Efficacy of calcium‐ and fluoride‐containing materials for the remineralization of primary teeth with early enamel lesion

The aim of the study was to determine the efficacy of different products containing fluoride, calcium and phosphate for enamel remineralization in eroded primary teeth. A total of 90 sound primary canine teeth were randomly divided into 5 groups of 18 teeth each: 1) control (polished enamel), 2) 5% DuraShield sodium fluoride varnish, 3) 500 ppm fluoridated toothpaste, 4) casein phosphopeptide‐amorphous calcium phosphate (CPP‐ACP) cream, and 5) Clinpro White varnish containing functionalized tri‐calcium phosphate (fTCP). Enamel microhardness (EMH) was measured in all samples before and after demineralization and after 28 days of remineralization. Also 8 samples in groups 2 to 5 and four samples of sound and demineralized enamel were examined with atomic force microscopy (AFM). All data were analyzed with one‐way ANOVA (p<0.05). Mean microhardness of demineralized enamel was significantly lower than in enamel at baseline (p<0.001). Remineralization significantly increased microharness in groups 2 to 5 compared to the control group (p<0.001). Percent EMH after remineralization with CPP‐ACP was significantly higher than after fTCP (p=0.029), toothpaste (p< 0.001) or fluoride varnish (p<0.001); however, there was no significant difference between toothpaste and fluoride varnish (p=0.062). Microhardness increased more after fTCP treatment than after treatment with sodium fluoride varnish (p<0.001) or fluoridated toothpaste (p=0.045). AFM images showed that enamel roughness decreased most after treatment with fTCP, followed by CPP‐ACP, toothpaste and fluoride varnish. The efficacy of CPP‐ACP cream for remineralizing eroded enamel was greater than fluoride toothpaste, fluoride varnish or fTCP varnish. Microsc. Res. Tech. 78:801–806, 2015. © 2015 Wiley Periodicals, Inc.     

Thermal,morphological, and spectral changes after Er,Cr:YSGG laser irradiation at low fluences on primary teeth for caries prevention

The aim of this study was to determine the temperature increase in the pulp chamber and possible thermal effects on molecular structure of primary teeth during the irradiation with Er,Cr:YSGG laser. Primary central incisors were divided into three groups (n = 20). Labial surfaces in each group were irradiated by Er,Cr:YSGG laser within different power and frequencies as following groups: I: 0.25 W, 20 Hz, II: 0.50 W, 20 Hz, III: 0.75 W, 20 Hz. A thermocouple was placed inside the pulp chamber so that the temperature increments were recorded during the enamel irradiation. Morphological changes of enamel surfaces were experimentally evaluated by SEM. Fourier‐transform infrared spectroscopy and RAMAN analyses were carried out to determine the differentiations in the molecular structure. The experimental results obtained were analyzed statistically by means of one‐way analysis of variance. Statistically significant differences were detected between groups (p < .05). Group III exhibited the highest values for the temperature parameters. Besides, the conical craters, cracks, and formation of ablation areas were observed for all the groups. Also, it was obtained that the hydroxyapatite lost the hydroxyl ions due to the thermal effect of the laser. Temperature rise throughout the Er,Cr:YSGG laser irradiation for prevention of primary enamel demineralization presented a positive correlation with the laser output power level. The formations of adverse morphological and spectral changes were detected on the surface of teeth after the laser application. On this basis, the Er,Cr:YSGG laser applications should be treated with much more caution considering enamel surface and pulpal tissues in primary teeth.     

OM,SEM–EDX,and micro‐FTIR analysis of the Bronze Age pottery from the Băile Figa salt production site (Transylvania,Romania)

This article presents the results of analyses carried out on a lot of 11 fragments of Bronze Age ceramics discovered in the site from B?ile Figa (Beclean town, Transylvania, Romania), where salt exploitation occurred. The samples were analyzed by means of optical microscopy, on the basis of which the morphology and distribution of the inclusions in the ceramic paste was established. Likewise, the samples were analyzed by scanning electron microscopy with energy‐dispersive X‐ray spectrometry, producing microphotographs for each sample, and on the basis of the X‐ray spectra, the elemental composition in gravimetric percentages was established. Through the micro‐Fourier‐transform infrared spectroscopy analysis, on the basis of characteristic group vibrations, it was possible to ascertain the nature of the compounds from the ceramic samples. These analyses will contribute to the reconstruction of the prehistoric technologies for salt exploitation.     

Scanning electron microscopy and energy‐dispersive X‐ray spectroscopy analysis of electrochemically etched graphite tips created from pencil lead

Modern day pencil lead is a material of many possibilities. Manufacture process is fast, easy, and well established, yet the full potential of its use still remains to be uncovered. Graphite content ratio to binding clays determines basic properties of the lead like its toughness and color, but more interesting qualities like conductivity and reactivity as well. Properly employed electrochemical etching with a bubble membrane creates sharp and smooth graphite tips, which can be, given enough graphite content, used as probes in several measurement techniques. Observing and adjusting the tip creation process and the results for use in further research are the objectives of this paper.     

Peracetic acid as a single endodontic irrigant: effects on microhardness,roughness and erosion of root canal dentin

The aim was to assess the effects of 1% peracetic acid (PAA) as a single endodontic irrigant on microhardness, roughness, and erosion of root canal dentin, compared with 2.5% sodium hypochlorite (NaOCl) and with 2.5% NaOCl combined with 17% EDTA. Forty human, single‐rooted tooth hemisections were submitted to Knoop microhardness test, before and after the following irrigation protocols: PAA = 1% PAA; NaOCl = 2.5% NaOCl; NaOCl‐EDTA‐NaOCl = 2.5% NaOCl +17% EDTA +2.5% NaOCl; and SS = saline. Another 40 roots were instrumented, irrigated with the same protocols, and sectioned longitudinally. The roughness analysis was performed on the mesial section using a confocal laser scanning microscope, whereas erosion was analyzed on each third of the distal section, using a scanning electron microscope. The data were analyzed using ANOVA and Tukey post‐tests, and Kruskal‐Wallis and Dunn post‐tests (α = .05). The PAA and NaOCl‐EDTA‐NaOCl groups showed no significant differences (p > .05); both promoted reduction in microhardness and increase in roughness, compared with the NaOCl and SS groups (p < .05). NaOCl‐EDTA‐NaOCl promoted higher erosion in the cervical and middle thirds than the other groups (p < .05); there was no difference among PAA, NaOCl, and SS (p > .05). There was also no difference among the groups regarding the apical third (p > .05). PAA used as a single endodontic irrigant caused reduction in root canal dentin microhardness and increase in roughness in a similar way to NaOCl‐EDTA‐NaOCl; however, PAA caused less erosion than NaOCl‐EDTA‐NaOCl.     

Establishing the archaeo‐metallurgic ornamentation process of an axe from the bronze age by OM,SEM‐EDX,and Micro‐FTIR

Our article presents the results of the analyses we performed by corroborating the Optical Microscopy, Scanning Electron Microscopy, Energy Dispersive Xray Analysis and micro Fourier Transformed InfraRed Analysis techniques to identify the archaeo‐metallurgic casting and ornamentation procedure of a decorated disk‐butted axe, which was discovered recently east of the Carpathian mountains, in the Moldavian Plateau. There are few known axes of that type found (A1, according to the usual typologies), as they are specific to the Middle Bronze Age period west of the Carpathians—the Wietenberg, Suciu de Sus, and Otomani‐Füzesabony cultures. The experimental data on the item under study revealed the fact that after casting it in molds made from porous silicone‐based stone, the object was coated with a thin layer, by immersing it in a lightly fusible tin alloy, whose main alloy component was copper and arsenic and iron as secondary components. After refining the shiny white layer, they applied a beautiful decoration pattern made by incision and engraving. This battle axe was an indication of higher status, such items usually being owned by community leaders. This important fact proves that the ancient metallurgic craftsmen were able to elaborate and manufacture various alloys from which they made beautiful objects and it also offers a new insight into the social and symbolic function of certain antique bronze items. Microsc. Res. Tech. 77:918–927, 2014. © 2014 Wiley Periodicals, Inc.     

Effect of laser preparation on adhesion of a self‐adhesive flowable composite resin to primary teeth

The aim of the study was to evaluate the adhesion of a self‐adhering flowable composite resin to primary tooth enamel and dentin after silicon carbide paper (SiC) and laser pretreatment. Adhesive properties were evaluated as shear bond strength (SBS) and scanning electron microscopic (SEM) characteristics. A total 120 primary canine teeth were randomly divided into two groups to study enamel and dentin. Each group was divided into 6 subgroups (n = 10) according to type of surface preparation (SiC or Er:YAG laser) of enamel or dentin. Three methods were used to build cylinders of restoration on tooth surface: OptiBond All‐In‐One + Premise Flowable composite, OptiBond All‐In‐One + Vertise Flow and Vertise flow. After restoration, samples were tested for SBS and failure mode. Twenty eight samples were examined by SEM. The results of the study showed SBS of Vertise Flow was lower than others in enamel and dentin samples pretreated with SiC and in dentin samples pretreated with laser (P < 0.001). Compared to SiC pretreatment, laser pretreatment led to a significantly higher SBS with Vertise Flow on enamel (P < 0.001). Vertise Flow associated with the adhesive led to a higher SBS in enamel and dentin compared to Vertise Flow alone. Adhesive and mixed failure modes were observed more frequently in Vertise Flow groups. SEM images showed that Vertise Flow led to more irregularities on enamel and more open dentinal tubules after laser ablation compared SiC pretreatment. Microsc. Res. Tech. 79:334–341, 2016. © 2016 Wiley Periodicals, Inc.     

Technical advances in the sectioning of dental tissue and of on‐section cross‐linked collagen detection in mineralized teeth

Immunohistochemical detection of cross‐linked fibrillar collagens in mineralized tissues is much desired for exploring the mechanisms of biomineralization in health and disease. Mineralized teeth are impossible to section when embedded in conventional media, thus limiting on‐section characterization of matrix proteins by immunohistochemistry. We hypothesized that by using an especially formulated acrylic resin suitable for mineralized dental tissues, not only sectioning of teeth would be possible, but also our recently developed immunofluorescence labeling technique would be amenable to fully calcified tissues for characterization of dentinal fibrillar collagens, which remains elusive. The hypothesis was tested on fixed rodent teeth embedded in Technovit 9100 New®. It was possible to cut thin (1 μm) sections of mineralized teeth, and immunofluorescence characterization of cross‐linked type I fibrillar collagen was selected due to its abundance in dentine. Decalcified samples of teeth embedded in paraffin wax were also used to compare immunolabeling from either method using the same immunoreagents in equivalent concentrations. In the decalcified tissue sections, type I collagen labeling in the dentine along the tubules was “patchy” and the signal in the predentine was very weak. However, enhanced signal in mineralized samples with type I collagen was detected not only in the predentine but also at the limit between intertubular dentine, within the elements of the enamel organ and subgingival stroma. This report offers advances in sectioning mineralized dental tissues and allows the application of immunofluorescence not only for on‐section protein detection but importantly for detecting cross‐linked fibrous collagens in both soft and mineralized tissue sections. Microsc. Res. Tech. 73:741–745, 2010. © 2009 Wiley‐Liss, Inc.     

Micro‐ and nanoscale structures of mesiodens dentin: Combined study of FTIR and SAXS/WAXS techniques

A mesiodens is the most common type of supernumerary tooth present in conjunction to normal dentition. A mesiodens may commonly occur in the central region of the upper or lower jaw. A mesiodens is different from normal teeth in terms of structure and shape. The aim of this study is to evaluate the micro‐ and nanoscale structural properties of mesiodens dentin by combined small‐ and wide‐angle X‐ray scattering (SAXS/WAXS) and Fourier transform infrared (FTIR) spectroscopy. Five freshly extracted, noncarious mesiodens and five normal dentin disks prepared from human incisor teeth were compared. Using FTIR, the phosphate‐to‐amide I, carbonate‐to‐phosphate, and carbonate‐to‐amide I band area ratios and the crystallinity index were quantified. SAXS/WAXS were used to study the nanostructure of mesiodens. An increase in the mineral content in the mesiodens dentin with respect to the normal group was found. Crystallinity was also significantly increased and the protein content decreased in the mesiodens dentin compared with that of normal dentin. SAXS/WAXS results revealed that mesiodens dentin has a more calcified tissue. Further, SAXS analysis revealed a nonuniform distribution of dentin fibrils in mesiodens. Microsc. Res. Tech., 78:52–58, 2015. © 2014 Wiley Periodicals, Inc.     

Characterization of the calcification of cardiac valve bioprostheses by environmental scanning electron microscopy and vibrational spectroscopy

Bioprosthetic heart valve tissue and associated calcification were studied in their natural state, using environmental scanning electron microscopy (ESEM). Energy dispersive X‐ray micro‐analysis, X‐ray diffraction, Fourier‐transform infrared and Raman spectroscopy were used to characterize the various calcific deposits observed with ESEM. The major elements present in calcified valves were also analyzed by inductively coupled plasma–optical emission spectroscopy. To better understand the precursor formation of the calcific deposits, results from the elemental analyses were statistically correlated. ESEM revealed the presence of four broad types of calcium phosphate crystal morphology. In addition, two main patterns of organization of calcific deposits were observed associated with the collagen fibres. Energy dispersive X‐ray micro‐analysis identified the crystals observed by ESEM as salts containing mainly calcium and phosphate with ratios from 1.340 (possibly octacalcium phosphate, which has a Ca/P ratio of 1.336) to 2.045 (possibly hydroxyapatite with incorporation of carbonate and metal ion contaminants, such as silicon and magnesium, in the crystal lattice). Raman and fourier‐transform infrared spectroscopy also identified the presence of carbonate and the analyses showed spectral features very similar to a crystalline hydroxyapatite spectrum, also refuting the presence of precursor phases such as β‐tricalcium phosphate, octacalcium phosphate and dicalcium phosphate dihydrate. The results of this study raised the possibility of the presence of precursor phases associated with the early stages of calcification.     

Optimizing use of the structural chemical analyser (variable pressure FESEM‐EDX raman spectroscopy) on micro‐size complex historical paintings characterization

The novel Structural Chemical Analyser (hyphenated Raman spectroscopy and scanning electron microscopy equipped with an X‐ray detector) is gaining popularity since it allows 3‐D morphological studies and elemental, molecular, structural and electronic analyses of a single complex micro‐sized sample without transfer between instruments. However, its full potential remains unexploited in painting heritage where simultaneous identification of inorganic and organic materials in paintings is critically yet unresolved. Despite benefits and drawbacks shown in literature, new challenges have to be faced analysing multifaceted paint specimens. SEM?Structural Chemical Analyser systems differ since they are fabricated ad hoc by request. As configuration influences the procedure to optimize analyses, likewise analytical protocols have to be designed ad hoc. This paper deals with the optimization of the analytical procedure of a Variable Pressure Field Emission scanning electron microscopy equipped with an X‐ray detector Raman spectroscopy system to analyse historical paint samples. We address essential parameters, technical challenges and limitations raised from analysing paint stratigraphies, archaeological samples and loose pigments. We show that accurate data interpretation requires comprehensive knowledge of factors affecting Raman spectra. We tackled: (i) the in‐FESEM?Raman spectroscopy analytical sequence, (ii) correlations between FESEM and Structural Chemical Analyser/laser analytical position, (iii) Raman signal intensity under different VP‐FESEM vacuum modes, (iv) carbon deposition on samples under FESEM low‐vacuum mode, (v) crystal nature and morphology, (vi) depth of focus and (vii) surface‐enhanced Raman scattering effect. We recommend careful planning of analysis strategies prior to research which, although time consuming, guarantees reliable results. The ultimate goal of this paper is to help to guide future users of a FESEM‐Structural Chemical Analyser system in order to increase applications.     

基于PCA-SVM融合离子迁移谱与拉曼光谱的毒品鉴别方法

光学检测的指纹图谱具有专属性强、稳定性好、重现性好的特性。通过离子迁移谱毒品探测仪(IMS)与易制毒化学品拉曼快速检查仪分别采集离子与拉曼光谱的双谱图数据,然后将两个谱图进行创新数据融合后,结合主成分分析(PCA)和支持向量机(SVM)分类法对毒品进行鉴别。实验结果表明,融合后的数据相较于分别用单谱图数据进行鉴别,有效提高了对毒品的识别率和准确性。为鉴别毒品提供了一种安全、快速、可靠的新分析方法。     

X‐ray microdiffraction,TEM characterization and texture analysis of human dentin and enamel

Human tooth is a complex bioceramic composite, which consists of enamel, dentin and the interface, the dentin–enamel junction (DEJ). The crystal properties and ultrastructure of the inorganic phase through the thickness of healthy human molar teeth were investigated using X‐ray microdiffraction (μXRD), electron diffraction and transmission electron microscopy (TEM) techniques. The XRD data were analysed using the Le Bail profile fitting approach. The size and the texture of the crystallites forming enamel and dentin in the crown part of teeth were measured using both techniques and then compared. Results showed that the thickness of dentin crystallites was found to decrease towards the DEJ, whereas the thickness of the enamel crystallites increased from the DEJ towards the outer layers. It was demonstrated that enamel exhibited an increase of texture in 002 lattice planes from the DEJ towards the outer layers. Texture was also detected in 102 lattice planes. The texture effect in 002 planes at the scale of less than 1 μm was also demonstrated in dentin. The variation of lattice parameters as a function of the position within the thickness of dentin and enamel was also observed. The values of the nonuniform microstrain in the dentin and enamel crystallites were from 1.40 × 10^?6% to 4.44 × 10^?5%. The good correlation between XRD and TEM indicated that μXRD is a useful technique to study crystallography and microstructure of heterogeneous enamel and dentin. The observed gradient characteristics of texture and crystallite size in enamel and dentin maybe an evolutionary outcome to resist wear and fracture, thereby contributing to the excellent mechanical properties of teeth.     

联轴器法兰端面齿的设计及有限元分析

提出了联轴器法兰锥形端面齿的几何尺寸设计方法,建立了端面齿及连接螺栓的强度校核公式,并进行了有限元分析验证。该方法能用于Ф500～Ф1 200 mm联轴器法兰端面齿的系列化一般设计,也可供小规格联轴器法兰端面齿作设计参考。     

Effect of the root canal final rinse protocols on the debris and smear layer removal and on the push‐out strength of an epoxy‐based sealer

The aim of the present study was to evaluate the efficacy of QMiX, SmearClear, and 17% EDTA for the debris and smear layer removal from the root canal and its effects on the push‐out bond strength of an epoxy‐based sealer by scanning electron microscopy (SEM). Forty extracted human canines (n = 10) were assigned to the following final rinse protocols: G1‐distilled water (control), G2–17% EDTA, G3‐SmearClear, and G4‐QMiX. The specimens were submitted to a SEM analysis to evaluate the presence of debris and smear layer, respectively, in the apical or cervical segments. In sequence, forty extracted human maxillary canines with the root canals instrumented were divided into four groups (n = 10) similar to the SEM analysis study. After the filling with AH Plus, the roots were transversally sectioned to obtain dentinal slices. The specimens were submitted to a push‐out bond strength test using an electromechanical testing machine. The statistical analysis for the SEM and push‐out bond strength studies were performed using the Kruskal–Wallis and Dunn tests (α = 5%). There was no difference among the G2, G3, and G4 efficacy in removing the debris and smear layer (P > 0.05). The efficacy of these groups was superior to the control group. The push‐out bond strength values of G2, G3, and G4 were superior to the control group. The ability to remove the debris and smear layer by SmearClear and QMiX was as effective as the 17% EDTA. The final rinse with these solutions promoted similar push‐out bond strength values. Microsc. Res. Tech. 76:533–537, 2013. © 2013 Wiley Periodicals, Inc.     

Top‐down mass spectrometry for the analysis of combinatorial post‐translational modifications

Protein post‐translational modifications (PTMs) are critically important in regulating both protein structure and function, often in a rapid and reversible manner. Due to its sensitivity and vast applicability, mass spectrometry (MS) has become the technique of choice for analyzing PTMs. Whilst the “bottom‐up' analytical approach, in which proteins are proteolyzed generating peptides for analysis by MS, is routinely applied and offers some advantages in terms of ease of analysis and lower limit of detection, “top‐down” MS, describing the analysis of intact proteins, yields unique and highly valuable information on the connectivity and therefore combinatorial effect of multiple PTMs in the same polypeptide chain. In this review, the state of the art in top‐down MS will be discussed, covering the main instrumental platforms and ion activation techniques. Moreover, the way that this approach can be used to gain insights on the combinatorial effect of multiple post‐translational modifications and how this information can assist in studying physiologically relevant systems at the molecular level will also be addressed. © 2012 Wiley Periodicals, Inc., Mass Spec Rev 32:27–42, 2013     

Chemical and morphological evaluation of enamel and dentin near cavities restored with conventional and zirconia modified glass ionomer subjected to erosion‐abrasion

Microenergy dispersive X‐ray fluorescence (μ‐EDXRF) spectroscopy and scanning electron microscopy (SEM) were used to test the hypothesis that zirconia modified glass ionomer cement (GIC) could improve resistance to erosion‐abrasion to a greater extent than conventional cement. Bovine enamel (n = 40) and dentin (n = 40) samples were prepared with cavities, filled with one of the two restorative materials (GIC: glass‐ionomer cement or ZrGIC: zirconia‐modified GIC). Furthermore, the samples were treated with abrasion‐saliva (AS) or abrasion‐erosion cycles (AE). Erosive cycles (immersion in orange juice, three times/day for a duration of 1 min over a 5 day period) and/or abrasive challenges (electric toothbrush, three times/day for a duration of 1 min over a 5 day period) were performed. Positive mineral variation (MV%) on the enamel after erosion‐abrasion was observed for both materials (p < 0.05), whereas a negative MV% on the dentin was observed for both materials and treatments (p < 0.05). The SEM images showed clear enamel loss after erosion‐abrasion treatment and material degradation was greater in GIC_AE compared to those of the other groups. Toothbrush abrasion showed a synergistic effect with erosion on substance loss of bovine enamel, dentin, GIC, and ZrGIC restorations. Zirconia addition to the GIC powder improved the resistance to abrasive‐erosive processes. The ZrGIC materials may find application as a restorative material due to improved resistance as well as in temporary restorations and fissure sealants.