Validação em laboratório de método analítico para determinação do teor de adipato e ftalato de di-(2-etil-hexila) utilizados como plastificantes em filmes flexíveis de PVC

The validation of analytical methods was carried out for di-(ethylhexyl) phthalate (DEHP) and adipate (DEHA) the determination of in PVC films. The level of DEHP and DEHA in samples was determined by leaving the film in contact with n-heptane during 48 hours and analysis in a gas chromatograph (GC) equipped with a flame ionization detector and fused silica column with 5% phenylmethyl silicone in the dimensions 30 m x 0.53 mm x 2.65 mm. The results for detection and the quantification limits were smaller than the restriction limits. The recovery rates of DEHP and DEHA were, respectively, 69.10 and 75.30 %.

Caracterização dos produtos líquidos e do carvão da pirólise de serragem de eucalipto

This study proposes the low temperature pyrolysis as an alternative conversion process for residual biomass and for obtaining gaseous, liquid and solid chemical feedstocks. Using a bench electrical pyrolysis oven, four product fractions from eucalyptus sawdust were obtained: a gaseous one, two liquid (aqueous and oily), and a solid residue (char). These products were characterized by different analytical methods. The liquid fractions showed themselves as potential sources for input chemicals. The residual char revealed appreciable adsorption capability. The process demonstrated good efficiency, generating at least two fractions of great industrial interest: bio oil and char.

Espécies reativas de oxigênio e de nitrogênio, antioxidantes e marcadores de dano oxidativo em sangue humano: principais métodos analíticos para sua determinação

We review here the chemistry of reactive oxygen and nitrogen species, their biological sources and targets; particularly, biomolecules implicated in the redox balance of the human blood, and appraise the analytical methods available for their detection and quantification. Those biomolecules are represented by the enzymatic antioxidant defense machinery, whereas coadjutant reducing protection is provided by several low molecular weight molecules. Biomolecules can be injured by RONS yielding a large repertoire of oxidized products, some of which can be taken as biomarkers of oxidative damage. Their reliable determination is of utmost interest for their potentiality in diagnosis, prevention and treatment of maladies.

Planilha de validação: uma nova ferramenta para estimar figuras de mérito na validação de métodos analíticos univariados

This work presents the VALIDATION SPREADSHEET, a public domain tool that can be used to evaluate the figures of merit for univariate analytical methods. A real example of BTEX determination in environmental samples is included to illustrate its use. The spreadsheet has been developed for Excel® and Open Office®, and is available on the internet at http//lqta.iqm.unicamp.br.

Caracterização das cinzas de incineração de resíduos industriais e de serviços de saúde

Three ash samples from an incinerator in Belo Horizonte (Brazil) were physically and chemically characterized. The chemical composition of the ashes was not always the same, neither in terms of the chemical species nor in terms of the quantities of those that are common to the three ashes. The ashes called CF1 and CF3D contain heavy metals above the detection limits of the analytical methods and the zinc concentration is high enough to justify treatment of the ashes. For these ashes, a high loss on ignition was found, indicating that the process of incineration might present failures.

Métodos de amostragem e análise para compostos reduzidos de enxofre atmosférico

This work presents a review of sampling and analytical methods that can be applied to atmospheric traces of reduced sulphur compounds (RSC) in the atmosphere. Sampling methodology involving discontinuous methods with preconcentration is mostly used. For the most part, adsorption on solids and cryogenic capture are applied as a procedure. The analysis of these compounds has been done mainly by gas chromatography with FPD, fluorescence and spectrophotometry. Advantages and disadvantages of the methodologies are also mentioned in this paper, aiming to guide the reader towards the most appropriate choice of a sampling and analytical method for RSCs.

Contaminantes voláteis provenientes de embalagens plásticas: desenvolvimento e validação de métodos analíticos

Plastic packaging materials intended for use in food packaging is an area of great interest from the scientific and economic point of view due to the irreversible internationalization and globalization process of food products. Nevertheless, a debate related to food safety aspects has emerged within the scientific community. Therefore, the development of analytical methods that allow identifying and quantifying chemical substances of toxicological potential in the packaging is considered essential. This article focuses on the main analytical methods, including validation parameters, as well as extraction and quantification techniques for determination of volatile organic compounds from food packaging materials.

A espectrometria atômica e a determinação de elementos metálicos em material polimérico

Polymeric materials are widely used in the chemical industry and are part of our daily lives. Inorganic species may be added to them as additives, anti-oxidizing agents, stabilizers, plasticizers, colorants and catalysts and may be present in a wide range of concentrations. Their determination demands the development of analytical methods considering different kinds of polymeric materials, their composition and the final use of the material. Although many different analytical techniques may be used, this review emphasizes those based on atomic absorption and emission spectrometry. Solid sampling techniques and digestion methods are described and discussed and compared considering published results.

Resíduos de agrotóxicos em alimentos: uma preocupação ambiental global - Um enfoque às maçãs

This paper describes the use of pesticides in agriculture. Research has shown that significant quantities of pesticide residues have been found in many types of foods. Thus, an overview is given of pesticide residue determinations in fruits and vegetables, with special attention to apples. The toxicity and the adverse effects possibly caused by the exposure of these compounds are alerting the scientific community to develop studies about the validation of analytical methods for multiresidue pesticide determination in these samples. This review shows that pesticide-residue determination in apples is becoming a very important and challenging issue.

Biodiesel: parâmetros de qualidade e métodos analíticos

The establishment of quality standards for biodiesel was a key step to win the confidence of the market and the automotive industry, thus ensuring the success of the new fuel. In this review are presented standard methods and other analytical methods suggested for analysis of biodiesel. The methods of analysis were divided into groups according to information that may be provided on the contaminants from the raw material of the production process, the molecular structures of biodiesel and its degradation during storage.

Contaminação de produtos de higiene e cosméticos por n-nitrosaminas

N-nitrosamines are carcinogenic compounds that have been found during the last three decades in a variety of consumer products, including cosmetic and personal care products, and their raw materials. These compounds are formed from amine precursors and nitrosating agents present in the formulations. This paper reviews the formation and occurrence of N-nitrosamines in cosmetic products, as well as presents considerations about analytical, toxicological and regulatory aspects.

Validação de métodos cromatográficos de análise: um experimento de fácil aplicação utilizando cromatografia líquida de alta eficiência (CLAE) e os princípios da "Química Verde" na determinação de metilxantinas em bebidas

The validation of analytical methods is an important step in quality control. The main objective of this study is to propose an HPLC experiment to verify the parameters of validation of chromatographic methods, based on green chemistry principles, which can be used in experimental courses of chemistry and related areas.

Otimização e validação de métodos analíticos para determinação de BTEX em água utilizando extração por headspace e microextração em fase sólida

Three analytical methods for the determination of BTEX in water were optimized and validated. With the best method the analytes were extracted of 10 mL of sample with 2.50 g of NaCl in headspace vial of 20 mL by HS and SPME to 40 ºC for 30 min for adsorption and to 250 ºC for 4 min for desorption and were analyzed by GC-MS. The recovery was between 97.9% and 104.3%, and the limit of detection was 2.4 ng L-1 for o-xylene. This method was using to analyze BTEX in water supply and surface water in Ouro Preto city. No sample had concentrations of BTEX above the legislation.

Losartan potassium dissolution test for drug release evaluation in pharmaceutical capsules using HPLC and UV spectrophotometry

This work describes the development and validation of a dissolution test for 50 mg losartan potassium capsules using HPLC and UV spectrophotometry. A 2(4) full factorial design was carried out to optimize dissolution conditions and potassium phosphate buffer, pH 6.8 as dissolution medium, basket as apparatus at the stirring speed of 50 rpm and time of 30 min were considered adequate. Both dissolution procedure and analytical methods were validated and a statistical analysis showed that there are no significant differences between HPLC and spectrophotometry. Since there is no official monograph, this dissolution test could be applied for quality control routine.

Desenvolvimento de métodos analíticos para determinação de agrotóxicos em sedimentos por cromatografia gasosa monodimensional e bidimensional abrangente com micro detector de captura de elétrons

The development of analytical methods for determination of eight pesticides of different chemical classes (trichlorfon, propanil, fipronil, propiconazole, trifloxystrobin, permethrin, difenoconazole and azoxystrobin) in sediments with gas chromatography-micro-electron capture detector (GC/µECD) and comprehensive two-dimensional gas chromatography with micro-electron capture detector (GCxGC/µECD) is described. These methods were applied to real sediment samples, and the best results were obtained using a 5% diphenyl-methylpolysiloxane column for 1D-GC. For GCxGC the same column was employed in the first dimension and a 50%-phenyl-methylpolysiloxane stationary phase was placed in the second dimension. Due to the superior peak capacity and selectivity of GCxGC, interfering matrix peaks were separated from analytes, showing a better performance of GCxGC.