A simple and sensitive detection of diquat herbicide using a dental amalgam electrode A comparison using the chromatographic technique

This paper describes the use of a dental amalgam electrode (DAE) to evaluate the electrochemical behaviour and to develop an electroanalytical procedure for determination of diquat herbicide in natural water and potato samples. The work was based on the square wave voltammetry responses of diquat, which presented two well-defined and reversible reduction peaks, at -0.56 V (peak 1) and -1.00V (peak 2). The experimental and voltammetric parameters were optimised, and the analytical curves were constructed and compared to similar curves performed by high performance liquid chromatography coupled to ultraviolet-visible spectrophotometric detector (HPLC/UV-vis). The responses were directly proportional to diquat concentration in a large interval of concentration, and the calculated detection limits were very similar, around 10 mu g L(-1) (10 ppb) for voltammetric and chromatographic experiments. These values were lower than the maximum residue limit established for natural water by the Brazilian Environmental Agency. The recovery percentages in pure electrolyte, natural water and potato samples showed values from 70% to 130%, demonstrating that the voltammetric methodology proposed is suitable for determining any contamination by diquat in different samples, minimising the toxic residues due to the use of liquid mercury or the adsorptive process relative to use of other solid surfaces. (C) 2009 Published by Elsevier B.V.

Chemical Composition of Lipids Present in Cat and Dog Oocyte by Matrix-Assisted Desorption Ionization Mass Spectrometry (MALDI- MS)

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Determination of amfepramone hydrochloride, fenproporex, and diazepam in so-called natural capsules used in the treatment of obesity

A simple and rapid method was developed for the determination of amfepramone hydrochloride, fenprorex, and diazepam in capsules using high performance liquid chromatography (HPLC) with UV detection. This procedure provided conditions for the separation of the active ingredient from the complex matrices of the dosage forms by extraction in methanol. Isocratic reversed phase chromatography was performed using acetonitrile, methanol, and aqueous 0,1% ammonium carbonate (50:10:40) as a mobile phase, LiChrospher 100 RP 18 column (125 x 5 mm id, 5 mu m), a column temperature of 25 +/- 1 degrees C and detection at 230 nm.The calibration curves were linear over a wide concentration range (20-2000 mu g.mL(-1) to amfepramone hydrochloride, 8-800 mu g.mL(-1) to fenproporex, and 4-200 mu g.mL(-1) to diazepam) and good analytical recovery (87.1 to 107.8%) was obtained. The method is accurate and precise, as well as having advantages such as simplicity and short duration of analysis. Twenty samples of pharmaceutical preparations labelled as natural products were analysed. Anorectics and diazepam, were detected in 40% of the samples.

Determination of oxamniquine in capsules by HPLC

A sensitive, accurate, reliable and easy method was developed for the quantification of oxamniquine in capsules using high-performance liquid chromatography (HPLC) with UV detection. This technique provided conditions for the separation of the active ingredient from the dosage form by extraction in methanol. Isocratic reversed phase chromatography was performed using methanol, water, and triethanolamine (60:40:0.099, v/v/w) (System C) or methanol, acetonitrile, water and formic acid (40:30:30:0.083, v/v/w) (System D) as mobile phase, a stainless steel column (125 x 4 mm i.d., 5 mum) filled with LiChrospher 100 RP-18 (Merck), column temperature of 28 +/- 2 degreesC and detection at 260 nm. The calibration curves were linear over a wide concentration range (1.0-20.0 mug ml(-1) of oxamniquine) to the Systems C and D with good correlation factor (0.9990 and 0.9982, respectively). The average content obtained were 100.1 +/- 1.5% (System C) and 102.4 +/- 0.8% (System D). The presence of lactose, starch, magnesium stearate and sodium laurylsulphate did not interfere in the results of the analysis. The above findings showed the proposed method to be both simple and added advantage of allowing for fast analysis. (C) 2001 Elsevier B.V. B.V. All rights reserved.

Development and validation of HPLC method for analysis of dexamethasone acetate in microemulsions

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Tratamento eletroquímico de água produzida sintética para remoção de hidrocarbonetos policíclicos aromáticos

The aim of this work is the treatment of produced water from oil by using electrochemical technology. Produced water is a major waste generated during the process of exploration and production in the oil industry. Several approaches are being studied aiming at the treatment of this effluent; among them can be cited the biological process and chemical treatments such as advanced oxidation process and electrochemical treatments (electrooxidation, electroflotation, electrocoagulation, electrocoagulation). This work studies the application of electrochemical technology in the treatment of the synthetic produced water effluent through the action of the electron, in order to remove or transform the toxic and harmful substances from the environment by redox reactions in less toxic substances. For this reason, we used a synthetic wastewater, containing a mixture H2SO4 0,5M and 16 HPAs, which are: naphthalene, acenaphthylene, acenaphthene, fluorene, phenanthrene, anthracene, fluoranthene, pyrene, benzo (a) anthracene, chrysene, benzo(b)fluoranthene, benzo(k) fluoranthene, benzo(a)pyrene, indeno(1,2,3-cd)pyrene, dibenzo(a, h)anthracene, benzo(g, h, i)perylene. Bulk electrochemical oxidation experiments were performed using a batch electrochemical reactor containing a pair of parallel electrodes, coupled with a power supply using a magnetic stirrer for favoring the transfer mass control. As anodic material was used, a Dimensionally Stable Anode (DSA) of Ti/Pt, while as cathode was used a Ti electrode. Several samples were collected at specific times and after that, the analysis of these samples were carried out by using Gas Chromatography Coupled to Mass Spectrometry (GC - MS) in order to determine the percentage of removal. The results showed that it was possible to achieve the removal of HPAs about 80% (in some cases, more than 80%). In addition, as an indicator of the economic feasibility of electrochemical treatment the energy consumption was analyzed for each hour of electrolysis, and based on the value kWh charged by ANEEL, the costs were estimated. Thus, the treatment costs of this research were quite attractive

Influence of organic and mineral soil fertilization on essential oil of Spilanthes oleracea cv. Jambuarana

In the present study, the composition of essential oil of leaves and inflorescences of jambu (Spilanthes oleracea. Jambuarana), under organic manuring and mineral fertilization, was stuhed. Jambu plants show important chemical properties and their production has been addressed for the extraction of the essential oils for cosmetics industries, due to their pharmacolopcal properties. The experimental area of treatments contained urea as mineral fertilizer (120 g m2), applied twice and organic fertilizer (8 kg m2), applied at the planting. Jambu leaves and flowers were harvested twice: the first at 90 days after seedling transplantation and at the opening of the flower buds. Branches were cut at 7 cm from the soil, thus new branches can bud for the accomplishment of the second crop which happened 40 days after the re-budhng. The essential oil was analyzed by gas chromatography coupled with mass-spectrometry. According to our results the most representative compounds were trans-caryophyllene, germacrene-D, 1-dodecene, spathulenol and spilanthol (a compound presenting anesthetic properties) occurring in inflorescences. Fertilization procedure does not affect the content and the quality of the essential oil in Jambu plants. © 2012 Academic Journals Inc.

Anatomia foliar e influência da sazonalidade no óleo essencial de populações de Lychnophora pinaster Mart

Pós-graduação em Agronomia (Horticultura) - FCA

Desenvolvimento, rendimento, teor e componentes do óleo essencial em função de adubação orgânica e rebroto de Baccharis trimera (Less.) DC. cv. CPQBA-1

Pós-graduação em Agronomia (Horticultura) - FCA

Quantificação de contaminantes em aguardentes de cana/cachaças de alambique e de coluna

In the present study aimed to characterize and quantify four contaminants (ethyl carbamate, 2,3-butanedione, furfural and 5-hydroxymethylfurfural) present in alembic cachaça and industrial. Were collected forty-four samples of cachaça in the southern regions, the Midwest, southeast of Minas Gerais and São Paulo state, and subsequently subjected to physical, chemical and chromatographic analyzes. The physicochemical analyzes were performed according to the methodology described by the Ministry of Agriculture, Livestock and Supply (MAPA). The ethyl carbamate, 2,3-butanedione, furfuaral and 5 hydroxymethylfurfural were characterized and quantified by high-performance liquid chromatography (HPLC). The results of the ethyl carbamate analysis, it was found that both samples showed column cachaças outside the standards required by law, with the values 245.31 235.53 L-1 ug and none of the liquor samples alembic showed concentration greater than 210.0 ug L-1 , and the method is very sensitive to low limits of detection and quantification. In determining 2,3-butanedione, it was revealed that the column cachaças showed higher levels of contaminants when compared to cachaça alembic. In the quantification of furfural and 5-hydroxymethylfurfural was developed and validated analytical methods employed to high-performance liquid chromatography (HPLC) with DAD detector. Samples column cachaças showed higher values than the limit established by Brazilian legislation and ranged from 7.00 to 5.63 mg / 100 ml of anhydrous alcohol over the alembic cachaça.

Análise do teor de cocaína em amostras apreendidas pela polícia utilizando-se a técnica de cromatografia liquida de alta eficiência com detector UV-Vis

The HPLC technique with UV-Vis detection was employed in the analysis of cocaine content in apprehended samples of cocaine and crack. A peak signal for cocaine was obtained in 3.5 minutes run by using acetonitrile/water (95:5v/v) as a mobile phase. Optimized spectrophotometric signal was obtained at a wavelength of 224 nm. The analytical curve from 1.0 to 40.0 ppm of cocaine was obtained, showing a linear correlation coefficient of 0.9989, with detection and quantification limits of 0.75 ppm and 3.78 ppm, respectively. This methodology was employed at the dosage of confiscated samples of cocaine and crack in the Scientific Police Laboratory of Ribeirão Preto-SP city.

Contamination of cachaca by pahs from storage containers

Cachaça is a distiled beverage obtained from the fermentation of sugar cane syrup that, depending on the production procedures, may be susceptible to contamination by polycyclic aromatic hydrocarbons (PAHs). These compounds present carcinogenic and/or mutagenic properties and offer a risk to human health. Sixteen PAHs were determined in cachaças that had been stored in glass bottles and in polyethylene tank by gas chromatography coupled with mass spectrometry. The quantification of the PAHs utilised an internal standard. The limits of detection and quantification varied from 0.05 to 0.10 μg L−1 and 0.20 to 0.30 μg L−1, respectively. A total PAH concentration of 51.57 μg L−1 was found in the beverages that were stored in the tank, while the concentration in the cachaça stored in glass jugs was 6.07 μg L−1. These results indicate that the polyethylene tank is a source for PAHs in cachaça.

Determinação de acetaldeído e formaldeído em água de chuva e suas correlações com carbono orgânico dissolvido em uma região canavieira: Daniely de Godoy Silva. -

Pós-graduação em Química - IQ

Histochemical investigation of Cochlospermum regium (Schrank) Pilg. leaves and chemical composition of its essential oil

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

Estudo lipidômico em folhas de cultivares de cana-de-açúcar e avaliação do papel desses metabólicos na ferrugem alaranjada

Pós-graduação em Química - IQ