Carbadox (CBX) and olaquindox (OLA) were used in poultry and swine feed for growth promotion, to improve feed efficiency and increase the rate of weight gain. However, the use of these agents in feedingstuffs was prohibited because of concerns about their toxicity. Regulatory laboratories are required to have suitably validated analytical methods to ensure compliance with the ban. A quantitative and confirmatory method for determining the presence of CBX and OLA in poultry and swine feed by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was developed, optimized, and validated. The analytes extraction was performed with a mixture of water and acetonitrile (1:1v/v) and cleanup with hexane and C18 (dispersive phase). The method was evaluated by the following parameters: specificity, linearity, matrix effect, decision limits (CCα), detection capability (CCβ), accuracy, precision, limits of detection (LoD), limits of quantification (LoQ) and measurement uncertainty. The validated method presented a broad linear study range and no significant matrix effect. The limit of detection (LoD) was defined at 9 μg kg(-1) for CBX and 80 μg kg(-1) for OLA, and the limit of quantification (LoQ) was defined at 12 μg kg(-1) and 110 μg kg(-1) for CBX and OLA, respectively. The accuracy of the method was adequate for CBX and OLA. The recovery values found in the repeatability conditions were 99.41% for CBX and 104.62% for OLA. Under intralaboratory reproducibility conditions, the values were 98.63% for CBX and 95.07% for OLA. It was concluded that the performance parameters demonstrated total method adequacy for the detection and quantification of CBX and OLA in poultry and swine feedingstuffs.

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Assessment of heavy metal residues in Brazilian poultry and swine tissue [ ABSTRACTThe aim of this study was to investigate the presence of arsenic, lead and cadmium residues in samples of liver, kidney and muscle of poultry and swine during the years from 2002 to 2008. A total of 1978 samples were analyzed: 1031 of poultry and 947 of swine from Brazilian slaughterhouses. The samples were analyzed at the National Agricultural Laboratory using the atomic absorption spectrometry technique. In poultry, the arsenic residues were detected in 53.6% of liver samples, although no results have exceeded the MRL. In kidneys, 39.7% of the samples showed measurable residues and there was no violation of the limits. Regarding lead, there were 5 contaminated liver samples and 24 contaminated kidney samples (1.5 and 3.6% respectively). In muscle tissue there was only one sample with residues. For cadmium, 3.8% of the samples were found below MRL. Cadmium residues were found in 110 kidney samples (16.3% of tested), but only one exceeded the legislation limits. In swine, arsenic residues were detected in 15.3% of liver samples, although no results exceeded the MRL. In kidneys, 14.2% of samples showed measurable residues. However, there was no violation of limits. Regarding lead levels, 7 liver samples and 18 kidney samples were contaminated (2.6 and 2.7% respectively). Cadmium was found below MRL in 14.9% of the analyzed samples. In kidneys, 448 samples (67.8% of the total tested) had cadmium residues and 4 samples exceeded the legislation limits. During the seven years of study (2002)(2003)(2004)(2005)(2006)(2007)(2008), only 5 (0.25%) out of 1978 tested samples violated the Brazilian law. However, even with low levels of violation, monitoring is essential, since the number of samples with residues was often greater than the number of violations, and in some cases, such as cadmium in the kidneys, the majority of samples contained quantifiable residues and with levels often near the limits. INTRODUCTIONAmong the obstacles currently faced by the Brazilian meat industry, one of the most concerning problems is, undoubtedly, the potential presence of residues in animal tissues, giving emphasis to toxic metals. Moreover, cadmium, arsenic and lead stand out as the main inorganic pollutants present in products of animal origin.The presence of heavy metals in tissues and products of animal origin might be a result of a natural occurrence of those elements in the soil, as well as harmful industrial activity, which causes environmental contamination. These substances have a diverse toxicity degree. Hence, the analysis of these residues is of vital importance, aiming to obtain information on the regional levels. Eventually, such data will allow the identification of areas of environmental pollution (WHO, 2007).Heavy metals constitute the greatest source of inorganic pollutant that affects soil and water, being introduced into the atmosphere mainly through fertilizers, pesticides, combustion of coal and oil, vehicular emissions, mining, fo...

A análise de sedimentos do café torrado e moído faz parte dos procedimentos de controle da qualidade do produto. O objetivo desse trabalho foi validar um método de determinação de sedimentos em café torrado e moído baseada no princípio da decantação com o uso de solvente orgânico. Um conjunto de 30 amostras do produto foi fortificado em cinco níveis crescentes de sedimentos, 0,4%, 0,8%, 1,2%, 1,6% e 3% e analisado com duplicação por dois analistas, totalizando 120 resultados. Na avaliação da precisão em condições de repetibilidade e intermediária foi obtido índice de dispersão numa faixa adequada, abaixo de 20%, apropriada para uso. A exatidão e a precisão do método foram consideradas satisfatórias, tendo a incerteza abaixo de 15%, comprovando adequação do uso do método para análise de rotina na determinação de sedimentos em café torrado e moído. PALAVRAS-CHAVE:café em pó, análise do café, impurezas do café, microscopia.