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

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Abstract

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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Acknowledgments

Financial supports from CAPES, CNPq, and FACEPE are gratefully acknowledgement. The authors are grateful to Professor Suzana P.V. Nova (UAG-UFRPE) and Professor Lilian S.S. de Andrade (UFRPE) for help in collecting and sending milk samples and for suggestions ans to Severino Granjeiro Junior (LAFEPE), Rogério Ferreira da Silva (UFPE), and Edén Cavalcanti de Albuquerque Júnior (ITEP) for technical support.

Conflict of Interest

Sueny Kêlia Barbosa Freitas declares that she has no conflict of interest. Ana Paula Silveira Paim declares that she has no conflict of interest. Paula Tereza de Souza e Silva declares that she has no conflict of interest. This article does not contain any studies with human or animal subjects.

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Authors and Affiliations

  1. Universidade Federal de Pernambuco, Centro de Ciências Exatas e da Natureza, Departamento de Química Fundamental, Av. Jornalista Aníbal Freire, s/n—Cidade Universitária, 50740-560, Recife, Pernambuco, Brazil

    Sueny Kêlia Barbosa Freitas & Ana Paula Silveira Paim

  2. Empresa Brasileira de Pesquisa Agropecuária, EMBRAPA Semiárido, BR 428, Km 152, Zona Rural, 56302-970, Petrolina, Pernambuco, Brazil

    Paula Tereza de Souza e Silva

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  1. Sueny Kêlia Barbosa Freitas
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  2. Ana Paula Silveira Paim
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  3. Paula Tereza de Souza e Silva
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Correspondence to Ana Paula Silveira Paim.

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Freitas, S.K.B., Paim, A.P.S. & de Souza e Silva, P.T. Development of a LC-IT-TOF MS Procedure to Quantify Veterinary Drug Residues in Milk Employing a QuEChERS Approach. Food Anal. Methods 7, 39–46 (2014). https://doi.org/10.1007/s12161-013-9595-7

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  • DOI: https://doi.org/10.1007/s12161-013-9595-7

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