Flow-batch analyser for preparation of calibration standard mixtures in simultaneous multicomponent spectrometric analysis

ABSTRACT: The application of multivariate calibration techniques to multicomponent analysis by UV-VIS molecular absorption spectrometry is a powerful tool for simultaneous determination of several chemical species. However, when this methodology is accomplished manually, it is slow and laborious, consumes high amounts of reagents and samples, is susceptible to contaminations and presents a high operational cost. To overcome these drawbacks, a flow-batch analyser is proposed in this work. This analyser was developed for automatic preparation of standard calibration and test (or validation) mixtures. It was applied to the simultaneous determination of Cu²⁺, Mn²⁺ and Zn²⁺ in polyvitaminic and polymineral pharmaceutical formulations, using 4-(2-piridilazo) resorcinol as reagent and a UV-VIS spectrophotometer with a photodiode array detector. The results obtained with the proposed system are in good agreement with those obtained by flame atomic absorption spectrometry, which was employed as reference method. With the proposed analyser, the preparation of calibration and test mixtures can be accomplished about four hours, while the manual procedure requires at least two days. Moreover, it consumes smaller amounts of reagents and samples than the manual procedure. After the preparation of calibration and test mixtures, 60 samples^-1 can be carried out with the proposed flow-batch analyser.

Preparation of refractory calcium aluminate cement using the sonochemical process

Calcium aluminate cements (CAC) were prepared using the sonochemical process, followed by heat treatment. A study was made of the action of ultrasonic waves and the influence of thermal treatment conditions on two initial molar compositions of 1:1 and 1:2 of calcia:alumina. The aqueous suspension containing the raw materials (A-50 alumina and CaO) was subjected to an ultrasonic bath, followed by drying and burning at 1000, 1200 and 1300 ºC. These cements were characterized by SEM, XRD and the mechanical strength was evaluated by splitting tensile tests, using commercial cement as a reference. Furthermore, the phases were semi-quantified using the Rietveld method. The results show that hydration and sonochemical action increased the reactivity of the raw materials during firing and that phase formation is dependent on the thermal treatment conditions. The CAC cements were obtained at temperatures at least 200 ºC lower than those used in conventional methods, indicating the potential of this route of synthesis.

Processes for the preparation of piperidinic derivatives and pharmaceutic compositions containing the same

Production processes for preparing pharmaceutical compositions containing new molecules capable of inhibiting acetylcholinesterase, thus being useful in the treatment of pathologies associated to cholinergic transmission, such as memory related disorders, neurodegenerative disorders such as Alzheimer's Disease, Miastenia Gravis or in the treatment of intoxications induced by chemical agents of central action.

Rapid preparation of alpha-FeOOH and alpha-Fe2O3 nanostructures by microwave heating and their application in electrochemical sensors

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Pharmacological Evaluation and Preparation of Nonsteroidal Anti-Inflammatory Drugs Containing an N-Acyl Hydrazone Subunit

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

Density, Refractive Index, Apparent Specific Volume, and Electrical Conductivity of Aqueous Solutions of Poly(ethylene glycol) 1500 at Different Temperatures

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Bacterial cellulose as a template for preparation of hydrotalcite-like compounds

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

Preparation of TiO2/SnO2 Thin Films by Sol-Gel Method and Periodic B3LYP Simulations

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

Use of a cashew nut shell liquid resin as a potential replacement for phenolic resins in the preparation of panels - a review

The Cashew Nut Shell Liquid (CNSL) can be considered as a versatile raw material with wide applications in the form of surface coatings, paints and varnishes, as well as the production of polymers. Within this context, the chemical constituents of CNSL (anarcadic acid, cardanol, 2-cardol and methylcardol) become promising in the development of new materials components. Once separated, CNSL can be used in the research and development of additives, surfactants, pharmaceuticals, pesticides, polymers, resins and others. Being a byproduct, CNSL used in the preparation of new materials is characterized as a truly technological innovation.

Antibiofilm activity of irrigating solutions associated with cetrimide. Confocal laser scanning microscopy

AimTo evaluate the antibiofilm activity of sodium hypochlorite (NaOCl) and chlorhexidine (CHX) solutions associated with cetrimide (CTR), and QMiX using confocal laser scanning microscopy.MethodologyEnterococcus faecalis (ATCC- 29212) biofilms were induced on bovine dentine blocks for 14days. The dentine blocks containing biofilm were immersed for 1min in the following solutions: 2.5% NaOCl; 2.5% NaOCl+0.2% CTR; 2% CHX; 2% CHX+0.2% CTR; 0.2% CTR; QMiX. After contact with the solutions, the dentine blocks were stained with Live/Dead((R)) BacLight for analysis of the remaining biofilm using confocal laser scanning microscope. Images were evaluated using the BioImage_L software to determine the total biovolume (m(3)), the green biovolume (live cells) (m(3)) and the percentage of substrate coverage (%). The data were subjected to nonparametric statistical test using Kruskal-Wallis and Dunn's tests at 5% significance level.ResultsAfter exposure to irrigants, the total biovolume observed for CHX, CHX+CTR, CTR, QMiX was similar to distilled water (P>0.05). NaOCl and NaOCl+CTR had the lowest total and green biovolume. The CTR and QMiX had intermediate green biovolume, with greater antibacterial activity than CHX and CHX+CTR (P<0.05). The NaOCl and NaOCl+CTR solutions were associated with microorganism removal and substrate cleaning ability.ConclusionsNaOCl and NaOCl+CTR solutions were effective on microorganism viability and were able to eliminate biofilm. The addition of cetrimide did not influence antibacterial activity.

Water activity of aqueous solutions of ethylene oxide-propylene oxide block copolymers and maltodextrins

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

A Family of Stationary Solutions to the Euler Equations and Generalized Solutions

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

Screening of Conditions for the Preparation of Poly( -Caprolactone) Nanocapsules Containing the Local Anesthetic Articaine

The local anesthetic articaine (ATC) is widely used in dentistry; however, its side effects can include paresthesia and nerve injury. Polymeric nanocapsules (PN) can be used as carriers for drugs, and help to reduce undesirable symptoms. The objective of this study was to evaluate the influence of different factors on the average size, polydispersion, and encapsulation efficiency of PN containing ATC. Poly(ε-caprolactone) (PCL) nanocapsules containing ATC were prepared by the oil-in-water emulsion/solvent evaporation method. The final ATC concentration was 2%. The preparation conditions were optimized using a central composite blocked cube-star design to investigate the influence of two variables at five levels, with 22 factorial points (–1 and +1), two replicates of the central point, 2×2 axial points (–1.414 and +1.414), and an orthogonal distribution, resulting in 10 experiments. The factors varied were the PVA concentration and the sonication time. The nanocapsules showed a satisfactory size range, a polydispersivity index less than 0.2, and high encapsulation efficiency. The values of the factors had no significant influence on either average size or polydispersion, although the encapsulation efficiency was significantly influenced by the sonication time. Improved formulations were identified using the central composite design, which revealed that the main consideration in selecting a suitable formulation was the encapsulation efficiency. Two of the formulations showed both high encapsulation efficiency and colloidal characteristics appropriate for the route of administration.

Effect of human whole saliva on the in vitro adhesion of Candida albicans to a denture base acrylic resin: a focus on collection and preparation of saliva samples

Objective In studies on Candida albicans adhesion to surfaces, diverse protocols have been used for collection and preparation of saliva samples. Thus, this study investigated whether variations in the centrifugation parameters and number of donors of saliva would influence the adhesion of C. albicans to a denture base resin. Methods Resin acrylic samples (n = 72) were made and then divided into four groups: (a) control – specimens were left without preconditioning in saliva; (b) three experimental groups, in which the specimens were preconditioned with saliva collected from 15 volunteers and centrifuged at 12 000 g for 5 min (G1); from 15 volunteers and centrifuged at 18 000 g for 30 min (G2); and from one volunteer and centrifuged at 12 000 g for 5 min (G3). Candida adhesion was evaluated by both the 2,3-bis(2-methoxy-4-nitro-5-sulfophenyl)-5-[(phenylamino) carbonyl]-2H-tetrazolium hydroxide (XTT) reduction method and crystal violet staining. Data were analyzed by one-way analyses of variance (P = 0.05). Results For XTT reduction assay, groups G2, G3, and control were not significantly different, whereas group G1 showed significantly higher absorbance value than control. For crystal violet staining there were no significant differences among all groups. Conclusion Variations in the centrifugation parameters and number of donors of saliva may influence C. albicans adhesion to denture base resins.

Effectiveness of several solutions to prevent the formation of precipitate due to the interaction between sodium hypochlorite and chlorhexidine and its effect on bond strength of an epoxy-based sealer

To evaluate the effectiveness of isopropyl alcohol, saline or distilled water to prevent the precipitate formed between sodium hypochlorite (NaOCl) and chlorhexidine (CHX) and its effect on the bond strength of an epoxy-based sealer in radicular dentine. Methodology The root canals of 50 extracted human canines (n = 10) were instrumented. In G1, root canals were irrigated with 17% EDTA and 2.5% NaOCl; G2, as G1, except that 2% CHX was used as the final irrigant. In the other groups, intermediate flushes with isopropyl alcohol (G3), saline (G4) or distilled water (G5) were used between NaOCl and CHX. The specimens were submitted to SEM analysis to evaluate the presence of debris and smear layer, in the apical and cervical segments. In sequence, fifty extracted human canines were distributed into five groups (n = 10), similar to the SEM study. After root filling, the roots were sectioned transversally to obtain dentine slices, in the cervical, middle and apical thirds. The root filling was submitted to a push-out bond strength test using an electromechanical testing machine. Statistical analysis was performed using Kruskal–Wallis and Dunn's tests (α = 5%). Results All groups had similar amounts of residue precipitated on the canal walls (P > 0.05). The push-out bond strength values were similar for all groups, independently of the root third evaluated (P > 0.05). Conclusions Isopropyl alcohol, saline and distilled water failed to prevent the precipitation of residues on canal walls following the use of NaOCl and CHX. The residues did not interfere with the push-out bond strength of the root filling.