In-house validation for multi-residue analysis of tetracycline in cow milk by HPLC with UV detection

Authors

  • Carolina Kato Prado Universidade Estadual de Maringá
  • Flavio Dias Ferreira Universidade Tecnológica Federal do Paraná
  • Erika Bando Universidade Estadual de Maringá
  • Miguel Machinski Junior Universidade Estadual de Maringá http://orcid.org/0000-0001-5380-9186

DOI:

https://doi.org/10.5433/1679-0359.2017v38n6p3539

Keywords:

In-house validation, Tetracycline residues, High-performance liquid chromatography, Cow milk, Toxicology analysis.

Abstract

The indiscriminate use of antibiotics in dairy cattle without complying with the waiting period results in residual contamination, whose effective control in produced milk requires validated methods toensure analytical results. The aim of this study was to optimize and validate the HPLC-UV/VIS method at 365 nm for analyzingthe tetracycline in pasteurized cow milk in accordance with the European Community (2002/657/EC). Spiked milk with analytes (oxytetracycline, tetracycline, doxycycline, and chlortetracycline) was submitted to deproteinization and cleaning by a C18 solid-phase column and analyzed by HPLC using a gradient system with 0.01 mol L?1 oxalic acid-acetonitrile-triethylamine (90:9.9:0.1) and acetonitrile on a reverse phase (C18) column. Accuracy and precision were assessed by adding analytes to levels of 0.5, 1, and 1.5 times the permissible maximum limit allowed in Brazil. The method presented selectivity with a decision limit (CC?) and detection capability (CC?) ranging from 114.2 to 143.7 and from 129.3 to 188.7 µg kg?1, respectively. The recovery of tetracyclines was higher than 82.5% with a precision of 7.1%, demonstrating theefficiency in determining tetracycline residues in cow milk.

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Author Biographies

Carolina Kato Prado, Universidade Estadual de Maringá

Discente de Pós-Graduação em Ciência de Alimentos, Universidade Estadual de Maringá, UEM, Maringá, PR, Brasil.

Flavio Dias Ferreira, Universidade Tecnológica Federal do Paraná

Prof., Universidade Tecnológica Federal do Paraná, UTFPR, Medianeira, PR, Brasil.

Erika Bando, Universidade Estadual de Maringá

Pesquisadora, UEM, Maringá, PR, Brasil.

Miguel Machinski Junior, Universidade Estadual de Maringá

Prof., UEM, Maringá, PR, Brasil.

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Published

2017-11-23

How to Cite

Prado, C. K., Ferreira, F. D., Bando, E., & Machinski Junior, M. (2017). In-house validation for multi-residue analysis of tetracycline in cow milk by HPLC with UV detection. Semina: Ciências Agrárias, 38(6), 3539–3548. https://doi.org/10.5433/1679-0359.2017v38n6p3539

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