Sensitive and fast determination of Sudan dyes in chilli powder by partial-filling micellar electrokinetic chromatography-tandem mass spectrometry

A fast and sensitive method for the simultaneous determination of Sudan dyes (I, II, III, and IV) in food samples was developed for the first time using partial filling micellar electrokinectic chromatography-mass spectrometry (MEKC-MS). The use of MEKC was essential to achieve the separation of these neutral analytes, while the partial filling technique was necessary to avoid the contamination of the ion source with non-volatile micelles. MEKC separation and MS detection conditions were optimized in order to achieve a fast, efficient, and sensitive separation of the four dyes. Filling 25% of the capillary with an MEKC solution containing 40 mM ammonium bicarbonate, 25 mM SDS, and 32.5% (v/v) acetonitrile, a baseline separation of the four azo-dyes was obtained in 10 min. Tandem MS was investigated in order to improve the sensitivity and selectivity of the analysis. Limits of detection (LOD) values 5, 8, 15, and 29 times better were obtained for Sudan III, I, II, and IV, respectively, using partial filling MEKC-MS/MS instead of partial filling MEKC-MS. Under optimized conditions, LOD from 0.05 to 0.2 mu g/mL were obtained. The suitability of the developed method was demonstrated through the fast and sensitive determination of Sudan I, II, III, and IV in spiked chilli powder samples. This determination could not be achieved by MEKC-UV due to the existence of several interfering compounds from the matrix.

Evaluation of epoxy resin sealer after three root canal filling techniques by confocal laser scanning microscopy

The aim of this study was to evaluate the penetration of endodontic sealer into the dentin tubules, the integrity of the sealer layer perimeter, and the sealer area at the apical third after different filling techniques by confocal laser scanning microscopy (CLSM). Forty-five mandibular premolars were mechanically prepared with ProTaper files, until F5 file. Thereafter, they were filled with an epoxy-resin sealer (AH Plus) mixed with Rhodamine B dye (0.1% proportion) and allocated in three groups: Group 1, single master cone; Group 2, cold lateral compaction; and Group 3, Thermafil. For confocal laser scanning microscopy analysis, the specimens were transversely sectioned at 4 mm from the apex. The images at x10 and x40 were analyzed by Imagetool 3.0 software. Significant differences were not found among the three experimental groups according the dentin-impregnate area by the sealer (P = 0.68) and between the sealer and root canal perimeter (P = 0.18). However, root canal filling techniques were significantly different when apical sealer areas were compared (P = 0.001). Thermafil group showed smaller sealer areas (8.09%) while cold lateral compaction and gutta-percha master cone showed similar areas (17.37 and 21.18%, respectively). The dentin-impregnated area was not dependent on the root canal filling technique. Single master cone, cold lateral condensation and Thermafil techniques presented integrity of the sealer perimeter close to 100% and Thermafil resulted in a significantly thinner sealer layer. Microsc. Res. Tech. 75:12771280, 2012. (C) 2012 Wiley Periodicals, Inc.

A method to investigate the shrinkage stress developed by resin-composites bonded to a single flat surface

Objectives. To purpose a method for predicting the shrinkage stress development in the adhesive layer of resin-composite cylinders that shrink bonded to a single flat surface, by measuring the deflection of a glass coverslip caused by the shrinkage of the bonded cylinders. The correlation between the volume of the bonded resin-composite and the stress-peak was also investigated. Methods. A glass coverslip deflection caused by the shrinkage of a bonded resin-composite cylinder (diameter: d = 8 mm, 4 mm, or 2 mm, height: h = 4 mm, 2 mm, 1 mm, or 0.5 mm) was measured, and the same set-up was simulated by finite element analysis (3D-FEA). Stresses generated in the adhesive layer were plotted versus two geometric variables of the resin-composite cylinder (C-Factor and volume) to verify the existence of correlations between them and stresses. Results. The FEA models were validated. A significant correlation (p < 0.01, Pearson's test) between the stress-peak and the coverslip deflection when the resin-composites were grouped by diameter was found for diameters of 2 and 4 mm. The stress-peak of the whole set of data showed a logarithmic correlation with the bonded resin-composite volume (p < 0.001, Pearson's test), but did not correlate with the C-Factor. Significance. The described method should be considered for standardizing the stress generated by the shrinkage of resin-composite blocks bonded to a single flat surface. (C) 2012 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Push-out strength of root fillings with or without thermomechanical compaction

Carneiro SMBS, Sousa-Neto MD, Rached-Junior FA, Miranda CES, Silva SRC, Silva-Sousa YTC. Push-out strength of root fillings with or without thermomechanical compaction. International Endodontic Journal, 45, 821828, 2012. Abstract Aim To evaluate the influence of thermomechanical compaction (Taggers hybrid technique THT) on the push-out strength of several root filling materials to root dentine. Methodology Root canals of eighty roots in human canines were prepared with the ProTaper system and filled with one of the following materials, using either lateral compaction (LC) (n = 40) or THT (n = 40): AH Plus/gutta-percha (GP) (n = 10), Sealer 26/GP (n = 10), Epiphany SE/Resilon (n = 10) and Epiphany SE/GP (n = 10). Three 2-mm-thick dentine slices were obtained from each third of each root. The root filling in the first slice was subjected to a push-out test to evaluate the bond strength of the materials to intraradicular dentine. Data (in MPa) were analysed using anova and post hoc Tukeys test (P < 0.05). Failure mode was determined at x25 magnification. The other two slices were prepared for scanning electron microscopy (SEM) to examine the surface of the filling materials. Results Lateral compaction (1.34 +/- 1.14 MPa) was associated with a significantly higher bond strength (P < 0.05) than the THT (0.97 +/- 0.88 MPa). AH Plus/GP (2.23 +/- 0.83 MPa) and Sealer 26/GP (1.86 +/- 0.50 MPa) had significantly higher bond strengths than the other materials and differed significantly from each other (P < 0.05). There was a significant difference (P < 0.05) between the coronal (1.36 +/- 1.15 MPa), middle (1.14 +/- 1.05 MPa) and apical thirds (0.95 +/- 0.83 MPa). Considering the technique and root filling material interaction, AH Plus/GP-LC was associated with the highest mean values (2.65 +/- 0.66 MPa) (P < 0.05). Sealer 26/GP-LC (2.10 +/- 0.46 MPa), AH Plus/GP-THT (1.81 +/- 0.78 MPa) and Sealer 26/GP-TH (1.63 +/- 0.44 MPa) had intermediate values that were not significantly different from each other (P > 0.05). Epiphany SE was associated with the lowest mean values (3.70 +/- 0.86 MPa) (P < 0.05), regardless of the root filling technique and type of solid material (cone). Adhesive failures predominated in the specimens filled with Epiphany SE, whilst mixed and cohesive failures were more frequent in those filled with AH Plus and Sealer 26, regardless of the root filling technique. SEM analysis revealed that LC produced a dense and well-compacted filling whilst the use of a hybrid thermomechanical technique resulted in the solid material (GP or Resilon) intermingled within sealer to form a nonhomogenous mass. Conclusion Lateral compaction was associated with higher bond strengths of the materials to intraradicular dentine than a hybrid technique using thermomechanical compaction. The greatest push-out strengths were obtained when the canals were filled with LC of AH Plus and GP cones.

Periapical Tissue Response After Use of Intermediate Restorative Material, Gutta-Percha, Reinforced Zinc Oxide Cement, and Mineral Trioxide Aggregate as Retrograde Root-End Filling Materials: A Histologic Study in Dogs

Purpose: To investigate the periapical tissue response of 4 different retrograde root-filling materials, ie, intermediate restorative material, thermoplasticized gutta-percha, reinforced zinc oxide cement (Super-EBA), and mineral trioxide aggregate (MTA), in conjunction with an ultrasonic root-end preparation technique in an animal model. Materials and Methods: Vital roots of the third and fourth right mandibular premolars in 6 healthy mongrel dogs were apicectomized and sealed with 1 of the materials using a standardized surgical procedure. After 120 days, the animals were sacrificed and the specimens were analyzed radiologically, histologically, and scanning electron microscopically. The Fisher exact test was performed on the 2 outcome values. Results: Twenty-three sections were analyzed histologically. Evaluation showed better re-establishment of the periapical tissues and generally lower inflammatory infiltration in the sections from teeth treated with the intermediate restorative material and the MTA. New root cement on the resected dentin surfaces was seen on all sections regardless of the used material. New hard tissue formation, directly on the surface of the material, was seen only in the MTA sections. There was no statistical difference in outcome among the tested materials. Conclusions: The results from this dog model favor the intermediate restorative material and MTA as retrograde fillings when evaluating the bone defect regeneration. MTA has the most favorable periapical tissue response when comparing the biocompatibility of the materials tested. (C) 2012 American Association of Oral and Maxillofacial Surgeons J Oral Maxillofac Surg 70:2041-2047, 2012

Qualitative SEM/EDS analysis of microleakage and apical gap formation of adhesive root-filling materials

Objective: The aim of this study was to compare the correspondence between gap formation and apical microleakage in root canals filled with epoxy resin-based (AH Plus) combined or not with resinous primer or with a dimethacrylate-based root canal sealer (Epiphany). Material and Methods: Thirty-nine lower single-rooted human premolars were filled by the lateral condensation technique (LC) and immersed in a 50-wt% aqueous silver nitrate solution at 37 degrees C (24 h). After longitudinal sectioning, epoxy resin replicas were made from the tooth specimens. Both the replicas and the specimens were prepared for scanning electron microscopy (SEM). The gaps were observed in the replicas. Apical microleakage was detected in the specimens by SEM/energy dispersive spectroscopy (SEM/EDS). The data were analyzed statistically using an Ordinal Logistic Regression model and Analysis of Correspondence (alpha=0.05). Results: Epiphany presented more regions containing gaps between dentin and sealer (p<0.05). There was correspondence between the presence of gaps and microleakage (p<0.05). Microleakage was similar among the root-filling materials (p>0.05). Conclusions: The resinous primer did not improve the sealing ability of AH Plus sealer and the presence of gaps had an effect on apical microleakage for all materials.