparation, the teeth were immersed in 45Ca solution for 18 h and contact radiographs were prepared. Microleakage was scored 0-3 at both the cervical and occlusal margins of the restorations. Microleakage was significantly greater at the cervical margins than at the occlusal margins. Differences within occlusal and cervical microleakages among the two resins were not significant.

Composite Resins↗

Quantifying the effect of resin type and sterilization method on the degradation of ultrahigh molecular weight polyethylene after 4 years of real-time shelf aging.

Alternative sterilization methods including ethylene oxide, gas plasma, and gamma-radiation in an inert environment were implemented in the late 1990s, to limit oxidative degradation of ultrahigh molecular weight polyethylene (PE). There was also a simultaneous transition to PE resins that did not contain calcium stearate. Shelf storage duration of PE inserts following gamma-irradiation in air has been correlated to poor clinical performance and increased wear. This study aimed to determine how sterilization method and resin type influenced degradation of PE after 4 years of real-time shelf aging. It was hypothesized that gamma-irradiation and stearate containing resins would incur significantly more degradation than nonradiated, stearate-free resins. Gamma-irradiated PE samples in air and nitrogen had a significantly increased density and oxidation index, compared to nonirradiated PE after 4 years of shelf aging. Alternative sterilization methods such as ethylene oxide and gas plasma appeared to have significantly less oxidation regardless of PE resin type. A partial correlation demonstrated that density and oxidation index were not correlated (r(2) = 0.079) when examining the influence of sterilization method. The data supported that after 4 years of real-time shelf aging, the type of sterilization method had a larger influence on PE degradation than resin type.

Biocompatible Materials↗

Influence of polymerization method, curing process, and length of time of storage in water on the residual methyl methacrylate content in dental acrylic resins.

This study compared the influence of different polymerization methods (heat, auto-, and microwave energy), different curing processes (in the case of heat- and autopolymerized specimens), and length of storage of the polymerized specimens in distilled water at 37 degrees C on the residual methyl methacrylate (MMA) content in dental acrylic resin specimens. Residual MMA of 120 resin specimens were measured using high-performance liquid chromatography. For the heat-polymerized resins, the lowest residual MMA content was obtained when they were given a long-term terminal boil and then stored in the distilled water for at least 1 day. For the autopolymerized resins, the lowest residual MMA content was obtained when they were additionally cured in water at 60 degrees C and then stored in the distilled water at least 1 day. For the microwave-polymerized resins, the lowest residual MMA content was obtained when they were stored in the distilled water at least 1 month. The lowest overall residual MMA content was obtained from heat-polymerized specimens that were given a long-term terminal boil cure and then stored in the distilled water at least 1 day. Different polymerization methods and curing processes have different effects on residual MMA content. It is thus shown that storing a dental acrylic resin specimen in distilled water at 37 degrees C is a simple but effective method of reducing its residual MMA content.

Acrylic Resins↗

Influence of a series of organic and chemical substances on the translucency of resin composites.

The objective of this study was to investigate the changes in the translucency of resin composites following a series of immersion treatments in organic and chemical substances. Color of resin composites was measured according to the CIELAB color scale relative to the standard illuminant D65 over a white and a black background. Translucency parameter (TP) of resin composites was calculated at baseline, and after sequential immersion: Step 1, porcine liver esterase (a substitute for a salivary esterase); Step 2, organic substances (mucin and serum) and phosphate-buffered saline (PBS) as a control; Step 3, chemical alteration agents [chlorhexidine (CH) and carbamide peroxide (CP)]; and Step 4, 2% methylene blue. Porcine liver esterase caused small changes in TP (DeltaTP = -0.5 to 0.2). After Step 2, DeltaTP values of three groups were similar in the range of -0.7 to 1.2. After Step 3, DeltaTP values of all groups were small in the range of -1.5 to 2.2. After Step 4, DeltaTP values were high and differences that varied by the resin composite and the immersion protocol were clearly observed (DeltaTP = -13.4 to -2.5). Changes in TP were mainly influenced by resin composite. After Step 4, mucin and serum groups showed generally small changes in TP compared to PBS group. It is a possibility that the high changes in TP after immersion in methylene blue is an indication of dye absorption which might be an indication of the degree of resin composite degradation.

Animals↗

Hybrid layer seals the cementum/4-META/MMA-TBB resin interface.

Although 4-META/MMA-TBB resin has adhesive properties to dentin, and has been clinically used for the bonding treatment of vertically fractured roots and apicoectomy, there has not been any investigation on the adhesion of 4-META/MMA-TBB resin to cementum. The purpose of this in vitro study was to evaluate the bonding and the sealing ability of 4-META/MMA-TBB resin to cementum. Bovine root cementum and dentin surfaces were treated with a citric acid and ferric chloride solution, and the 4-META/MMA-TBB resin was applied on the treated surfaces before testing. The microtensile bond strength and the leakage levels obtained for the cementum were almost equal to those for the dentin. In SEM and TEM observations, a hybrid layer approximately 2-3 microm in thickness was observed at the interface between the resin and the cementum. It is concluded that 4-META/MMA-TBB resin adhered to cementum via a hybrid layer on cementum, as previously reported for dentin.

Acid Etching, Dental↗

Direct determination of resin and fatty acids in process waters of paper industries by liquid chromatography/mass spectrometry.

Liquid chromatography/mass spectrometry (LC/MS)-based methods were developed for the analysis of 10 resin acids and five fatty acids in process waters of paper industries. No fragmentation of target compounds was observed using atmospheric pressure chemical ionization (APCI) with negative ionization. The [M - H](-) ion permitted the individual quantification of fatty and aromatic resin acids, whereas the non-aromatic resin acids presented a single and common ion at m/z 301. Separation with two columns of different polarity permitted peak confirmation. The method that used a C(8) column with 2-propanol in the mobile phase allowed a certain separation and identification of the non-aromatic resin acids, whereas the method using a C(18) column provided detection limits 10-fold lower for fatty acids. Limits of detection were 0.10 ng for all compounds. Direct sample introduction was compared with liquid-liquid extraction, with similar recoveries (70-101%). Whereas slightly lower detection limits were obtained with liquid-liquid extraction, better reproducibility was observed for direct sample introduction. Resin and fatty acids were determined in process waters of several paper industries. Palmitic, dehydroabietic and non-aromatic resin acids were encountered in most water samples, at levels between 22 and 403 micro g l(-1). LC/MS with direct sample introduction was found to be a good alternative to traditional liquid-liquid extraction and gas chromatography for the analysis of such compounds since no derivatization was required and sample manipulation was minimal.

Calibration↗

A novel class of chemically modified iodo-containing resins: design, synthesis and application to mass spectrometry-based proteome analysis.

A novel class of chemically modified iodo-containing resins with isotope-labeled tagging for mass spectrometry-based proteome analysis is described. This iodo-containing resin contains a thiol-reactive group that is used to capture the cysteine (Cys)-containing peptides from peptide mixtures, one 'tag' amino acid, and an aminomethyl polystyrene resin with Rink Amide Linker. The 'tag' amino acid is synthesized in both heavy and light isotope-coded forms and therefore permits the direct relative quantification of peptides/proteins through mass spectrometric analysis. In the iodo-containing resin strategy, the Cys-containing peptides of two samples covalently captured by either light or heavy iodo-containing resin were mixed and washed extensively under stringent conditions. Then the Cys-containing peptides were retrieved by acid-catalyzed elution. Finally, the eluted peptides were directly analyzed by micro liquid chromatography/mass spectrometry for identification and relative quantification. The iodo-containing resins were synthesized by a simple but effective method. Their abilities to identify and quantify the Cys-containing part in two samples were proved by the analysis of mixtures of amino acids, peptides and proteins.

Amino Acid Sequence↗

Sustained-release drug delivery system I: Coated ion-exchange resin system for phenylpropanolamine and other drugs.

Ion-exchange resin-drug complexes have been used to formulate sustained-release products of acidic and basic drugs. However, sustained release may be difficult to achieve due to many variables. A novel technique is reported that minimizes these variables by providing a polymeric film coating to the ion-exchange resin-drug complex particles, making drug release from these particles diffusion controlled. Direct application of an atomized polymer solution to the fluidized ion-exchange resin-drug complex particles was ineffective in controlling drug release since the coating came off in the dissolution medium due to swelling and fracturing of the particles. Pretreatment of the ion-exchange resin-drug complex particles with an agent such as polyethylene glycol was essential for the particles to retain their geometry and coating during dissolution. With divinylbenzenesulfonic acid resin complexed with phenylpropanolamine as a model, mixtures of ethylcellulose-coated and uncoated resin-drug complex particles were prepared. These mixtures gave varying drug release profiles that showed rank-order correlation with plasma concentration profiles obtained in bioavailability studies with suspension dosage forms.

Biological Availability↗

DNA changes in tissues entrapped in plant resins (the precursors of amber).

There have been many reports characterizing DNA from amber, which is a fossil version of plant resin. Here we report an investigation of the effects of plant resin (from Pseudotsuga menziesii) and drying conditions on the preservation of DNA in biological tissues. We examined the degree of degradation of the DNA by agarose gel electrophoresis of extracted DNA, by polymerase chain reaction, and by DNA sequencing. The plant resin alone appeared to cause little or no damage to DNA. Tissue immersed in plant resin that dried rapidly (exposed to sunlight) contained DNA with little apparent damage. Tissue immersed in the resin that was dried slowly (in shade without sunlight) contained DNA with some degradation (3.5% nucleotide changes). The tissue that was immersed in the resin that was constantly hydrated (by immersion in water) yielded DNA that was severely damaged (50-62% nucleotide changes). Transversions outnumbered transitions in these samples by a ratio of 1.4 : 1. A piece of Baltic amber immersed in water for 5 days appeared to be impervious to the water. Thus amber inclusions that initially dried rapidly have the potential to yield undamaged DNA. Those that dried slowly may contain damaged DNA and may be unsuitable for phylogenetic and other studies.

Amber↗