Laboratorio Nacional Agropecuario LANAGRO MG

Pedro Leopoldo, Brazil

Laboratorio Nacional Agropecuario LANAGRO MG

Pedro Leopoldo, Brazil
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Silva G.R.D.,Federal University of Minas Gerais | Lima J.A.,Laboratorio Nacional Agropecuario Lanagro MG | Souza L.F.D.,Laboratorio Nacional Agropecuario Lanagro MG | Santos F.A.,Laboratorio Nacional Agropecuario Lanagro MG | And 3 more authors.
Talanta | Year: 2017

A quantitative and confirmatory multiresidue method for determining the presence of avermectins, benzimidazoles and nitroimidazoles in bovine muscle tissue by ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) was developed, optimized and validated, using a QuEChERS extraction. The evaluated performance parameters were linearity, selectivity, matrix effect, decision limits (CCα), detection capability (CCβ), limits of detection (LOD), limits of quantification (LOQ), accuracy, precision and robustness. The validated method exhibited linearity with coefficient of determination (R2) higher than 0.90 in the working range from 0.5 to 2.0 times the maximum residue limit (MRL) or the minimum required performance level (MRPL) for the studied analytes, except for closantel, for which the linear study range was defined from 50 to 200 µg kg−1. The method was selective in the presence of macrolides and lincosamides for all the studied analytes. The LOD varied from 0.007 to 66.715 µg kg−1, whereas LOQ values ranging from 0.011 to 113.674 µg kg−1 were found. The results of the evaluation of the accuracy and precision were satisfactory for all the studied analytes, and according to the assessment of the robustness, the method was not robust only for the analytes abamectin, moxidectin, doramectin fenbendazole sulfone, closantel, thiabendazole, hydroxyl-metronidazole and ronidazole. The performance parameters demonstrated total method adequacy for the detection and quantification of avermectins, benzimidazoles and nitroimidazoles residues in bovine muscle tissues. © 2017 Elsevier B.V.


Rocha D.G.,Federal University of Minas Gerais | Santos F.A.,Laboratorio Nacional Agropecuario LANAGRO MG | da Silva J.C.C.,Federal University of Minas Gerais | Augusti R.,Federal University of Minas Gerais | Faria A.F.,Federal University of Minas Gerais
Journal of Chromatography A | Year: 2015

This work involved the optimization and validation of two methods according to the Commission Decision 2002/657/EC directives for determining fluoroquinolones residues in samples of poultry muscle and kidney: ciprofloxacin, danofloxacin, difloxacin, enrofloxacin, flumequine, marbofloxacin, nalidixic acid, norfloxacin, ofloxacin, oxolinic acid, pipemidic acid and sarafloxacin. The extraction procedure was based on a QuEChERS approach, whose optimization employed a Box-Behnken 33 factorial design. A liquid chromatography-tandem mass spectrometry method (LC-MS/MS) was developed for determining the twelve analytes using the multiple reaction monitoring mode (MRM). Accuracy, evaluated by recovery studies, varied from 88.8 to 112.2% for the selected levels with RSD values lower than 12.3%. The second validated method employed high resolution mass spectrometry (HRMS) performed in the single ion monitoring mode (SIM), determining nine among twelve analytes. The validation parameters were evaluated as satisfactory, with recoveries from 82.5 to 114.4% and RSD lower than 8.7%. Decision limits and detection capabilities for both methods were reported. The two methods were statistically compared using the Student's t test, at 95% confidence level, resulting in no significant difference. © 2015 .


Cassimiro Belo R.F.,Federal University of Minas Gerais | Nunes C.M.,Laboratorio Nacional Agropecuario LANAGRO MG | Vieira Dos Santos E.,Laboratorio Nacional Agropecuario LANAGRO MG | Augusti D.V.,Laboratorio Nacional Agropecuario LANAGRO MG | Pissinatti R.,Laboratorio Nacional Agropecuario LANAGRO MG
Analytical Methods | Year: 2012

This article describes a method for the quantification of seven Polycyclic Aromatic Hydrocarbons (PAHs) in edible oils (soy, sunflower and olive). It involved the application of a low-volume liquid-liquid extraction (LLE) technique followed by a solid-phase extraction (SPE) clean-up with C 18 and silica cartridges. Separation and analysis of compounds were performed by gas chromatography coupled to mass spectrometry (GC-MS). 13C-labeled PAHs as internal standards were used to aid the identification of compounds and to determine the efficiency of the extraction method in an isotope dilution mass spectrometry (IDMS) approach. Low-volume LLE and SPE clean-up procedures allowed the reduction of solvent consumption, eliminated the necessity of a previous saponification step and provided less sample preparation time when compared to traditional PAHs extraction and clean-up methods. The analytical procedure was validated according to recommendations of the European Commission Decision 2002/657/EC and European Commission Regulations (2007/333/EC and 2011/836/EU). Acceptable values (except for chrysene) were obtained for the following parameters: linearity (r 2 > 0.98), limit of quantification (0.12 < LOQ < 0.68 μg kg-1), limit of detection (0.04 < LOD < 0.23 μg kg -1), trueness (recovery rates and certified reference material normalized error), and precision (repeatability and intermediate precision). Recoveries higher than 80% were attained for seven PAHs, at three concentration levels (0.75, 2.00 and 4.00 μg kg-1). This validated method will be used by the Ministry of Agriculture, Livestock and Food Supply in Brazil. © 2012 The Royal Society of Chemistry.


Dias C.,Federal University of Minas Gerais | Oliveira F.A.,Laboratorio Nacional Agropecuario LANAGRO MG | Madureira F.D.,Laboratorio Nacional Agropecuario LANAGRO MG | Silva G.,Laboratorio Nacional Agropecuario LANAGRO MG | And 2 more authors.
Food Additives and Contaminants - Part A Chemistry, Analysis, Control, Exposure and Risk Assessment | Year: 2013

Coffee is a major tropical agricultural commodity and represents a significant fraction of the economy of many countries. However, certain plant and animal species can damage coffee crops, affecting trade. A solution to this issue is the use of pesticides, some of which are harmful to human health and the environment. This work consisted of the development of a multi-residue method for the analysis of pesticides in coffee by using LC-MS/MS. The QuEChERS extraction procedure was used. The following analytical parameters were optimised: selectivity, analytical range, linearity, LOD, LOQ, precision (RSD%) and recovery of the method. The results showed that the method is selective, as they were linear in the range of 10.0-100.0 μg kg-1. The sensitivity, recovery and precision were adequate for the multi-residue analysis of pesticides in coffee. The method was applied to the analyses of 15 Brazilian coffee samples. © 2013 Copyright Taylor & Francis.


Lopes R.P.,Federal University of Minas Gerais | De Freitas Passos T.E.,Laboratorio Nacional Agropecuario LANAGRO MG | De Alkimim Filho J.F.,Laboratorio Nacional Agropecuario LANAGRO MG | Vargas E.A.,Laboratorio Nacional Agropecuario LANAGRO MG | And 2 more authors.
Food Control | Year: 2012

A multiresidue method for the quantification of 13 sulfonamides in animal feed is described. It involves the application of a modified QuEChERS procedure followed by HPLC-MS/MS (high performance liquid chromatography coupled to tandem mass spectrometry) analysis. The best conditions for the extraction solution and PSA (primary secondary amine) mass were determined. After optimization, the method was validated according to the European Commission Decision 2002/657/EC. The validation levels employed were 25, 50 and 75 μg kg -1. Acceptable values were obtained for the following parameters: linearity (0.9864 < r 2 < 0.9993), decision limit (50.4 μg kg -1 < CC α < 55.8 μg kg -1), detection capability (50.7 μg kg -1


PubMed | Federal University of Minas Gerais and Laboratorio Nacional Agropecuario LANAGRO MG
Type: Journal Article | Journal: PloS one | Year: 2016

The depletion times of enrofloxacin and its metabolite ciprofloxacin as well as sulfaquinoxaline and oxytetracycline were evaluated in broiler chickens that had been subjected to pharmacological treatment. The presence and residue levels of these drugs in muscle tissue were evaluated using an ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method that was validated in this work. The results showed the presence of all antimicrobial residues; however, the presence of residues at concentrations higher than the drugs maximum residue limit (MRL) of 100 g kg-1 was found only during the treatment period for oxytetracycline and until two days after discontinuation of the medication for enrofloxacin, ciprofloxacin and sulfaquinoxaline. It was concluded that the residues of all antimicrobials were rapidly metabolized from the broiler muscles; after four days of withdrawal, the levels were lower than the limit of quantification (LOQ) of the method for the studied analytes.


PubMed | Federal University of Minas Gerais and Laboratorio Nacional Agropecuario Lanagro MG
Type: | Journal: Talanta | Year: 2015

Methods are validated by a process that defines the analytical requirements and confirms that the investigated method is capable of performing consistently. A quantitative and confirmatory method for determining the presence of -lactam and tetracycline multiresidues in avian, bovine, equine, and swine kidney tissues using ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed, optimized, and validated. Analytes were extracted from the kidneys by a mixture of water and acetonitrile, and the extract was then purified with hexane and C18 (dispersive phase). The method was evaluated by the following parameters: linearity, matrix effect, specificity, decision limits (CC), detection capability (CC), accuracy, precision, trueness, limits of detection (LOD), limits of quantification (LOQ), and robustness. The validated method presented a broad linear study range and significant matrix effect. The limit of detection (LOD) was defined from 2.5 to 25.0 g kg(-1), and the limit of quantification (LOQ) was defined from 5.0 to 50.0 g kg(-1) for individual analytes. The resultant recovery values ranged from 98.1% to 107.3% in repeatability conditions and from 95.2% to 106% under intralaboratory reproducibility conditions for the studied analytes. It was concluded that the performance parameters demonstrated total method adequacy for detecting and quantifying -lactam and tetracycline residues in swine, equine, bovine, and avian kidneys.


PubMed | Federal University of Minas Gerais and Laboratorio Nacional Agropecuario Lanagro MG
Type: | Journal: Talanta | Year: 2015

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 (CC), detection capability (CC), 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 g kg(-1) for CBX and 80 g kg(-1) for OLA, and the limit of quantification (LoQ) was defined at 12 g kg(-1) and 110 g 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.


de Oliveira M.L.G.,Laboratorio Nacional Agropecuario LANAGRO MG | Madureira F.D.,Laboratorio Nacional Agropecuario LANAGRO MG | Aurelio F.,Laboratorio Nacional Agropecuario LANAGRO MG | Pontelo A.P.,Laboratorio Nacional Agropecuario LANAGRO MG | And 3 more authors.
Food Additives and Contaminants - Part A Chemistry, Analysis, Control, Exposure and Risk Assessment | Year: 2012

An EI-GC/MS method for the determination of pesticide residues in vegetable matrices with high water content was validated using papaya samples. The validation of a multi-residue pesticide method was in agreement with national and international regulations enabling the Ministry of the Agriculture, Livestock and Food Supply of Brazil to cover a large number of matrices and pesticide residues in its monitoring and control programmes. The extraction used 60 mL of ethyl acetate and 30 g of sample previously processed. After extraction, clean-up of all the extracts was carried out by percolation through GBC cartridges. The samples were then injected in an EI-GC/MS system. Calibration curves were prepared in quadruplet by fortifying blank extracts with a standard solution containing all the pesticides studied at 0.000, 0.005, 0.010, 0.020, 0.030, 0.050, 0.080 and 0.100 mg kg-1. For the recovery study, blank samples were fortified at 0.010, 0.020, 0.030, 0.050 and 0.080 mg kg-1 and then submitted to the extraction procedure. The complete procedure was repeated over four different days by two analysts. The regression parameters of calibration curves were calculated for each validation day. Linearity, selectivity, specificity, robustness, limits of detection and quantification were also assessed. The uncertainty was estimated for each analyte at each spike level studied. The method had recoveries between 91% and 105% and precision results ≤20%. Limits of quantification were below or equal to the maximum residue limits (MRLs) regulated by Brazilian legislation. The MRLs of the selected pesticides are not regulated by CODEX Alimentarius. The results are also in agreement with SANCO/10684/2009. © 2012 Taylor & Francis.


Madureira F.D.,Laboratorio Nacional Agropecuario LANAGRO MG | da Silva Oliveira F.A.,Laboratorio Nacional Agropecuario LANAGRO MG | de Souza W.R.,Laboratorio Nacional Agropecuario LANAGRO MG | Pontelo A.P.,Laboratorio Nacional Agropecuario LANAGRO MG | And 2 more authors.
Food Additives and Contaminants - Part A Chemistry, Analysis, Control, Exposure and Risk Assessment | Year: 2012

A method using QuEChERS extraction and LC-MS/MS in electrospray positive ionisation mode was developed and validated for the analysis of 90 pesticides in a high water content matrix (tomato) in a single chromatographic run. To assess the intra-laboratory reproducibility of the method, validation was conducted on four different days by two different analysts. The validation data was treated using a spreadsheet developed in-house, which sets the most appropriate model for linear fit by determining whether the residuals of the calibration curves are homocedastic or heterocedastic. A statistical test for the significance of regression was also carried out. Calibration was always matrix-matched and the curves were obtained over the range 0.0075-0.10 or 0.020-0.125 mg kg-1. Identification of analytes was based on retention times and MRM ratios. Recoveries were assessed at four different levels for each analyte and were between 73 and 106%, with relative standard deviations under reproducibility conditions of <20%. The measurement uncertainties of the method for each pesticide analysed were below 50%. Previous validation of the same method, applied to papaya samples and satisfactory results obtained in various proficiency tests with different high water content matrices, demonstrated the applicability of the method to these classes of commodities, without clean-up. The validated method will be applied routinely in the pesticide residues monitoring programme that constitutes the National Residue and Contaminant Control Plan of Brazil. © 2012 Taylor & Francis.

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