Toxicological and ultrastructural analysis of the impact of pesticides used in temperate fruit crops on two populations of Chrysoperla externa (Neuroptera, Chrysopidae)

This study aimed to evaluate the effects of (g a.i. L-1) abamectin (0.02), carbaryl (1.73), sulphur (4.8), fenitrothion (0.75), methidathion (0.4), and trichlorfon (1.5) on the survival of larvae and pupae, on the oviposition of adults and hatching of eggs from treated Chrysoperla externa third-instar larvae from two different populations (Bento Gonçalves and Vacaria, Rio Grande do Sul State, Brazil). Morphological changes caused by abamectin to eggs laid by C. externa from Vacaria population were evaluated by mean of ultrastructural analysis. The pesticides were applied on glass plates. Distilled water was used as control. For the evaluation of larvae mortality, a fully randomized experimental design in a 2 x 7 (two populations x seven treatments) factorial scheme was used, whereas for the effects of the compounds on oviposition capacity and egg viability, a 2 x 4 factorial scheme was used. Carbaryl, fenitrothion, and methidathion caused 100% mortality of larvae. Abamectin reduced the hatching of eggs from treated third-instar larvae of both populations; however, this pesticide presented highest toxicity on insects from Vacaria. The ultrastructural analysis showed that abamectin caused malformations in micropyle and in chorion external surface of C. externa eggs. Based in the total effect (E), carbaryl, fenitrothion, and methidathion are harmful to C. externa; trichlorfon is harmless to third-instar larvae, while abamectin and sulphur are harmless and slightly harmful to third-instar larvae from Bento Gonçalves and Vacaria, respectively.

Numerical analysis of the impact of charcoal production on soil hydrological behavior, runoff response and erosion susceptibility

The impact of charcoal production on soil hydraulic properties, runoff response and erosion susceptibility were studied in both field and simulation experiments. Core and composite samples, from 12 randomly selected sites within the catchment of Kotokosu were taken from the 0-10 cm layer of a charcoal site soil (CSS) and adjacent field soils (AFS). These samples were used to determine saturated hydraulic conductivity (Ksat), bulk density, total porosity, soil texture and color. Infiltration, surface albedo and soil surface temperature were also measured in both CSS and AFS. Measured properties were used as entries in a rainfall runoff simulation experiment on a smooth (5 % slope) plot of 25 x 25 m grids with 10 cm resolutions. Typical rainfall intensities of the study watershed (high, moderate and low) were applied to five different combinations of Ks distributions that could be expected in this landscape. The results showed significantly (p < 0.01) higher flow characteristics of the soil under charcoal kilns (increase of 88 %). Infiltration was enhanced and runoff volume reduced significantly. The results showed runoff reduction of about 37 and 18 %, and runoff coefficient ranging from 0.47-0.75 and 0.04-0.39 or simulation based on high (200 mm h-1) and moderate (100 mm h-1) rainfall events over the CSS and AFS areas, respectively. Other potential impacts of charcoal production on watershed hydrology were described. The results presented, together with watershed measurements, when available, are expected to enhance understanding of the hydrological responses of ecosystems to indiscriminate charcoal production and related activities in this region.

Local influence for spatial analysis of soil physical properties and soybean yield using student's t-distribution

The modeling and estimation of the parameters that define the spatial dependence structure of a regionalized variable by geostatistical methods are fundamental, since these parameters, underlying the kriging of unsampled points, allow the construction of thematic maps. One or more atypical observations in the sample data can affect the estimation of these parameters. Thus, the assessment of the combined influence of these observations by the analysis of Local Influence is essential. The purpose of this paper was to propose local influence analysis methods for the regionalized variable, given that it has n-variate Student's t-distribution, and compare it with the analysis of local influence when the same regionalized variable has n-variate normal distribution. These local influence analysis methods were applied to soil physical properties and soybean yield data of an experiment carried out in a 56.68 ha commercial field in western Paraná, Brazil. Results showed that influential values are efficiently determined with n-variate Student's t-distribution.

An improved method for measuring soil microbial activity by gas phase flow injection analysis

The rate of carbon dioxide production is commonly used as a measure of microbial activity in the soil. The traditional method of CO2 determination involves trapping CO2 in an alkali solution and then determining CO2 concentration indirectly by titration of the remaining alkali in the solution. This method is still commonly employed in laboratories throughout the world due to its relative simplicity and the fact that it does not require expensive, specific equipment. However, there are several drawbacks: the method is time-consuming, requires large amounts of chemicals and the consistency of results depends on the operator's skills. With this in mind, an improved method was developed to analyze CO2 captured in alkali traps, which is cheap and relatively simple, with a substantially shorter sample handling time and reproducibility equivalent to the traditional titration method. A comparison of the concentration values determined by gas phase flow injection analysis (GPFIA) and titration showed no significant difference (p > 0.05), but GPFIA has the advantage that only a tenth of the sample volume of the titration method is required. The GPFIA system does not require the purchase of new, costly equipment but the device was constructed from items commonly found in laboratories, with suggestions for alternative configurations for other detection units. Furthermore, GPFIA for CO2 analysis can be equally applied to samples obtained from either the headspace of microcosms or from a sampling chamber that allows CO2 to be released from alkali trapping solutions. The optimised GPFIA method was applied to analyse CO2 released from degrading hydrocarbons from a site contaminated by diesel spillage.

Efficiency of nitrogen fertilizer applied at corn sowing in contrasting growing seasons in Paraguay

In order to select soil management practices that increase the nitrogen-use efficiency (NUE) in agro-ecosystems, the different indices of agronomic fertilizer efficiency must be evaluated under varied weather conditions. This study assessed the NUE indices in no-till corn in southern Paraguay. Nitrogen fertilizer rates from 0 to 180 kg ha-1 were applied in a single application at corn sowing and the crop response investigated in two growing seasons (2010 and 2011). The experimental design was a randomized block with three replications. Based on the data of grain yield, dry matter, and N uptake, the following fertilizer indices were assessed: agronomic N-use efficiency (ANE), apparent N recovery efficiency (NRE), N physiological efficiency (NPE), partial factor productivity (PFP), and partial nutrient balance (PNB). The weather conditions varied largely during the experimental period; the rainfall distribution was favorable for crop growth in the first season and unfavorable in the second. The PFP and ANE indices, as expected, decreased with increasing N fertilizer rates. A general analysis of the N fertilizer indices in the first season showed that the maximum rate (180 kg ha-1) obtained the highest corn yield and also optimized the efficiency of NPE, NRE and ANE. In the second season, under water stress, the most efficient N fertilizer rate (60 kg ha-1) was three times lower than in the first season, indicating a strong influence of weather conditions on NUE. Considering that weather instability is typical for southern Paraguay, anticipated full N fertilization at corn sowing is not recommended due the temporal variability of the optimum N fertilizer rate needed to achieve high ANE.

Spatial statistical analysis and selection of genotypes in plant breeding

The objective of this study was to evaluate the efficiency of spatial statistical analysis in the selection of genotypes in a plant breeding program and, particularly, to demonstrate the benefits of the approach when experimental observations are not spatially independent. The basic material of this study was a yield trial of soybean lines, with five check varieties (of fixed effect) and 110 test lines (of random effects), in an augmented block design. The spatial analysis used a random field linear model (RFML), with a covariance function estimated from the residuals of the analysis considering independent errors. Results showed a residual autocorrelation of significant magnitude and extension (range), which allowed a better discrimination among genotypes (increase of the power of statistical tests, reduction in the standard errors of estimates and predictors, and a greater amplitude of predictor values) when the spatial analysis was applied. Furthermore, the spatial analysis led to a different ranking of the genetic materials, in comparison with the non-spatial analysis, and a selection less influenced by local variation effects was obtained.

A simple and rapid method for urinary acetone analysis by headspace/gas chromatography

Urinalysis of acetone is important to monitor workers occupationally exposed to acetone and/or isopropanol, as well as in diagnosis of some diseases related to lipid metabolism impairment. This work shows a sensitive, simple and rapid static headspace-gas chromatographic procedure for quantitative determination of acetone in urine. The method was applied to measure acetone in 207 samples from general population volunteers, resulting in a mean level of 1.12 mg/L (± 0.47) and a range of 0.20 - 1.95 mg/L. The method is reproducible and reliable, making it suitable for routine analysis of acetone in urine.

A thermogravimetric analysis of the combustion of a Brazilian mineral coal

Knowledge of coal combustion kinetics is crucial for burner design. This work aims to contribute on this issue by determining the kinetics of a particular Brazilian bituminous coal. Non-isothermal thermogravimetry was applied for determining both the pre-exponential factor and the activation energy. Coal samples of 10 mg and 775 mm mean size were used in synthetic air atmospheres (21 % O2). Heating rates from 10 to 50 ºC/min were applied until the temperature reached 850 ºC, which was kept constant until burnout. The activation energy for the primary and the secondary combustion resulted, respectively, in 135.1 kJ/mol and 85.1 kJ/mol.

Validation of an analytical methodology for the quantitative analysis of petroleum hydrocarbons in marine sediment samples

This work describes a validation of an analytical procedure for the analysis of petroleum hydrocarbons in marine sediment samples. The proposed protocol is able to measure n-alkanes and polycyclic aromatic hydrocarbons (PAH) in samples at concentrations as low as 30 ng/g, with a precision better than 15% for most of analytes. The extraction efficiency of fortified sediments varied from 65.1 to 105.6% and 59.7 to 97.8%, for n-alkanes and PAH in the ranges: C16 - C32 and fluoranthene - benzo(a)pyrene, respectively. The analytical protocol was applied to determine petroleum hydrocarbons in sediments collected from a marine coastal zone.

Photometric procedure for quantitative analysis of Aflatoxin B1 in peanuts by thin-layer chromatography using charge coupled device detector

A photometric procedure was developed for determination of aflatoxin B1 in peanuts by TLC-CCD technique. The quantification and detection limit were 1.2 μg kg-1 and 0.4 ng per spot, respectively, with mean recovery of 98%. The CCD camera is sufficiently sensitive to detect small changes in spots fluorescence intensity and the results for performance confirmed the efficiency of the method. Another important property of CCD detector is its linearity for a wide range of luminous stimulus determined by analysis of five-point calibration curves using the intensity of AFB1 fluorescence versus AFB1 concentration (0.8 to 4.8 ng per spot). The method was applied to the analysis of thirty nine peanut samples and aflatoxin B1 levels ranged from 16 to 115 μg kg-1. The TLC-CCD and the photometric procedure developed in this study demonstrated to be a simple and efficient tool for quantitative analyses of AFB1 in peanut samples.

Development and validation of a dissolution test with reversed-phase liquid chromatography analysis for rupatadine in tablet dosage forms

A dissolution test for in vitro evaluation of tablet dosage forms containing 10 mg of rupatadine was developed and validated by RP-LC. A discriminatory dissolution method was established using apparatus paddle at a stirring rate of 50 rpm with 900 mL of deaerated 0.01 M hydrochloric acid. The proposed method was validated yielding acceptable results for the parameters evaluated, and was applied for the quality control analysis of rupatadine tablets, and to evaluate the formulation during an accelerated stability study. Moreover, quantitative analyses were also performed, to compare the applicability of the RP-LC and the LC-MS/MS methods.

Simple and sensitive spectrophotometric methods for the analysis of mesalamine in bulk and tablet dosage forms

Three simple, sensitive, economical and reproducible spectrophotometric methods (A, B and C) are described for determination of mesalamine in pure drug as well as in tablet dosage forms. Method A is based on the reduction of tungstate and/or molybdate in Folin Ciocalteu's reagent; method B describes the reaction between the diazotized drug and α-naphthol and method C is based on the reaction of the drug with vanillin, in acidic medium. Under optimum conditions, mesalamine could be quantified in the concentration ranges, 1-30, 1-15 and 2-30 µg mL-1 by method A, B and C, respectively. All the methods have been applied to the determination of mesalamine in tablet dosage forms. Results of analysis are validated statistically.

Characterization of the antibiotic doripenem using physicochemical methods: chromatography, spectrophotometry, spectroscopy and thermal analysis

Doripenem was characterized through physicochemical and spectroscopic techniques, as well as thermal analysis. TLC (Rf = 0.62) and HPLC (rt = 7.4 min) were found to be adequate to identify the drug. UV and infrared spectra showed similar profile between doripenem bulk and standard. The ¹H and 13C NMR analysis revealed chemical shifts that allowed identifying the drug. Thermal analysis demonstrated three steps with mass loss, at 128, 178 and 276 ºC. The work was successfully applied to qualitative analysis of doripenem, showing the reported methods can be used for physicochemical characterization of doripenem

Liquid-phase microextraction for simultaneous chromatographic analysis of three antidepressant drugs in plasma

A method using Liquid Phase Microextraction for simultaneous detection of citalopram (CIT), paroxetine (PAR) and fluoxetine (FLU), using venlafaxine as internal standard, in plasma by high performance liquid chromatography with fluorescence detection was developed. The linearity was evaluated between 5.0 and 500 ng mL-1 (r > 0.99) and the limit of quantification was 2.0, 3.0 and 5.0 ng mL-1 for CIT, PAR and FLU, respectively. Therefore, it can be applied to therapeutic drug monitoring, pharmacokinetics or bioavailability studies and its advantages are that it necessary relatively inexpensive equipment and sample preparation techniques.

A quantitative validated method using liquid chromatography and chemometric analysis for evaluation of raw material oF Maytenus ilicifolia (Schrad.) Planch., Celastraceae

The hydroalcoholic extracts prepared from standard leaves of Maytenus ilicifolia and commercial samples of espinheira-santa were evaluated qualitatively (fingerprinting) and quantitatively. In this paper, fingerprinting chromatogram coupled with Principal Component Analysis (PCA) is described for the metabolomic analysis of standard and commercial espinheira-santa samples. The epicatechin standard was used as an external standard for the development and validation of a quantitative method for the analysis in herbal medicines using a photo diode array detector. This method has been applied for quantification of epicatechin in commercialized herbal medicines sold as espinheira-santa in Brazil and in the standard sample of M. ilicifolia.