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

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Oxidative stress status of highly prolific sows during gestation and lactation

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Patulin determination in apples with rotten areas

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

Determinação simultânea de resíduos de cloranfenicol, tianfenicol e florfenicol em leite bovino por cromatografia eletrocinética micelar

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

Avaliação de contaminantes inorgânicos e orgânicos em álcool combustível utilizando eletroforese capilar

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

Indirect determination of chloride and sulfate ions in alcohol fuel by capillary electrophoresis

A capillary zone electrophoresis method using indirect UV detection for the analysis of chloride and sulfate in alcohol fuel samples was developed. The anions were analyzed in less than 3 min using an electrolyte containing 10 mmol 1(-1) chromate and 0.75 mmol 1(-1) hexamethonium bromide (HMB) as electroosmotic flow modifier. Coefficients of variation were better than 0.6% for migration time (n = 10) and between 2.05 and 2.82% for peak area repeatabilities. Analytical curves of peak area versus concentration in the range of 0.065-0.65 mg kg(-1) for chloride and 0.25-4.0 mg kg(-1) for sulfate were linear with coefficients of correlation higher than 0.9996. The limits of detection for sulfate and chloride were 0.033 and 0.041 mg kg(-1), respectively. Recovery values ranged from 85 to 103%. The method was successfully applied for the quantification of sulfate and chloride in five alcohol fuel samples. The concentration of sulfate varied from 0.45 to 3.12 mg kg(-1). Chloride concentrations were below the method's LOD.

Determination of olive oil acidity by CE

In this work, a CE method for the determination of olive oil acidity was proposed. The method was based on an ethanolic extraction (at 60 degrees C) of the oil long-chain free fatty acids (LC-FFAs) components followed by CE determination in pH 6.86 phosphate buffer at 15 mmol/L concentration containing 4 mmol/L sodium dodecylbenzenesulfonate (SDBS), 10 mmol/L polyoxyethylene 23 lauryl ether (Brij 35((R))), 2% v/v 1-octanol and 45% v/v ACN under indirect UV detection at 224 nm. Although this electrolyte promoted baseline separation of myristic acid (C14:0) (internal standard (IS)) and olive oil major components (palmitic acid (C16:0), oleic acid (C18:1c) and linoleic acid (C18:2cc)) in less than 8 min, after a few injections, the electropherogram profiles were severely altered (peak broadening, migration time shifts, etc.) and the current increased substantially. An adsorption study was conducted revealing that the dissolution of the capillary external polyimide coating during the electrophoretic run caused the detrimental effect. After removal of the capillary tip coating, ten consecutive injections could be performed without any disturbances and this simple procedure was, therefore, implemented during quantitative purposes. The reliability of the proposed method was further investigated by the determination of acidity of an extra virgin olive oil sample in comparison to the established methodology (AOCS method Ca 5a40, alkaline volumetric titration (AVT)). No statistical differences were found within 95% confidence level. A % acidity of 0.39 +/- 0.02 was found for the olive oil sample under consideration.

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.

LC-DAD Determination of Fleroxacin in Bulk and Pharmaceutical Dosage Forms

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Determination and persistence of methiocarb in artichokes

A simple and rapid method for the determination of methiocarb in artichokes by high-performance liquid chromatography with UV detection is described. No derivatization is needed and the limit of determination (0.01 ppm) is analogous to that of fluorometric detection. The results of trials carried out with granular and liquid formulations of this active ingredient are also reported. Immediately after treatment with the liquid formulation methiocarb residues averaged 1.47 ppm, while after treatment with the granular formulation residues were considered fortuitous. The decay rate of methiocarb residues in artichokes shows that the decrease and eventual disappearance of this active ingredient can chiefly be ascribed to the dilution effect due to head growth.

Determination of flutamide in tablets by high-performance liquid chromatography

Flutamide is a potent antiandrogen used for the treatment of prostatic cancer. A simple, sensitive and accurate high-performance liquid Chromatographic (HPLC) method is presented for quantitative determination of flutamide in tablets, using a reversed-phase technique and UV detection at 240 nm. The isocratic elution was used to quantify the analyte. The samples were chromatographed on Luna-C18 column and the mobile phase was 0.05 M phosphate buffer pH 4.0 - acetonitrile (50:50, v/v). The method was linear between 2.9 - 11.6 mg L -1. Over the tested concentration range the intra-day relative standard deviation for replicate analysis in tablets ranged from 0.44 to 0.78%. It was also found that the excipients in the commercial tablets did not interfere with the method.

Sorção de sulfentrazone em função da textura, matéria orgânica e umidade de solos

Pós-graduação em Agronomia (Energia na Agricultura) - FCA

Análise químico-farmacêutica de teicoplanina em pó liofilizado

Pós-graduação em Ciências Farmacêuticas - FCFAR

Análise químico-farmacêutica de preparações injetáveis de ampicilina sódica

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

Desenvolvimento de sistemas de screening automatizados para determinação de sulfonamidas em mel e procedimento limpo para a quantificação de sulfaquinoxalina em medicamentos veterinários

Pós-graduação em Química - IQ