Analysis of camphorquinone in composite resins as a function of shade

Objective. To identify and quantify the camphorquinone (CQ) used in different brands of composite resins as a function of the shade analyzed.Materials and methods. Filtek Z250 A3 (FZA3), Filtek Z-250 Incisal (FZI), Pyramid Enamel A1 (PEA1), Pyramid Enamel Translucent (PET), Filtek Supreme A3E (FSA3) and Filtek Supreme GT (FSGT) were used. Five hundred milligrams of each resin were weighed and then dissolved in 1.0 ml of methanol. The samples were centrifuged to accelerate the sedimentation of the inorganic particles. 0.8 ml of the supernatant solution was collected with a pipette and assessed under gas chromatography coupled to the mass spectrometer (GC-MS). The results were compared to pure CQ solutions, used as a standard. Student's t-test, (p = 0.05) significant at the level of 5%, compared the results of each brand shade.Results. A smaller amount of camphorquinone was found in Filtek Z-250 (FZI) resin incisal shade when compared to (FZA3) A3 shade. on the other hand, Filtek Supreme resin featured a statistically larger camphorquinone amount in the incisal shade. in Pyramid Enamel resin camphorquinone was found only in shade Al, while the photoinitiator used in the Translucent shade was not identified.Significance. Based on the data obtained, it is possible to conclude that a single composite resin brand may feature differences in amount and type of photoinitiator used. (C) 2006 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Determination of fluquinconazole, pyrimethanil, and clofentezine residues in fruits by liquid chromatography with ultraviolet detection

A simple method was developed for the determination of fluquinconazole, pyrimethanil, and clofentezine in whole fruit; peel; and pulp of mango, apple, and papaya. These compounds were extracted from fruit samples with a mixture of ethyl acetate-n-hexane (1 + 1, v/v). An aliquot (2 mL) of the extract was evaporated to near dryness under a stream of nitrogen, and the residue was dissolved with 2 mL methanol. The analysis was performed by means of liquid chromatography with ultraviolet detection at 254 nm using a gradient solvent system. The method was validated with fortified fruit samples at concentration levels of 0.05, 0.10, 0.20, and 0.50 mg/kg. Average recoveries (4-8 replicates) ranged from 80 to 95% with relative standard deviations between 3.5 and 12.7%. Detection limits ranged from 0.03 to 0.05 mg/kg for fruit pulp and 0.03 mg/kg for whole fruit. The quantitation limits ranged from 0.05 to 0.10 mg/kg for fruit pulp and 0.05 mg/kg for whole fruit. The analytical method was applied to fruit samples obtained from local markets.

Validation of an immunoassay method for the determination of traces of carbaryl in vegetable and fruit extracts by liquid chromatography with photodiode array and mass spectrometric detection

A competitive enzyme-linked immunosorbent assay (ELISA) method for carbaryl quantitation in crop extracts was validated by liquid chromatography (LC) with diode array detection (DAD). For this purpose, six crops (banana, carrot, green bean, orange, peach and potato) were chosen for recovery and reproducibility studies. The general sample preparation included extraction with methanol followed by liquid-liquid partitioning and clean-up on Celite-charcoal adsorbent column of the vegetable extracts. ELISA samples consisted of a diluted LC extract in assay phosphate buffer (pH 7.5). The potential effect of methanol in these samples was evaluated. It was observed that a maximum content of 10% methanol present in the assay buffer could be tolerated without expressive losses in the ELISA performance. Under these conditions, a IC50 similar to 1.48 mu g l(-1) was obtained. A minimum matrix effect with a 1:50 dilution of the methanolic extracts in assay buffer was noticed, except for green bean samples that inhibited completely the assay. For the vegetable extracts, the ELISA sensitivities varied from 3.9 to 5.7 mu g l(-1), and good recoveries (82-96%) with R.S.D.s ranging from 5.7 to 12.1% were found. An excellent correlation between the LC-DAD and ELISA techniques was obtained. The confirmation of the carbaryl in less concentrated samples was achieved by LC-mass spectrometry interfaced with atmospheric pressure chemical ionisation. The [M + H](+)= 202 and [M + H-57](+)=145 ions, equivalent to the protonated molecular and l-naphthol ions, respectively, were used to carbaryl identification in these samples. (C) 1998 Elsevier B.V. B.V. All rights reserved.

Determination of acetaldehyde in fuel ethanol by high-performance liquid chromatography with electrochemical detection

The cyclic voltammetric behavior of acetaldehyde and the derivatized product with 2,4-dinitrophenylhydrazine (DNPHi) has been studied at a glassy carbon electrode. This study was used to optimize the best experimental conditions for its determination by high-performance liquid chromatographic (HPLC) separation coupled with electrochemical detection. The acetaldehyde-2,4-dinitrophenyl.hydrazone (ADNPH) was eluted and separated by a reversed-phase column, C-18, under isocratic conditions with the mobile phase containing a binary mixture of methanol/LiCl(aq) at a concentration of 1.0 x 10(-3) M (80:20 v/v) and a flow rate of 1.0 mL min(-1). The optimum condition for the electrochemical detection of ADNPH was +1.0 V vs. Ag/AgCl as a reference electrode. The proposed method was simple, rapid (analysis time 7 min) and sensitive (detection limit 3.80 mu g L-1) at a signal-to-noise ratio of 3:1. It was also highly selective and reproducible [standard deviation 8.2% +/- 0.36 (n = 5)]. The analytical curve of ADNPH was linear over the range of 3-300 mg L-1 per injection (20 mu L), and the analytical recovery was > 99%.

Determination of 2,4-dichlorophenoxyacetic acid and its major transformation product in soil samples by liquid chromatographic analysis

The 2,4-dichlorophenoxyacetic acid (2,4-D) is one of the most applied herbicides around the world to control broad leave herbs in many crops: In this study, a method was developed for simultaneous extraction and determination of 2,4D and its major transformation product, i.e., the 2,4-dichlorophenol (2,4-DCP), in soil samples. The herbicide and its degradation product were extracted twice from soil samples, after acidification, by dichloromethane on ultrasound system for 1 h. Both extracts were combined and filtrated in qualitative filter paper and Celitee. The total extract was concentrated in rotatory evaporator, dried under N-2 and finally dissolved in 1 ml of methanol. High Performance Liquid Chromatography with UV detection at 230 nm was used for analysis. Recoveries were obtained from soil samples fortified at 0.1, 1.0, 2.0, 3.0 and 4.0 mg kg(-1) levels and the results varied from 85 to 111% (for 2,4-D) and from 95 to 98% (for 2,4-DCP). For both compounds, the limits of quantification were 0.1 mg kg(-1), which were the loss level at which the accuracy and the precision were studied. Nevertheless, the limits of detection, calculated by considering the blank standard deviation and the minimum concentration level, were 0.03 and 0.02 mg kg for 2,4-D and 2,4-DCP, respectively. This proposed method was applied to soil samples of eucalyptus crops, which was previously treated with the herbicide. Despite that, neither 2,4-D nor its degradation product were detected 30 days after the herbicide application. (C) 2003 Elsevier B.V. B.V. All rights reserved.

Determination of aldehydes and ketones in fuel ethanol by high-performance liquid chromatography with electrochemical detection

A new methodology was developed for analysis of aldehydes and ketones in fuel ethanol by high-performance liquid chromatography (HPLC) coupled to electrochemical detection. The electrochemical oxidation of 5-hydroxymetkylfurfural, 2-furfuraldehyde, butyraldehyde, acetone and methyl ethyl ketone derivatized with 2,4-dinitrophenylhydrazine (DNPH) at glassy carbon electrode present a well defined wave at +0.94 V; +0.99 V; +1.29 V; +1.15 V and +1.18 V, respectively which are the basis for its determination on electrochemical defector. The carbonyl compounds derivatized were separated by a reverse-phase column under isocratic conditions with a mobile phase containing a binary mixture of methanol /LiClO4(aq) at a concentration of 1.0 x 10(-3) mol L-1 (80:20 v/v) and a flow-rate of 1.1 mL min(-1). The optimum potential for the electrochemical detection of aldehydes-DNPH and ketones-DNPH was +1.0 V vs. Ag/AgCl. The analytical curve of aldehydes-DNPH and ketones-DNPH presented linearity over the range 5.0 to 400.0 ng mL(-1), with detection limits of 1.7 to 2.0 ng mL(-1) and quantification limits from 5.0 to 6.2 ng mL(-1), using injection volume of 20 mu L. The proposed methodology was simple, low time-consuming (15 min/analysis) and presented analytical recovery higher than 95%.

Dinuclear Azide-Bridged Copper(II) Complex as Building Block for the Assembly of a 2D-Supramolecular Array

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

Optimization of the Transesterification Reaction in Biodiesel Production and Determination of Density and Viscosity of Biodiesel/Diesel Blends at Several Temperatures

Waste frying oil has been used to optimize the production of biodiesel. Biodiesel was prepared through sodium ethoxide catalyzed methanolysis from the transesterification of recycled waste frying oil. Optimization of the transesterification reaction for biodiesel production was carried out by means of statistical analyses using ANOVA. The optimum conditions for reaction were the following: a oil methanol mole ratio of 1:9, temperature of 50 degrees C, catalyst mass fraction of 0.9 %, and reaction time of 40 min, which enabled a yield of 98.7 % determined by gas chromatography/mass spectrometry (GC/MS) analysis. The density and viscosity of biodiesel/diesel blends have been determined as a function of composition at several temperatures.

Quercetin-PVP K25 solid dispersions: Preparation, thermal characterization and antioxidant activity

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Potencialidade energética em diferentes extratores e tempos de extração do óleo de pinhão-manso (jatropha curcas l.) em soxletter

The current rhythm of petroliferous exploration is esteem that the existing reserves will be depleted in next the 45 years. Thus being, it has that to study intensely, what it has come to be fact, the alternative power plants, as well as the technologies economically capable to ultilizar them. The potential demand of biodiesel for 2020 is taken in consideration that, in accordance with the International Agency of Energia (AIE), in only eight countries, will jump of 34,7 million tons in 2010 for 133,8 million in 2020, with an increment next to 300%. The tame nut is a producing oil plant with all the qualities necessary to be transformed into oil diesel. Beyond perennial and of easy culture, it presents good conservation of the harvested seed, being able to become great producer of substance cousin as optional fuel source. For these authors, this is a culture that can be developed in the small properties, with the available familiar man power, being plus a source of income for the country properties of the Northeast Region. The objective of this work is to evidence the capacity of oil production of the nut-bellwether, and the quality of extration with hexano and methanol in 6 distinct times.

A Validated Stability-Indicating LC Method for Orbifloxacin in the Presence of Degradation Products

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

Optical chemical sensors using polythiophene derivatives as active layer for detection of volatile organic compounds

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

Application of methylotrophic yeast Pichia pastoris in the field of food industry - A review

Since ancient times, the utilization of yeasts by the man has a great impact on the socio-economic development. After the advent of the technology of recombinant DNA, great advances have occurred due to the acquisition of strains of mutant yeasts in the field of applied research, and Saccharomyces cerevisiae has soon been outstanding as an interesting candidate for the expression of heterologous proteins of biotechnological interest. As the time goes by other alternative systems of expression have been shown because they have advantages over Saccharomyces cerevisiae. Among those new systems, Pichia pastoris is outstanding as methylotrophic yeast capable of growing in a culture medium containing methanol as the only source of carbon and energy. The induction of production of glycerol-3-phosphate dehydrogenase (GPD, NAD(+): oxido-redutase EC 1.1. 1.8) by Pichia pastoris was accomplished in the medium containing methanol. One of the most important key parameters in Pichia pastoris expression system is the methanol concentration. Bibliographic reviews on the Pichia pastoris production system have shown that the best culture conditions vary according to the strain used and/or kind of heterologous protein desired to be expressed. Therefore, we have sought to develop a system, involving expression of glycerol-3-phosphate dehydrogenase in the yeast Pichia pastoris, for generating sufficient quantities of the enzyme in order to asses its potential value for use in various food bioanalytical determination. Dehydrogenases have been widely used in the enzymatic assays of diverse composites of industrial interest, being enclosed among them glycerol and a number of important bioanalytical applications.

Effects of Synthesis Conditions on the Nanostructure of Hybrid Sols Produced by the Hydrolytic Condensation of (3-Methacryloxypropyl)trimethoxysilane

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Detection of Toxoplasma gondii DNA in the milk of naturally infected ewes

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