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216 result(s) for "Polymethacrylic Acids - analysis"
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Evaluation of Residual Monomers Eluted from Pediatric Dental Restorative Materials
Unreacted monomers eluted from resin-based restorative materials have been considered a reason of local and systemic adverse reactions. This study was designed to determine the effect of finishing and polishing procedures on the elution of Bis-GMA, TEGDMA, UDMA, and HEMA monomers from compomer and bulk-fill composite resins. Bulk-fill composite (3M ESPE GmbH, Seefeld, Germany) and compomer (Dentsply DeTrey GmbH, Konstanz, Germany) specimens with 3×4 mm diameters were prepared. The specimens were randomly divided into two groups, and finishing-polishing procedures were applied only to the experimental groups. Release of residual monomers was analyzed by using High-Performance Liquid Chromatography (HPLC) after 24, 48, and 72 hours. Repeated measures ANOVA and Tukey post hoc tests were used for comparisons. Finishing and polishing procedures had a significant effect on reducing the quantity of UDMA release in the Filtek™ Bulk Fill composite and Bis-GMA, HEMA, and TEGDMA in the Dyract XP compomer (p<0.05). The restorative materials investigated here are not chemically stable after polymerization, and concentrations of eluted monomers may reach critical toxicity levels even after one restoration placement. Finishing and polishing procedures are mandatory to reduce residual monomers.
Eudragit S-100 coated sodium alginate microspheres of naproxen sodium: formulation, optimization and in vitro evaluation
The aim of the study was to prepare site specific drug delivery of naproxen sodium using sodium alginate and Eudragit S-100 as a mucoadhesive and pH-sensitive polymer, respectively. Core microspheres of alginate were prepared by a modified emulsification method followed by cross-linking with CaCl2, which was further coated with the pH dependent polymer Eudragit S-100 (2.5 or 5 %) to prevent drug release in the upper gastrointestinal environment. Microspheres were characterized by FT-IR spectroscopy, X-ray diffraction, differential scanning calorimetry and evaluated by scanning electron microscopy, particle size analysis, drug loading efficiency, in vitro mucoadhesive time study and in vitro drug release study in different simulated gastric fluids. Stability studies of the optimized formulation were carried out for 6 months. SEM images revealed that the surface morphology was rough and smooth for core and coated microspheres, respectively. Core microspheres showed better mucoadhesion compared to coated microspheres when applied to the mucosal surface of freshly excised goat colon. The optimized batch of core microspheres and coated microspheres exhibited 98.42 ± 0.96 and 95.58 ± 0.74 % drug release, respectively. Drug release from all sodium alginate microsphere formulations followed Higuchi kinetics. Moreover, drug release from Eudragit S-100 coated microspheres followed the Korsmeyer-Peppas equation with a Fickian kinetics mechanism. Stability study suggested that the degradation rate constant of microspheres was minimal, indicating 2 years shelf life of the formulation.
Compositional Analysis of Low Quantities of Phase Separation in Hot-Melt-Extruded Solid Dispersions: A Combined Atomic Force Microscopy, Photothermal Fourier-Transform Infrared Microspectroscopy, and Localised Thermal Analysis Approach
ABSTRACT Purpose To characterise phase separations in aged hot-melt-extruded solid dispersions at a micron to submicron scale. Methods Hot-melt-extruded felodipine and Eudragit ® E PO systems at a range of compositions were studied after a standard period of aging to allow phase separation to occur. The samples were characterised using combined nano-thermal analysis, photothermal FTIR microspectroscopy coupled with pulsed force mode AFM as a novel characterisation approach. Result Crystalline felodipine presents in all formulations with drug loadings from 10–70% (w/w). In formulations with high drug loadings (50 and 70%), amorphous felodipine co-exists with crystalline forms, and higher drug concentration is observed in the centre compared to the outer surface of the extrudates. Drug crystal dimensions in extrudates with low drug loadings (10–30%) are small, in the micron to submicron range. We propose that uneven drug distribution is principally caused by processing-associated factors such as expansion of extrudates during extrusion. Conclusions We have demonstrated that the novel combined approach allows site-specific characterisation of the extruded systems and that drug distribution may be uneven across the extrudates, with concomitant implications for understanding stability and drug release behaviour.
Evaluation of polypropylene and poly (butylmethacrylate-co-hydroxyethylmethacrylate) nonwoven material as oil absorbent
Polypropylene (PP) and poly(butylmethacrylate- co -hydroxyethylmethacrylate) (PBMA- co -HEMA) nonwoven materials as oil absorbents have been fabricated for the first time via melt blown method. As-prepared nonwovens were investigated in terms of mass per unit area, density, air permeability, contact angle, and morphology observations for fiber diameter distribution and single fiber surface by a field emission scanning electron microscope. The nonwovens are demonstrated as fast and efficient absorbents for various kinds of oils with oil absorbency up to seven to ten times their own weight. The nonwovens show excellent water repulsion but superoleophilic properties. The measured contact angles for water and toluene are more than 127° and ca. 0°, respectively. The addition of PBMA- co -HEMA makes the nonwoven surface more hydrophobic while conserving superoleophilicity. Compared with PP nonwoven, broad diameter distribution of the blend nonwoven is attributed to poor melt fluidity of PBMA- co -HEMA. In terms of single fiber, coarse surface and the presence of point-like convexities lead to the fibers being more readily wetted by oil. More interesting, oil–water separation and oil recovery can be easily carried out by filter and absorption–desorption process, the recovered materials contained hardly any oil droplet and could be reused for next cycles.
HPLC analysis of components released from dental composites with different resin compositions using different extraction media
Components released from dental composite resins are essential factors in the assessment of biocompatibility of these materials. The effect of different extraction media on monomer release from composite resins based on different monomer types was evaluated. Three types of visible light cured composite resins were formulated based on the following monomers: triethylene glycol dimethacrylate (TEGDMA), bisphenol A glycerolate dimethacrylate (BisGMA), and urethane dimethacrylate (UDMA). Seventy-five composite resin discs were fabricated and light cured for 1 min in the absence of oxygen. Extraction media used were: distilled water, saline solution, artificial saliva, serum-free culture medium, and culture medium with 10% fetal calf serum. The analysis of extracts from the composite resins was carried out by High Performance Liquid Chromatography (HPLC). Quantifiable amounts of TEGDMA were released into the aqueous media. However, BisGMA and UDMA were not detectable in any of the extracts from the composite resins. Statistical analysis by one-way ANOVA followed by Tukey's test showed that there was a significant difference in TEGDMA release between culture media and other media (p < 0.05). From the results of this experiment it can be concluded that TEGDMA-based composite resins can release a high quantity of monomer into aqueous environments. The type of extraction medium may have a significant effect on monomer release from composite resins.
In Vitro and ex Vivo Intestinal Tissue Models to Measure Mucoadhesion of Poly (Methacrylate) and N-Trimethylated Chitosan Polymers
The adhesion of a range of polymers based on poly(2-(dimethylamino-ethyl) methacrylate (pDMAEMA) was assessed using human mucus-secreting and non mucus-secreting intestinal cell monolayers, HT29-MTX-E12 (E12) and HT29 monolayers, as well as excised non-everted intestinal sacs from rats. Differentiation of mucoadhesion from bioadhesion was achieved by pre-treatment with the mucolytic agent, N-acetyl cysteine (NAC). Adherence of pDMAEMA polymers was compared to that obtained with the mucoadhesive, N-trimethylated chitosan (TMC). The quantity of adherent coumarin 343-conjugated polymers to HT29, E12, and intestinal sacs was measured by fluorescence. Confocal laser scanning microscopy (CLSM), light microscopy, and fluorescent microscopy were used to provide direct evidence. Measurements of transepithelial electrical resistance (TEER), permeability to FITC-dextran 4000 (FD-4), and the release of lactate dehydrogenase (LDH) were used to assess potential cytotoxicity of polymers. Adherence of unquaternized and of 10%, 24%, and 32% methyl iodide-quaternized pDMAEMA polymers was measured in E12, HT29, and sacs. All pDMAEMA polymers showed significantly higher levels of adhesion to mucus (mucoadhesion) than to epithelium (bioadhesion). Colocalization of pDMAEMA with mucus was confirmed in E12 by microscopy. TMC showed equally high levels of mucoadhesion as unquaternized and 24% quaternized pDMAEMA, but displayed higher levels of bioadhesion. pDMAEMA-based polymers demonstrated lower levels of adherence to E12 and rat sacs in the presence of NAC, whereas adherence of TMC was unchanged. pDMAEMA significantly decreased the permeability of FD-4 across E12 monolayers and sacs and was less cytotoxic in E12 than in HT29. In contrast, TMC increased the permeability of FD-4 across E12 and sacs and was less cytotoxic in E12 than in HT29. Human mucus-producing E12 monolayers can be used to assess polymer mucoadhesion and give similar data to isolated rat intestinal sacs. pDMAEMA displayed similar levels of mucoadhesion and lower levels of bioadhesion than a chitosan derivative and it was not cytotoxic. pDMAEMA decreased FD-4 flux in the presence of mucus, whereas TMC increased it. The combination of mucus and methacrylate polymers appears to increase barrier function of the apical membrane.
Quantitative determination of TEGDMA, BHT, and DMABEE in eluates from polymerized resin-based dental restorative materials by use of GC/MS
This study investigated the leaching of ingredients from several commercial dental composite resins cured with LED, and immersed in methanol or water for 24 h, respectively. The composites used were: Admira Dentin (VOCO), Artemis Schmelz (Enamel) (Ivoclar Vivadent), Els extra low shrinkage (Saremco Dental), Filtek Supreme XT Dentin (3 M ESPE), Gradia Direct (GC), Venus & Venus flow (Heraeus Kulzer), and XRV Herculite Prodigy Enamel (Kerr). From each dental composite four specimens with defined structure and 100-mg net weight were made. After the polymerization process, according to manufacturer's instructions, the specimens were immersed in either 1 ml water or 1 ml methanol and incubated at 37°C for 24 h. Eluted ingredients triethyleneglycoldimethacrylate (TEGDMA), 2,6-di-tert-butyl-4-methylphenol (BHT), and 4-N,N-dimethylaminobenzoicacidethylester (DMABEE) were detected and quantified using gas chromatography-mass spectrometry (GC-MS). The amounts of the detected analytes from 100 mg polymerized composites ranged between the following values: TEGDMA: 0-0.5 mg (water), 0-1.6 mg (methanol); BHT: 0-0.03 μg (water), 0-0.11 mg (methanol); and DMABEE: 0-0.11 mg (water), 0-1.4 mg (methanol). We conclude from the results that the elution rates into methanol and water differ significantly. Furthermore, it is concluded that all the determined amounts eluting from the composites are far below toxic-relevant concentrations.
Identification of Phase Separation in Solid Dispersions of Itraconazole and Eudragit® E100 Using Microthermal Analysis
To evaluate the phase separation in itraconazole/Eudragit E100 solid dispersions prepared by hot-stage extrusion. Extrudates were prepared using a corotating twin-screw extruder at 180 degrees C. Micro-TA was used to evaluate the phase separation, where the AFM mode is used to visualize the different phases and local thermal analysis (LTA) to characterize the different phases Itraconazole formed a homogeneous mixture with Eudragit E100 with drug concentrations up to approximately 20%. Above this concentration, phase separation was observed. MTDSC revealed two Tgs and the mesophase of free glassy itraconazole. Performing micro-TA on the surface of these dispersions indicated an increase in sample roughness in the z-axis piezo signal, which could be an indication of free glassy itraconazole. However, thermal conductivity did not reveal differences between separate phases. Performing LTA, where only a small area (20 x 20 microm) is heated, showed two separate and mixed phases of itraconazole and Eudragit E100. Tip penetration in itraconazole and Eudragit E100 occurred at 332K and 383K respectively. The difference in tip penetration was explained in terms of the difference in fragility. Micro-TA makes it possible to characterize separate phases of itraconazole and Eudragit E100, thereby confirming the MTDSC results on phase separation.
Acrylic scaffolds with interconnected spherical pores and controlled hydrophilicity for tissue engineering
Polymer scaffolds are obtained in which the geometric characteristics (pore size, connectivity, porosity) and the physico-chemical properties of the resulting material can be controlled in an independent way. The interconnected porous structure was obtained using a template of sintered PMMA microspheres of controlled size. Copolymerization of hydrophobic ethyl acrylate and hydrophilic hydroxyethyl methacrylate comonomers took place in the free space of the template, different comonomer ratio gave rise to different hydrophilicity degrees of the material keeping the same pore architecture. The morphology of the resulting scaffolds was investigated by scanning electron microscopy (SEM), the porosity of the material calculated, and the mechanical properties compared with those of the bulk (non porous) material of the same composition.
Strategies for the Analysis of Poly(Methacrylic Acid) by Matrix-Assisted Laser Desorption/Ionization Time-of-Flight Mass Spectrometry
We evaluated several aqueous-based sample preparation protocols for the analysis of poly(methacrylic acid) (PMAA) by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOFMS). The sample contained a pentaerythritol tetra(3-mercaptopropionate) end-group, and was characterized in positive and negative ion modes using 2,5-dihydroxybenzoic acid (DHB) and 2,4,6-trihydroxyacetophenone (THAP) matrices. The major series observed were the [M + Na] + species, in positive ion mode, and the [M − H] − species, in negative ion mode. The performance of DHB and THAP matrices was comparable in positive ion mode, but THAP outperformed DHB in negative ion mode. The use of ion-exchange beads (IXB) benefited the analysis, while the addition of sodium acetate (NaOAc) or trifluoroacetic acid (TFA) proved disadvantageous in positive ion mode.