Influence of digestion methods on the recovery of Iron, Zinc, Nickel, Chromium, Cadmium and Lead contents in 11 organic residues

There are currently many devices and techniques to quantify trace elements (TEs) in various matrices, but their efficacy is dependent on the digestion methods (DMs) employed in the opening of such matrices which, although "organic", present inorganic components which are difficult to solubilize. This study was carried out to evaluate the recovery of Fe, Zn, Cr, Ni, Cd and Pb contents in samples of composts and cattle, horse, chicken, quail, and swine manures, as well as in sewage sludges and peat. The DMs employed were acid digestion in microwaves with HNO3 (EPA 3051A); nitric-perchloric digestion with HNO3 + HClO4 in a digestion block (NP); dry ashing in a muffle furnace and solubilization of residual ash in nitric acid (MDA); digestion by using aqua regia solution (HCl:HNO3) in the digestion block (AR); and acid digestion with HCl and HNO3 + H2O2 (EPA 3050). The dry ashing method led to the greatest recovery of Cd in organic residues, but the EPA 3050 protocol can be an alternative method for the same purpose. The dry ashing should not be employed to determine the concentration of Cr, Fe, Ni, Pb and Zn in the residues. Higher Cr and Fe contents are recovered when NP and EPA 3050 are employed in the opening of organic matrices. For most of the residues analyzed, AR is the most effective method for recovering Ni. Microwave-assisted digestion methods (EPA3051 and 3050) led to the highest recovery of Pb. The choice of the DM that provides maximum recovery of Zn depends on the organic residue and trace element analyzed.

Biomass decomposition and nutrient release from black oat and hairy vetch residues deposited in a vineyard

A significant quantity of nutrients in vineyards may return to the soil each year through decomposition of residues from cover plants. This study aimed to evaluate biomass decomposition and nutrient release from residues of black oats and hairy vetch deposited in the vines rows, with and without plastic shelter, and in the between-row areas throughout the vegetative and productive cycle of the plants. The study was conducted in a commercial vineyard in Bento Gonçalves, RS, Brazil, from October 2008 to February 2009. Black oat (Avena strigosa) and hairy vetch (Vicia villosa) residues were collected, subjected to chemical (C, N, P, K, Ca, and Mg) and biochemical (cellulose - Cel, hemicellulose - Hem, and lignin - Lig content) analyses, and placed in litter bags, which were deposited in vines rows without plastic shelter (VPRWS), in vines rows with plastic shelter (VPRS), and in the between-row areas (BR). We collected the residues at 0, 33, 58, 76, and 110 days after deposition of the litter bags, prepared the material, and subjected it to analysis of total N, P, K, Ca, and Mg content. The VPRS contained the largest quantities and percentages of dry matter and residual nutrients (except for Ca) in black oat residues from October to February, which coincides with the period from flowering up to grape harvest. This practice led to greater protection of the soil surface, avoiding surface runoff of the solution derived from between the rows, but it retarded nutrient cycling. The rate of biomass decomposition and nutrient release from hairy vetch residues from October to February was not affected by the position of deposition of the residues in the vineyard, which may especially be attributed to the lower values of the C/N and Lig/N ratios. Regardless of the type of residue, black oat or hairy vetch, the greatest decomposition and nutrient release mainly occurred up to 33 days after deposition of the residues on the soil surface, which coincided with the flowering of the grapevines, which is one of the phenological stages of greatest demand for nutrients.

Cultivation of Flammulina velutipesmushroom using various agro-residues as a fruiting substrate

The objective of this work was to evaluate the feasibility of different agro-residues as a carbon source in the fruiting substrates of Flammulina velutipesmushroom and the effect of supplementation with the nitrogen sources spent brewer's yeast and rice bran. The following fruiting substrates were evaluated: rubber wood sawdust (SD), paddy straw (PS), palm empty fruit bunches (EFB), and palm-pressed fiber (PPF). Cultivation was done on each agro-residue, based on formulations consisting of two substrates at the ratios of 3:1, 1:1, and 1:3. Mycelial growth rate and basidiocarp yield were evaluated. The best fruiting substrates were PS+EFB (25:75), PS+PPF (50:50), and PPF (100), with biological efficiency of 185.09±36.98, 150.89±50.35, and 129.06±14.51%, respectively. No significant effects of supplementation with rice bran and spent yeast were observed on mycelial growth rate and biological efficiency. The cultivation of F. velutipes on oil palm wastes does not require additional nitrogen sources.

Residues of carbosulfan and its carbofuran metabolites and 3-hydroxy-carbofuran in oranges

The objectives of this study were to evaluate the residues of the insecticide carbosulfan and its carbofuran metabolites and 3-hydroxy-carbofuran in orange compartments (whole fruit, bagasse and juice) and comparison between the residual levels found in fruits with the maximum residue level and the safety interval established by the Brazilian legislation. Two field experiments were carried out, both with the following treatments: a-check; b-one application of 10 g of carbosulfan . 100 L-1 of water; c-one application with twice the rate applied in treatment b; d-four applications with the same rate applied in treatment b. Samples were taken at (-1), zero, 1, 3, 7, 14, 21 and 28 days after the last or unique application. The quantitative determinations were done by gas chromatography technique, using a nitrogen-phosphorus detector. The carbosulfan metabolism to its carbofuran metabolite was rapid (3 days), being both analytes concentrated in the bagasse (peel + flavedo + albedo). However, the metabolism of carbofuran to 3-hydroxy-carbofuran was of low intensity or this metabolite was quickly dissipated. Carbosulfan residues and its metabolites did not penetrate into the fruit, thus not contaminating the juice. The use of the pesticide was adequate, with respect to fruit consumption, in relation to the Brazilian legislation.

Spectrophotometric determination of cefaclor in pharmaceutical preparations

A simple spectrophotometric method is proposed for the determination of cefaclor. The method involves alkaline hydrolysis of the drug in ammonia buffer solution at pH 10 to yield diketopiperazine-2,5-dione derivative and subsequent measurement at 340 nm. Beer's law is obeyed in the concentration range 1.8 - 55 mg/mL. The proposed method was successfully applied to the determination of cefaclor in pharmaceutical formulations.

Fármacos no meio ambiente

Pharmaceutical drugs have been detected in sewage treatment plants, surface waters, underground waters and potable waters. Some investigations have been conducted in several countries such as Germany, Brazil, Canada, United States, The Netherlands, England and Italy. Patients and animals excrete part of pharmaceuticals used for human and veterinary medicine after administration in domestic sewage or on the soil. Drugs residues which have not been completely removed during passage through a sewage treatment plant (STP) enter the aquatic environment. The effects of such residual drugs in terrestrial and aquatic organisms are scarcely known.

A simplified procedure for determination of clofentezine residues in fruits by liquid chromatography with UV detection

A rapid and sensitive method is described for the determination of clofentezine residues in apple, papaya, mango and orange. The procedure is based on the extraction of the sample with a hexane:ethyl acetate mixture (1:1, v/v) and liquid chromatographic analysis using UV detection. Mean recoveries from 4 replicates of fortified fruit samples ranged from 81% to 96%, with coefficients of variation from 8.9% to 12.5%. The detection and quantification limits of the method were of 0.05 and 0.1 mg kg-1, respectively.

Investigation of the occurrence of pesticide residues in rural wells and surface water following application to tobacco

In this work the exposure of wells and surface water to pesticides, commonly used for tobacco cropping, was assessed. Water consumption wells and surface water flows were sampled at different times. After a preconcentration step with solid phase extraction (SPE), the selected pesticides were determined by gas chromatography with electron capture detection (GC-ECD) or high performance liquid chromatography with diode array detection (HPLC-DAD). No pesticides were detected in the well water samples and surface water flow in the winter season. However, in the spring and summer higher concentrations of chlorpyrifos and imidacloprid were found in the water source samples. Atrazine, simazine and clomazone were also found. The occurrence of pesticides in collected water samples was related with the application to tobacco.

Simultaneous spectrophotometric determination of ezetimibe and simvastatin in pharmaceutical preparations using chemometric techniques

Two spectrophotometric methods are described for the simultaneous determination of ezetimibe (EZE) and simvastatin (SIM) in pharmaceutical preparations. The obtained data was evaluated by using two different chemometric techniques, Principal Component Regression (PCR) and Partial Least-Squares (PLS-1). In these techniques, the concentration data matrix was prepared by using the mixtures containing these drugs in methanol. The absorbance data matrix corresponding to the concentration data matrix was obtained by the measurements of absorbances in the range of 240 - 300 nm in the intervals with Δλ = 1 nm at 61 wavelengths in their zero order spectra, then, calibration or regression was obtained by using the absorbance data matrix and concentration data matrix for the prediction of the unknown concentrations of EZE and SIM in their mixture. The procedure did not require any separation step. The linear range was found to be 5 - 20 µg mL-1 for EZE and SIM in both methods. The accuracy and precision of the methods were assessed. These methods were successfully applied to a pharmaceutical preparation, tablet; and the results were compared with each other.

Development and application of spectrophotometric method for the determination of cefaclor in pharmaceutical formulations

A simple, fast and sensitive spectrophotometric method for the determination of cefaclor in pharmaceutical raw and dosage forms based on reaction with ninhydrin is developed, optimized and validated. The purple color (Ruhemenn's purple) that resulted from the reaction was stabilized and measured at 560 nm. Beer's law is obeyed in the concentration range of 4-80 µg mL-1 with molar absorptivity of 1.42 × 10(5) L mole-1 cm-1. All variables including the reagent concentration, heating time, reaction temperature, color stability period, and cefaclor/ninhydrin ratio were studied in order to optimize the reaction conditions. No interference was observed from common pharmaceutical adjuvant. The developed method is easy to use, accurate and highly cost-effective for routine studies relative to HPLC and other techniques.

Flow-injection spectrophotometric determination of tetracycline and doxycycline in pharmaceutical formulations using chloramine-T as oxidizing agent

A flow-injection (FI) spectrophotometric procedure is proposed for tetracycline (TC) and doxycycline (DXC) determination in pharmaceuticals. The method is based on the reaction of oxidation of these drugs by chloramine-T in alkaline medium producing red color products (λmax = 535 and 525 nm). Beer´s law is obeyed in the concentration range from 6.62 x 10-5 to 7.72 x 10-4 mol L-1 and 5.37 x 10-5 to 7.16 x 10-4 mol L-1 for TC and DXC, respectively. The analytical frequency was 50 h"1 and 45 h-1 for TC and DXC, respectively. The results obtained by the proposed method were in good agreement with those obtained by the official method at 95% confidence level.

Development and validation of a GC-FID assay for determination of fluvastatin in pharmaceutical preparations

A gas chromatographic method has been developed for the assay of fluvastatin sodium (FLU). FLU was silylated with N,O-bis(trimethylsilyl)trifluoroacetamide-1% trimethylchlorosilane at 90 ºC for 30 min and analysed in a DB-1 column by capillary gas chromatograph with a flame ionization detector. The method was validated. The assay was linear over the concentration range at 10.0 to 50.0 µg mL-1. The limit of detection and the limit of quantitation were 1.0 and 3.0 µg mL-1, respectively. The recoveries of FLU derivatives were in the range of 99.25-99.80%. In inter-day and intra-day analysis, the values of relative standard deviation (%) and the relative mean error (%) were found between 0.20-0.80% and -0.20-0.75%, respectively. The developed method was succesfully applied to analyze the FLU content in tablet formulation. The results were statistically compared with those obtained by the official method, and no significant difference was found between the two methods. Therefore, it can be recommended for the quality control assay of FLU in pharmaceutical industry.

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.

Flow injection green method for the quantitative analysis of ketoconazole in pharmaceutical preparations

A flow injection method for the quantitative analysis of ketoconazole in tablets, based on the reaction with iron (III) ions, is presented. Ketoconazole forms a red complex with iron ions in an acid medium, with maximum absorbance at 495 nm. The detection limit was estimated to be 1×10--4 mol L-1; the quantitation limit is about 3×10--4 mol L-1 and approximately 30 determinations can be performed in an hour. The results were compared with those obtained with a reference HPLC method. Statistical comparisons were done using the Student's t procedure and the F test. Complete agreement was found at the 0.95 significance level between the proposed flow injection and the HPLC procedures. The two methods present similar precision, i.e., for HPLC the mean relative standard deviation was ca. 1.2% and for FIA ca. 1.6%.

Development of a simple, rapid and validated spectrophotometric method for nitazoxanide in pharmaceutical formulations and comparison with HPLC

A rapid, economical, reproducible, and simple direct spectrophotometric method was developed and validated for the assay of nitazoxanide in pharmaceutical formulations. Nitazoxanide concentration was estimated in water at 345 nm and pH 4.5. The method was suitable and validated for specificity, linearity, precision, and accuracy. There was no interference of the excipients in the determination of the active pharmaceutical ingredient. The proposed method was successfully applied in the determination of nitazoxanide in coated tablets and in powders for oral suspension. This method was compared to a previously developed and validated method for liquid chromatography to the same drug. There was no significative difference between these methods for nitazoxanide quantitation.