Laboratorio Nacional Agropecuario LANAGRO RS

Porto Alegre, Brazil

Laboratorio Nacional Agropecuario LANAGRO RS

Porto Alegre, Brazil
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Daguer H.,Laboratorio Nacional Agropecuario LANAGRO RS | Assis M.T.Q.M.,Federal University of Santa Catarina | Bersot L.D.S.,Federal University of Paraná
Ciencia Rural | Year: 2010

Meat production and consumption growth has been accompanied by a wide diversification of processed products, while the trading of non-processed meat has decreased. Phosphates and non-meat proteins, mainly soy and whey proteins, are widely used to marinate meat, improving its texture and promoting the fluids retention that can bring sensorial benefits to the consumers and improve producers' yield. On this technology, the main processes employed are the injection and the tumbling of raw materials. However, some fraudulent practices must be avoided by the meat inspection service, setting limits to the replacement of meat proteins by water and non-meat ingredients. The present article reviewed the main aspects of the use of such ingredients enlightening the importance of appropriate analytical techniques to control injected, and marinated products.


Hoff R.,Federal University of Rio Grande do Sul | Hoff R.,Laboratorio Nacional Agropecuario LANAGRO RS | Pizzolato T.M.,Federal University of Rio Grande do Sul | Diaz-Cruz M.S.,IDAEA
Trends in Environmental Analytical Chemistry | Year: 2016

The sulfonamides were the first class of anti-infective agents discovered in therapy for the treatment of infectious diseases, even prior to the discovery of penicillin. Since their discovery, sulfonamides (SAs) are used in the human and veterinary medicine. Through the organic waste or manure utilization or other routes as discharge of effluent wastewaters into surface water, SAs could migrate to soil and water, affecting microbiota, fauna and flora. SAs are a ubiquitous group of drugs, widely detected in environment and specific resistance genes occurrence have been correlated with SAs presence. Thus, the development of robust and reliable method for SAs monitoring is of great concern. Trace and ultra-trace levels of SAs can be detected in several matrices. In order to achieve this level of detection sample preparation strategies combined with advanced mass spectrometry techniques as triple quadrupole, linear ion trap and time of flight mass detection associated with post-run strategies were currently used to SAs monitoring. In this work, a review of the most recent published reports, including the last five years, is presented. © 2016 Elsevier B.V.


Bittencourt M.S.,Laboratorio Nacional Agropecuario LANAGRO RS | Martins M.T.,Laboratorio Nacional Agropecuario LANAGRO RS | Martins M.T.,Federal University of Rio Grande do Sul | de Albuquerque F.G.S.,Laboratorio Nacional Agropecuario LANAGRO RS | And 4 more authors.
Food Additives and Contaminants - Part A Chemistry, Analysis, Control, Exposure and Risk Assessment | Year: 2012

A multiresidue and multiclass method based on liquid chromatography-tandem mass spectrometry for the determination of antibacterials was developed and validated for screening purposes. This method can be applied to commonly used drugs in veterinary medicine such as tetracyclines, quinolones and sulfonamides. Sample preparation consists in cell disruption with sand (previously purified and washed with EDTA 100 mM) followed by protein precipitation with acidified acetonitrile. Validation was conducted in accordance to European Union requirements (2002/657/EC) for qualitative methods covering detection capability (CCβ), selectivity, specificity and stability. The method enabled the detection of 21 different drugs and had a false-compliant rate of <5% (β error) at between 25% and 50% of the maximum residue levels established by legal authorities. The methodology was successfully applied to incurred poultry samples. © 2012 Taylor & Francis.


Jank L.,Laboratorio Nacional Agropecuario Lanagro RS | Jank L.,Federal University of Rio Grande do Sul | Hoff R.B.,Laboratorio Nacional Agropecuario Lanagro RS | Hoff R.B.,Federal University of Rio Grande do Sul | And 4 more authors.
Food Additives and Contaminants - Part A Chemistry, Analysis, Control, Exposure and Risk Assessment | Year: 2012

This study presents the development and validation of a simple method for the detection and quantification of six β-lactam antibiotics residues (ceftiofur, penicillin G, penicillin V, oxacillin, cloxacillin and dicloxacillin) in bovine milk using a fast liquid-liquid extraction (LLE) for sample preparation, followed by liquid chromatography-electrospray-tandem mass spectrometry (LC-MS/MS). LLE consisted of the addition of acetonitrile to the sample, followed by addition of sodium chloride, centrifugation and direct injection of an aliquot into the LC- MS/MS system. Separation was performed in a C18 column, using acetonitrile and water, both with 0.1% of formic acid, as mobile phase. Method validation was performed according to the criteria of Commission Decision 2002/657/EC. Limits of detection ranged from 0.4 (penicillin G and penicillin V) to 10.0 ngml-1 (ceftiofur), and linearity was achieved. The decision limit (CCα), detection capability (CCβ), accuracy, inter- and intra-day repeatability of the method are reported. © 2012 Taylor & Francis.


Barreto F.,Laboratorio Nacional Agropecuario LANAGRO RS | Barreto F.,Federal University of Rio Grande do Sul | Ribeiro C.,Laboratorio Nacional Agropecuario LANAGRO RS | Hoff R.B.,Laboratorio Nacional Agropecuario LANAGRO RS | And 2 more authors.
Food Additives and Contaminants - Part A Chemistry, Analysis, Control, Exposure and Risk Assessment | Year: 2012

A reliable, simple and sensitive liquid chromatography-electrospray ionisation-tandem mass spectrometry (LC-ESI-MS/MS) confirmation method has been developed for chloramphenicol (CAP) determination in honey, fish and prawns. For honey, samples were extracted with ethyl acetate, an aliquot was evaporated to dryness and re-dissolved in mobile phase. For fish and prawns, tissues were extracted with acetonitrile and chloroform. The organic layer was evaporated to dryness and the residue was re-constituted with water: acetonitrile (90:10). LC separation was achieved on a C18 column with gradient elution using a mobile phase of acetonitrile and water. Analysis was carried out on a triple-quadrupole tandem mass spectrometer in multiple reaction monitoring (MRM) mode via electrospray interface operated in negative ionisation mode, with deuterated chloramphenicol-d5 (d5-CAP) as internal standard. Method validation was performed according to the criteria of Commission Decision 2002/657/EC. Four identification points were obtained for CAP with one precursor ion and two product ions. The limit of detection (LOD) was 0.02μg kg-1. Linear calibration curves were obtained over concentration ranges of 0.1-1.0 μg kg-1 in tissues. Mean recoveries ranged from 85.5% to 115.6%, with the corresponding intra- and inter-day variation ranging from 1.0% to 22.5%, depending on matrix type and level of concentration. The decision limit (CCα) and detection capability (CCβ) of the method were obtained for all matrices: 0.04 and 0.06 μg kg-1, respectively, for prawns and fish and 0.05 and 0.09 μg kg-1 for honey. © 2012 Taylor & Francis.


Hoff R.B.,Federal University of Rio Grande do Sul | Hoff R.B.,Laboratorio Nacional Agropecuario LANAGRO RS | Barreto F.,Laboratorio Nacional Agropecuario LANAGRO RS | Melo J.,Laboratorio Nacional Agropecuario LANAGRO RS | And 3 more authors.
Food Additives and Contaminants - Part A Chemistry, Analysis, Control, Exposure and Risk Assessment | Year: 2014

Validation is a required process for analytical methods. However, scope extension, i.e. inclusion of more analytes, other matrices and/or minor changes in extraction procedures, can be achieved without a full validation protocol, which requires time and is laborious to the laboratory. This paper presents a simple and rugged protocol for validation in the case of extension of scope. Based on a previously reported method for analysis of sulfonamide residues using LC-MS/MS, inclusion of more analytes, metabolites, matrices and optimisation for the extraction procedure are presented in detail. Initially, the method was applied only to liver samples. In this work, milk, eggs and feed were also added to the scope. Several case-specific validation protocols are proposed for extension of scope. © 2014 Taylor & Francis.


Rubensam G.,Laboratorio Nacional Agropecuario LANAGRO RS | Barreto F.,Laboratorio Nacional Agropecuario LANAGRO RS | Hoff R.B.,Laboratorio Nacional Agropecuario LANAGRO RS | Hoff R.B.,Federal University of Rio Grande do Sul | Pizzolato T.M.,Federal University of Rio Grande do Sul
Food Control | Year: 2013

A simple and inexpensive sample preparation method based on solvent extraction, followed by low temperature cleanup, was demonstrated to be applicable for the determination of avermectin and milbemycin residues in bovine muscle by liquid chromatography-tandem mass spectrometry (LC-MS/MS) and liquid chromatography with fluorescence (LC-FL) detection. The analytical methodology was validated according to the Commission Decision 2002/657/EC, using LC-MS/MS for confirmatory and LC-FL for quantitative purposes. Mean recovery was between 88.9 and 100.7% in three distinct concentrations. The coefficient of variation for repeatability and within-laboratory reproducibility ranged from 0.78 to 5.1% and from 0.28 to 9.0%, respectively. Method precision led to satisfactory values of decision limits (CCα) and detection capabilities (CCβ). The proposed method has been applied in the Brazilian National Residue Control Plan since 2010 for the determination of avermectins and milbemycin residues in bovine muscle samples. A total of 760 samples were analyzed and none of them presented residues at concentrations above the permitted levels established by the more recently applied directives. © 2012 Elsevier Ltd.


Rubensam G.,Federal University of Rio Grande do Sul | Rubensam G.,Laboratorio Nacional Agropecuario LANAGRO RS | Barreto F.,Laboratorio Nacional Agropecuario LANAGRO RS | Hoff R.B.,Laboratorio Nacional Agropecuario LANAGRO RS | And 2 more authors.
Analytica Chimica Acta | Year: 2011

In this work a method is proposed and demonstrated for the analysis of the macrocyclic lactones abamectin, doramectin, eprinomectin, ivermectin and moxidectin in bovine milk by liquid chromatography coupled to mass spectrometry (LC-MS/MS) and liquid chromatography with fluorescence detection (LC-FL). The method is based on liquid-liquid extraction followed by a low temperature purification (LLE-LTP) step. Moreover, the proposed method was validated according to the Commission Decision 2002/657/EC, using LC-MS/MS and LC-FL for confirmatory and quantitative analysis, respectively. For LC-MS/MS the recovery rates observed ranged from 101.2 to 141.6% with coefficient of variation from 2.6 to 19.8%. For LC-FL the recovery rates observed ranged from 100.2 to 105% and coefficient of variations from 2.9 to 8.8%. Matrix effects were negligible due to the low temperature purification step. The quantification limits were far below the maximum limits established by regulations of all countries consulted. The proposed method proved to be simple, easy, and adequate for high-throughput analysis of a large number of samples per day at low cost. © 2011 Elsevier B.V.


PubMed | Laboratorio Nacional Agropecuario LANAGRO RS and Federal University of Rio Grande do Sul
Type: Journal Article | Journal: Food additives & contaminants. Part A, Chemistry, analysis, control, exposure & risk assessment | Year: 2016

A reliable and simple method for the detection and quantification of residues of 14 non-steroidal anti-inflammatory drugs and a metamizole metabolite in swine muscle was developed using liquid chromatography-electrospray ionisation-tandem mass spectrometry (LC-ESI-MS/MS). The samples were extracted with acetonitrile (ACN) in solid-liquid extraction followed by a low-temperature partitioning (LLE-LTP) process at -202C. After evaporation to dryness, the residue was reconstituted with hexane and a mixture of water:acetonitrile (1:1). LC separation was achieved on a reversed-phase (RP18) column with gradient elution using water (phase A) and ACN (phase B) both containing 1mmoll(-)(1) ammonium acetate (NH4COO) with 0.025% acetic acid. Analysis was carried out on a triple-quadrupole tandem mass spectrometer (LC-MS/MS) in multiple reaction monitoring mode using an electrospray interface in negative and positive mode in a single run. Method validation was performed according to the criteria of Commission Decision No. 2002/657/EC. The matrix effect and linearity were evaluated. Decision limit (CC), detection capability (CC), accuracy and repeatability of the method are also reported. The proposed method proved to be simple, easy and adequate for high-throughput analysis and was applied to routine analysis by the Brazilian Ministry of Agriculture, Livestock and Food Supply.


PubMed | Laboratorio Nacional Agropecuario LANAGRO RS and Federal University of Rio Grande do Sul
Type: | Journal: Journal of chromatography. A | Year: 2016

A simple, rapid and sensitive method for confirmatory and quantitative purposes using liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI-MS/MS) was developed and validated for determination of chloramphenicol, thiamphenicol, florfenicol and its metabolite, florfenicol amine, in poultry, swine, bovine and fish muscle. Sample preparation was based on extraction with organic solvent (ethyl acetate: ammonium hydroxide, 98:2) followed by evaporation and fat removal using hexane. The chromatographic separation was carried out with an XTerra C18 column with a gradient elution using water and acetonitrile both with 2mM of ammonium acetate. Mass spectrometry with electrospray ionization was operated in positive or negative polarity using selected-reaction monitoring (SRM) analysis mode, achieving the requirements of four identification points for each compound. Chloramphenicol-D5 was added as internal standard. Method validation was performed according to the criteria of Commission Decision 2002/657/EC. Parameters as precision, reproducibility, trueness, CC and CC were determined. Trueness values were within the range 82-108% and 84-111% for bovine and fish, respectively. Precision ranged from 1.1% to 10.1% and within-laboratory reproducibility ranged from 4.3 to 18.1%, depending on matrix. The CC and CC for bovine muscle, for instance, were established as 0.06 and 0.11gkg(-1), respectively. The method was successfully applied for several interlaboratory proficiency testing programs, achieving 100% of satisfactory results.

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