Preparative isolation of a novel flavonoid from an infusion of Byrsonima basiloba leaves by high-speed counter-current chromatography

A method for the isolation of three compounds from the infusion of leaves of Byrsonima basiloba A. Juss. by high-speed counter-current chromatography (HSCCC) was developed. This technique led to the separation of a novel compound, quercetin 3-O-alpha-L-rhamnopyranosyl-(1 -> 3)-O-[alpha-L-rhamnopyranosyl-(1 -> 6)]-beta-D-allopyranoside, and two known compounds quercetin3-O-(X-L-rhamnopyranosyl-(1 -> 6)-beta-D-galactopyranoside and (+)-catechin in 4 h with purities of over 92%. The structures of the compounds were determined by one- and two-dimensional NMR spectroscopy and HPLC.

Preparative separation of the naphthopyranone glycosides by high-speed counter-current chromatography

High-speed counter-current chromatography was applied to the preparative separation and purification of naphthopyranone glycosides from a crude 70% ethanolic extract of the capitula of Paepalanthus microphyllus. The solvent system used was composed of water-ethanol-ethyl acetate-hexane (10:4:10:4, v/v). This technique led to the separation of four different naphthopyranone glycosides in pure form in only 7 h. (C) 2001 Elsevier B.V. B.V. All rights reserved.

High-speed video observations of positive ground flashes produced by intracloud lightning

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

A high speed 3.3V current mode CMOS comparators with 10-b resolution

This paper presents a high speed current mode CMOS comparator. The comparator was optimized for allows wide range input current 1mA, ±0.5uA resolution and has fast response. This circuit was implemented with 0.8μm CMOS n-well process with area of 120μm × 105μm and operates with 3.3V(±1.65V).

Quick preparative separation of natural naphthopyranones with antioxidant activity by high-speed counter-current chromatography

The natural naphthopyranones paepalantine (1), paepalantine-9O-β-D-glucopyranoside (2) and paepalantine-9-O-β-D-allopyranosyl-(1→6)-O-β-D-glucopyranoside (3) were separated in a preparative scale from the ethanolic extract of the capitula of Paepalanthus bromelioides by high-speed counter-current chromatography (HSCCC). The solvent system used was composed of water-ethanol-ethyl acetate-hexane (10:4:10:4, v/v/v/v). This technique led to the separation of the three different naphthopyranone glycosides in pure form in approximately 7 hours. Paepalantine showed a good antioxidant activity when assayed by the DPPH radical spectrophotometric assay.

Fast preparative separation of flavones from capitula of Eriocaulon ligulatum (Vell.) L.B.Smith (Eriocaulaceae) by High-speed countercurrent chromatography (HSCCC)

High-speed countercurrent chromatography (HSCCC) is a leading method for the fast separation of natural products from plants. It was used for the preparative isolation of two flavone monoglucosides present in the capitula of Eriocaulon ligulatum (Veil.) L.B.Smith (Eriocaulaceae). This species, known locally as botão-dourado, is exported to Europe, Japan and North America as an ornamental species, constituting an important source of income for the local population of Minas Gerais State, Brazil. The solvent system, optimized in tests prior to the HSCCC run, consisted of the two phases of the mixture ethyl acetate: n-propanol: water (140:8:80, v/v/v), which led to the successful separation of 6-methoxyluteolin-7-O-β-D-allopyranoside and 6-methoxyapigenin-7-O-β-D-allopyranoside in only 3 hours. The two flavonoids were identified by NMR (1-D and 2-D) and ESI-MS, comparing their spectra with published data.

An overview of the microstructures present in high-speed steel - Carbides crystallography

The aim of the work was to prepare an overview about the microstructures present in high-speed steel, focused on the crystallography of the carbides. High-speed steels are currently obtained by casting, powder metallurgy and more recently spray forming. High-speed steels have a high hardness resulting from a microstructure, which consists of a steel matrix (martensite and ferrite), in which embedded carbides of different crystal structure, chemical composition, morphology and size, exist. These carbides are commonly named MxC, where M represents one or more metallic atoms. These carbides can be identified by X-ray diffraction considering M as a unique metallic atom. In this work, it is discussed, in basis of the first principles of physics crystallography, the validation of this identification when it is considered that other atoms in the structure are substitutional. Further, it is discussed some requirements for data acquisition that allows the Rietveld refinement to be applied on carbide crystallography and phase amount determination.

Influence of cavity preparation and curing method on the marginal seal of resin composite restorations: an in vitro evaluation.

OBJECTIVE: To evaluate the influence of cavity design and photocuring method on the marginal seal of resin composite restorations. METHOD AND MATERIALS: Seventy-two bovine teeth were divided into 2 groups: group 1 received box-type cavity preparations, and group 2 received plate-type preparations. Each group was divided into 3 subgroups. After etching and bonding, Z250 resin composite (3M Espe) was applied in 2 equal increments and cured with 1 of 3 techniques: (1) conventional curing for 30 seconds at 650 mW/cm2; (2) 2-step photocuring, in which the first step was performed 14 mm from the restoration for 10 seconds at 180 mW/cm2 and the second step was performed in direct contact for 20 seconds at 650 mW/cm2; or (3) progressive curing using Jetlite 4000 (J. Morita) for 8 seconds at 125 mW/cm2 and then 22 seconds at 125 mW/cm2 up to 500 mW/cm2. The specimens were thermocycled for 500 cycles and then submitted to dye penetration with a 50% silver nitrate solution. Microleakage was assessed using a stereomicroscope. Data were analyzed using analysis of variance and Tukey test (5% level of significance). RESULTS: A statistically significant difference was found between groups when a double interaction between photocuring and cavity preparation was considered (P = .029). CONCLUSIONS: No one type of cavity preparation or photocuring method prevented micro-leakage. The plate-type preparation showed the worst dye penetration when conventional and progressive photocuring methods were used. The best results were found using the 2-step photocuring with the plate-type preparation.

Influence of the tool edge geometry on specific cutting energy at high-speed cutting

This paper presents specific cutting energy measurements as a function of the cutting speed and tool cutting edge geometry. The experimental work was carried out on a vertical CNC machining center with 7,500 rpm spindle rotation and 7.5 kW power. Hardened steels ASTM H13 (50 HRC) were machined at conventional cutting speed and high-speed cutting (HSC). TiN coated carbides with seven different geometries of chip breaker were applied on dry tests. A special milling tool holder with only one cutting edge was developed and the machining forces needed to calculate the specific cutting energy were recorded using a piezoelectric 4-component dynamometer. Workpiece roughness and chip formation process were also evaluated. The results showed that the specific cutting energy decreased 15.5% when cutting speed was increased up to 700%. An increase of 1 °in tool chip breaker chamfer angle lead to a reduction in the specific cutting energy about 13.7% and 28.6% when machining at HSC and conventional cutting speed respectively. Furthermore the workpiece roughness values evaluated in all test conditions were very low, closer to those of typical grinding operations (∼0.20 μm). Probable adiabatic shear occurred on chip segmentation at HSC Copyright © 2007 by ABCM.

Separation of the toxic zierin from Zollernia ilicifolia by high speed countercurrent chromatography

Preliminary pharmacological assays of the 70% methanol extract from the leaves of the Brazilian medicinal plant Zollernia ilicifolia Vog. (Fabaceae) showed analgesic and antiulcerogenic effects. Previous analyses have shown that this extract contains, besides flavonoid glycosides and saponins, a toxic cyanogenic glycoside. Flavonoids and saponins are compounds reported in literature with antiulcerogenic activity. In this work, we developed a methodology to separate the cyanogenic glycoside from these compounds in order to obtain enough amount of material to perform pharmacological assays. The cyanogenic glycoside zierin (2S)-β-D-glucopyranosyloxy-(3-hydroxy-phenyl)- acetonitrile was separated from the other components by high speed countercurrent chromatography (HSCCC). The solvent system used was composed of chloroform-methanol-n-propanol-water (5:6:1:4, v/v/v/v). This technique led to the separation of zierin from the possible active compounds of Zollernia ilicifolia.

Influence of the power level of an ultra-sonic system on dental cavity preparation

The aim of this study was to evaluate the shape of dental cavities made with the CVDentus® system using different ultrasound power levels. One standard cavity was made on the buccal aspect of 15 bovine incisors with a CVDentus® cylindrical bur (82142). The sample was divided into three groups: G1 - ultrasound with power II; G2 - ultrasound with power III; and G3 - ultrasound with power IV. A standardizing device was used to obtain standardized preparations and ultrasound was applied during one minute in each dental preparation. The cavities were sectioned in the middle, allowing observation of the cavity's profile with a magnifying glass, and width and depth measurement using the Leica Qwin program. The Kruskal-Wallis (p < 0.05) and Dunn statistical analyses demonstrated differences between the dental cavity shapes when powers III and IV were used. However, the cavities that were made with power III presented dimensions similar to those of the bur used for preparation. We concluded that the power recommended by the manufacturer (III) is the most adequate for use with the CVDentus® system.

LED light attenuation through human dentin: A first step toward pulp photobiomodulation after cavity preparation

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Temperature rise during Er:YAG cavity preparation of primary enamel

This study aimed to assess in vitro thermal alterations taking place during the Er:YAG laser cavity preparation of primary tooth enamel at different energies and pulse repetition rates. Forty healthy human primary molars were bisected in a mesio-distal direction, thus providing 80 fragments. Two small orifices were made on the dentin surface to which type K thermocouples were attached. The fragments were individually fixed with wax in a cylindrical PlexiglassA (R) abutment and randomly assigned to eight groups, according to the laser parameters (n = 10): G1 -aEuro parts per thousand 250 mJ/ 3 Hz, G2 -aEuro parts per thousand 250 mJ/ 4 Hz, G3 -aEuro parts per thousand 250 mJ/ 6 Hz, G4 -aEuro parts per thousand 250 mJ/10 Hz, G5 -aEuro parts per thousand 250 mJ/ 15 Hz, G6 -aEuro parts per thousand 300 mJ/ 3 Hz, G7 -aEuro parts per thousand 300 mJ/ 4 Hz and G8 -aEuro parts per thousand 300 mJ/ 6 Hz. An area of 4 mm(2) was delimited. Cavities were done (2 mm long x 2 mm wide x 1 mm thick) using non-contact (12 mm) and focused mode. Temperature values were registered from the start of laser irradiation until the end of cavity preparation. Data were analyzed by one-way ANOVA and Tukey test (p a parts per thousand currency signaEuro parts per thousand 0.05). Groups G1, G2, G6, and G7 were statistically similar and furnished the lowest mean values of temperature rise. The set 250 mJ/10 and 15 Hz yielded the highest temperature values. The sets 250 and 300 mJ and 6 Hz provided temperatures with mean values below the acceptable critical value, suggesting that these parameters ablate the primary tooth enamel. Moreover, the temperature elevation was directly related to the increase in the employed pulse repetition rates. In addition, there was no direct correlation between temperature rise and energy density. Therefore, it is important to use a lower pulse frequency, such as 300 mJ and 6 Hz, during cavity preparation in pediatric patients.