Development of a multi-class method for the identification and quantification of residues of antibiotics, coccidiostats and corticosteroids in milk by liquid chromatography–tandem mass spectrometry

Nebot, Carolina; Iglesias, A.; Regal, Patricia; Miranda, José M.; Cepeda, Alberto; Fente, C.

doi:10.1016/j.idairyj.2011.09.001

Cited by 40 publications

(13 citation statements)

References 36 publications

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“…14 Também na Espanha, foram analisadas 100 amostras de leite cru de fazenda e 15 amostras de leite do comércio utilizando ELL com acetonitrila e clean up com cartucho Strata TM -X. 48 Apenas uma amostra apresentou resultado positivo, para decoquinato, um coccidioestático, na concentração de 1 ng/mL. Resíduos de lincomicina foram encontrados em 16 das 17 amostras de leite analisadas por UPLC-MS/ MS em Taiwan, todas com resíduos abaixo do LMR (150 ng/mL).…”

Section: Outros Paísesunclassified

Resíduos de medicamentos veterinários em leite e ovos

Pacheco-Silva¹,

Souza²,

Caldas³

2014

Quím. Nova

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VETERINARY DRUG RESIDUES IN MILK AND EGGS. The use of veterinary drugs in food producing animals may result in the presence of residues in foods, including milk and eggs. Immunoassay or microbiological tests are used to screen for residues, but chromatographic methods are needed to confirm positive results. In most methods, the sample is extracted with acetonitrile, submitted to clean up or directly analyzed by LC-MS/MS. Results of the Brazilian governmental monitoring programs from 2006 to 2011 have shown that the antiparasitic ivermectin was the drug most frequently found in milk. Residues in eggs are only monitored by one of the programs, and few studies have reported the incidence of veterinary drugs in this matrix in Brazil.Keywords: veterinary drugs; milk; eggs. INTRODUÇÃOMedicamentos são usados na medicina veterinária no tratamento e prevenção de doenças ou como promotores de crescimento. 1,2 Estes compostos compreendem uma variedade de classes químicas com ações terapêuticas diversas, incluindo antibiótica/antimicrobiana, antiparasitária, inseticida, fungicida e sedativa. 3 Os antimicrobianos (b-lactâmicos, aminoglicosídeos e tetraciclinas) e os antiparasitários (avermectinas, piretróides e organofosforados) são os produtos mais comercializados no Paraná para tratamento do rebanho leiteiro. 4 O uso de medicamentos veterinários em animais produtores de alimentos pode deixar resíduos nos alimentos, como carne, leite e ovos, cujos níveis não devem ultrapassar o Limite Máximo de Resíduos (LMR). O LMR é a concentração máxima de resíduo em um alimento de origem animal resultante do uso de um medicamento veterinário (expresso em mg/kg ou µg/kg, em peso fresco) que é recomendado para ser legalmente permitido ou reconhecido como sendo aceitável no alimento. 5 Estes limites são estabelecidos para garantir o uso adequado destes produtos, limitar a exposição e proteger a saúde dos consumidores dos alimentos provenientes de animais tratados. 5 A presença de resíduos em um alimento acima do LMR estabelecido indica que o produto não foi utilizado segundo as boas práticas de uso de medicamentos veterinários (BPMV), ou o uso de um produto não autorizado. 6 O Brasil não estabelece LMR para medicamentos veterinários, adotando aqueles recomendados pelo Mercosul, Codex Alimentarius, União Européia ou Estados Unidos. 7 A exposição humana a resíduos de medicamentos veterinários presentes nos alimentos pode causar efeitos adversos, incluindo reações alérgicas em indivíduos hipersensíveis 8 e câncer. 9,10 Adicionalmente, a exposição a antimicrobianos/antibióticos pode provocar o desenvolvimento de microrganismos resistentes, que dificulta a ação terapêutica destes medicamentos em indivíduos que consumiram alimentos de animais tratados. 11,12 Resíduos de medicamentos veterinários no leite podem também causar problemas tecnológicos nos processos de fermentação dos laticínios. 13,14 No Brasil, há dois programas nacionais que monitoram a presença de resíduos de medicamentos veterinários em produtos de origem animal. O Plano Nacional...

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Section: Outros Paísesunclassified

Resíduos de medicamentos veterinários em leite e ovos

Pacheco-Silva¹,

Souza²,

Caldas³

2014

Quím. Nova

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“…The research group has developed, validated, and published various methods for the analysis of trace levels of veterinary drugs (coccidiostats, sulfonamides, and other antibiotics) in animal food and feed samples [32,33,34,35]. Validation for this type of sample and the matrix has typically been conducted following the European guideline (Decision 2002/657/EC) [10], which permits method implementation and comparisons in EU reference laboratories.…”

Section: Resultsmentioning

confidence: 99%

Determination of Florfenicol, Thiamfenicol and Chloramfenicol at Trace Levels in Animal Feed by HPLC–MS/MS

et al. 2019

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Administration of florfenicol and thiamfenicol through medicated feed is permitted within the European Union, always following veterinary prescription and respecting the withdrawal periods. However, the presence of low levels of florfenicol, thiamfenicol, and chloramfenicol in non-target feed is prohibited. Since cross-contamination can occur during the production of medicated feed and according to Annex II of the European Regulation 2019/4/EC, the control of residue levels of florfenicol and thiamfenicol in non-target feed should be monitored and avoided. Based on all the above, a sensitive and reliable method using liquid chromatography tandem mass spectrometry was developed for the simultaneous detection of chloramfenicol, florfenicol, and thiamfenicol at trace levels in animal feed. Analytes were extracted from minced feed with ethyl acetate. Then, the ethyl acetate was evaporated, the residue was resuspended in Milli-Q water and the extract filtered. The method was in-house validated at carryover levels, with concentration ranging from 100 to 1000 µg/kg. The validation was conducted following the European Commission Decision 2002/657/EC and all performance characteristics were successfully satisfied. The capability of the method to detect amfenicols at lower levels than any prior perspective regulation literature guarantees its applicability in official control activities. The developed method has been applied to non-compliant feed samples with satisfactory results.

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“…Although various analytical methods have been reported to detect and quantify antibiotics in milk (Mamani et al 2009;Gamba et al 2009;Rønning et al 2006;Kinsella et al 2009;Van Holthoon et al 2010;Santos et al 2007;Stolker et al 2008;Ortelli et al 2009;Nebot et al 2012), none of them have reported on the use of the QuEChERS method to extract milk for the detection and quantification of the particular antibiotics used in the present study.…”

Section: Introductionmentioning

confidence: 82%

Development of a LC-IT-TOF MS Procedure to Quantify Veterinary Drug Residues in Milk Employing a QuEChERS Approach

2013

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A sensitive liquid chromatography coupled to high-resolution tandem mass spectrometry (LC-IT-TOF MS) with electrospray ionization method for the identification and quantification of five antibiotic residues in milk has been developed. For sample preparation, a simple modification of the QuEChERS method was used with further sample cleanup using dispersive solid phase extraction according to AOAC official standards 2007.01. The method yielded acceptable accuracy values for each drug at each level, with mean recoveries (n=3) ranging from 83 to 92 %. The recovery of antibiotics of the intra-assay ranged from 85 to 95 % (RSD<9 %) and the inter-assay from 84 to 95 % (RSD<11 %). A total of 31 milk samples, either pasteurized or fresh whole milk, were analyzed following the method. Amoxicillin and oxytetracycline (two of the pasteurized milk samples), ampicillin and amoxicillin (3 of 25 fresh milk samples), and tetracycline and oxytetracycline (two other fresh milk samples out of 25) were detected at levels below the current Brazilian maximum residue levels.

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Development of a multi-class method for the identification and quantification of residues of antibiotics, coccidiostats and corticosteroids in milk by liquid chromatography–tandem mass spectrometry

Cited by 40 publications

References 36 publications

Resíduos de medicamentos veterinários em leite e ovos

Resíduos de medicamentos veterinários em leite e ovos

Determination of Florfenicol, Thiamfenicol and Chloramfenicol at Trace Levels in Animal Feed by HPLC–MS/MS

Development of a LC-IT-TOF MS Procedure to Quantify Veterinary Drug Residues in Milk Employing a QuEChERS Approach

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