Resposta antioxidante, formação de fitoquelatinas e composição de pigmentos fotoprotetores em Brachiaria decumbens Stapf submetida à contaminação com Cd e Zn

In order to evaluate the response of Brachiaria decumbens Stapf to Cd and Zn, plants were hydroponically exposed to 50 and 100 mmol L-1 of Cd and 500 and 2000 mmol L-1 of Zn. Metal content of shoots and roots was determined, as well as alterations in photosynthetic and photoprotective pigments, antioxidant metabolites and phytochelatin synthesis. Plants concentrated elevated levels of Cd and Zn, especially in roots. Zinc exposure negatively affected chlorophyll and β-carotene content, whereas the highest dose of Cd reduced VAZ cycle pigments and tocopherol levels in plant shoots. Cadmium was the maximum inducer of the phytochelatin synthesis pathway.

Aumento da resposta analítica por meio da otimização do sistema de injeção sem divisão de fluxo em cromatografia gasosa empregando a lei dos gases ideais

This paper reports the development of an easy, fast and effective procedure for the verification of the ideal gas law in splitless injection systems in order to improve the response. Results of a group of pesticides were used to demonstrate the suitability of the approach. The procedure helps establish experimental parameters through theoretical aspects. The improved instrumental response allowed extraction with lower sample volumes, the minimization of time and costs and the simplification of sample preparation.

Planejamento fatorial e superfície de resposta: otimização de um método voltamétrico para a determinação de ag(i) empregando um eletrodo de pasta de nanotubos de carbono

A factorial design applied in a voltammetric stripping method for the measurement of Ag(I) in natural water is described. The procedure is based on the effective pre-concentration of silver ions on electrode surface. The calibration graph was linear in the silver concentration range from 7.92 x 10"7 to 1.07 x 10"5 mol L"1 with a detection limit of 3.81 x 10-7 mol L-1. The determination of Ag(I) in natural water samples was carried out satisfactory with the proposed electrode.

Sistema de análises em fluxo polivalente para a determinação espectrofotométrica de fármacos

A flow system based on the sandwich technique is proposed for the sequential determination of ascorbic acid, dipyrone, acetylcysteine, captopril and paracetamol. The procedure is based on the reduction of Cu(II) by the analytes followed by the spectrophotometric measurement of the complex of Cu(I) with 2,2'-biquinoline 4,4'-dicarboxylic acid. Linear responses were achieved in the µmol L-1 range, with coefficients of variation better than 1.7%. Sampling rate was estimated as 60 determinations per hour, consuming 230 µg of BQA and generating 2.5 mL of waste per determination. Results for commercial samples agreed with those obtained by procedures recommended by the American and European pharmacopeias at the 95% confidence level.

Otimização das condições de extração de saponinas em Ampelozizyphus amazonicus usando planejamento experimental e metodologia de superfície de resposta

This works describes the use of experimental design and surface response methodology for optimization of saponin extraction from Ampelozizyphus amazonicus. For this purpose, a method employing extraction based on maceration assisted by ultrasound technique was utilized. The following factors were studied: extraction length of time and solvent composition. The total saponin was determined by using a gravimetric method and the results expressed by their relative proportion to total crude extract. For the specific condition, 60% hydro-alcoholic solution and 18 minutes extraction length of time has shown the best results. This method can be useful for extraction of substances with biological importance

Aspectos analíticos da resposta do detector de ionização em chama para ésteres de ácidos graxos em biodiesel e alimentos

The analysis of fatty acid (FA) esters by gas chromatography and flame ionization detector (FID) normally uses the normalization method. However, if one FA is wrongly estimated, the results could be greatly affected. In this study, methodologies using internal standards and correction factors for the FID response are described. The results show that by using theoretical correction factors associated to the internal standardization, the quantitative analyses of the FAs are expressed in mass, increasing the accuracy and facilitating the interpretation and comparison of the results for foods and biodiesels.

Identificação de extratos etanólicos de madeiras utilizando seu espectro eletrônico de absorção e análise multivariada

The application of multivariate analysis to spectrophotometric (UV) data was explored for distinguishing extracts of cachaça woods commonly used in the manufacture of casks for aging cachaças (oak, cabreúva-parda, jatobá, amendoim and canela-sassafrás). Absorbances close to 280 nm were more strongly correlated with oak and jatobá woods, whereas absorbances near 230 nm were more correlated with canela-sassafrás and cabreúva-parda. A comparison between the spectrophotometric model and the model based on chromatographic (HPLC-DAD) data was carried out. The spectrophotometric model better explained the variance data (PC1 + PC2 = 91%) exhibiting potential as a routine method for checking aged spirits.

Implantação e implementação das normas das Boas Práticas Laboratoriais (BPL) no laboratório de análises de resíduos da Universidade Estadual de Campinas

In the context of quality and good laboratory practices, the article recovers some historical data. From a specific Institutional situation (CPQBA/UNICAMP), is presented an experience of establishing and implementing a standard (NIT-DICLA-035) for good laboratory practice according to definitions of the Brazilian authority (INMETRO) responsible for regulating, monitoring, supervising and recognition in this area. The issue aims to focus on studies of pesticide residues in GLP parameters.

Caracterização de chás de genótipos de Lippia gracilis schauer através de perfil cromatográfico por CLAE-DAD combinado com análises quimiométricas

In order to evaluate the effects of environmental factors on the content of secondary metabolites, the chemical profiles of infusions from leaves of seven genotypes of Lippia gracilis Schauer, sourced from two locations (Sergipe and Bahia state) and collected during different seasons: summer (with and without irrigation) and winter, were determined by HPLC-DAD. The fingerprint chromatograms were analyzed by PCA to evaluate similarities and differences among the samples. Results revealed differences among genotypes collected and cultivated under the same conditions, suggesting that three genotypes have greater resistance to drought conditions.

Análises quali e quantitativas de micotoxinas em águas da cadeia produtiva do arroz por CCD e CCDAE

This study validated a simple and applied method for determining mycotoxins aflatoxin B1, aflatoxin B2, ochratoxin A, zearalenone and deoxynivalenol, in water from the rice production chain. Five solvent combinations for extraction were tested, with quantification performed by TLC/HPTLC and confirmation by LC-MS/MS. Mycotoxins in water from field and rice industries were evaluated. Mycotoxin recovery levels were around 90%. Two samples from rice parboiling waste were contaminated (deoxynivalenol/aflatoxin B1, 110/9 ng mL-1; and deoxynivalenol, 100 ng mL-1). Zearalenone, deoxynivalenol and ochratoxin A (36, 30 and 28%) were carried to soaking water during parboiling.

Influência de processos antagônicos no desenvolvimento de sistema de análises em fluxo para a determinação espectrofotométrica de propiltiouracil em medicamentos

A multi-commuted flow system was developed to determine propylthiouracil (PTU) based on the reaction of its thiol form with iminoquinone radical generated by the oxidation of N,N-dimethyl-p-phenylenediamine in an alkaline medium. PTU can be found in tautomeric forms and the tautomeric equilibrium was displaced to enhance the thiol form. However, the reaction product is unstable and its residence time in the flow path was carefully investigated. The proposed procedure showed good precision (< 1.5%) and a limit of detection (3s) of 0.11 mg L-1. High recoveries were obtained in the validation test. The procedure was employed for propylthiouracil determination in medications.

Validação de método quantitativo por RMN de ¹H para análises de formulações farmacêuticas

The need for effective and reliable quality control in products from pharmaceutical industries renders the analyses of their active ingredients and constituents of great importance. This study presents the theoretical basis of ¹H NMR for quantitative analyses and an example of the method validation according to Resolution RE Nº 899 by the Brazilian National Health Surveillance Agency (ANVISA), in which the compound paracetamol was the active ingredient. All evaluated parameters (selectivity, linearity, accuracy, repeatability and robustness) showed satisfactory results. It was concluded that a single NMR measurement provides structural and quantitative information of active components and excipients in the sample.

Métodos para análises de HPA e BTEX em águas subterrâneas de postos de revenda de combustíveis: um estudo de caso em Campo Grande, MS, Brasil

Two methods using headspace solid-phase microextraction and gas chromatography - mass spectrometry were developed for the determination of polycyclic aromatic hydrocarbons (PAH) and BTEX. Best results were obtained using DVB/CAR/PDMS fiber, with 10 min extraction at 25 °C and 0.15 min desorption at 260 °C (BTEX), and PDMS/DVB fiber, with 60 min extraction at 90 °C, 10% NaCl and 5 min desorption at 270 °C (PAH). LOD intervals were 3x10-2 - 5x10-2 µg L-1 (BTEX) and 1.6x10-3 - 1.4 µg L-1 (PAH). The methods were applied to forty-five groundwater samples from monitoring wells of gas stations and only benzene level exceeded the limit established by Brazilian regulations.

Uso de hardware de código fonte aberto "Arduino" para acionamento de dispositivo solenoide em sistemas de análises em fluxo

This paper describes the use of the open source hardware platform, denominated "Arduino", for controlling solenoid valves for solutions handling in flow analysis systems. System assessment was carried out by spectrophotometric determination of iron (II) in natural water. The sampling rate was estimated as 45 determinations per hour and the coefficient of variation was lower than 3%. Per determination, 208 µg of 1-10-phenanthroline and ascorbic acid were consumed, generating 1.3 mL of waste. "Arduino" proved a reliable microcontroller with low cost and simple interfacing, allowing USB communication for solenoid device switching in flow systems.

Autoagregação da 5,10,15,20-tetrakis(4-metoxifenil)porfirina (tmpp): estudos espectroscópicos e análises multivariadas

In this work, the spectroscopic properties of 5,10,15,20-tetrakis(4-methoxyphenyl)porphyrin (TMPP) in solvents of different polarities and water/ethanol mixtures were studied by electronic absorption spectroscopy and resonance light scattering associated with statistical analysis. The molar absorption coefficient and emission maximum of TMPP were dependent on solvent polarity. In the water/ethanol mixture, TMPP remained monomeric up to 25% of water, when it reaches its critical aggregation percentage. Oblique head-to-tail aggregate was found at intermediate water content (35 - 55%), while formation of a J-type aggregate was observed at higher water content (> 60%).