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Validation of a method for sedatives and β-blockers determination in swine, bovine and equine kidney using liquid chromatography coupled with tandem mass spectrometry.

Abstract: A method for the determination of five sedatives and 14 β-blocker residues in swine, bovine and equine kidney was validated. Samples were extracted with acetonitrile and purified using dispersive solid phase extraction (d-SPE) with Celite 545 with subsequent analysis by LC-MS/MS. A simplified protocol was applied to validate the method scope extension to include new matrices. Parameters such as recovery, trueness, linearity (r), relative standard deviation (RSD), decision limit (CCα) and method capability (CCβ) were measured for the bovine and equine kidney matrices. The method was applied to the analysis of more than 300 real samples and is currently included in the Brazilian National Residue Control Plan.
Publication Date: 2016-11-21 PubMed ID: 27869552DOI: 10.1080/19440049.2016.1252468Google Scholar: Lookup
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  • Journal Article
  • Validation Study

Summary

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This research aims to validate a method for determining residues of sedatives and ß-blocker drugs in swine, bovine, and equine kidney samples. These residues were identified and quantified through a procedure that involved extraction with acetonitrile, purification using dispersive solid phase extraction, and analysis through liquid chromatography and mass spectrometry.

Introduction

  • The research study focused on confirming the effectiveness and reliability of a method for identifying the presence of residues of specific sedatives and ß-blocker drugs in animal kidneys. This method is crucial in ensuring the safety of meat products.
  • The study aimed to understand if this method could be reliably used with different animal kidney samples, including those from pigs, cattle, and horses.

Method

  • The method being validated involved extracting potential drug residues from kidney samples using acetonitrile, a solvent effective in breaking down complex molecules.
  • After extraction, the sample was purified using dispersive solid phase extraction (d-SPE) with Celite 545. This step helps to isolate and identify the drug residues from other organic compounds.
  • The final analysis was done through liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS), a powerful tool in identifying and quantifying specific organic compounds.

Validation and Results

  • This method was validated by considering several parameters such as recovery (how much of the original compound can be retrieved after processing), trueness (accuracy of the final results), linearity (consistency of results over a range of measurements), standard deviation (how much variability in the results), decision limit (the minimum concentration level that can be detected), and method capability (how well the method performs).
  • The method was validated using over 300 real animal kidney samples and received positive results that support its reliability and effectiveness.
  • The validation process and results have led to this method being included in the Brazilian National Residue Control Plan, indicating its acceptance as a standard practice in ensuring the safety of the meat industry.

Cite This Article

APA
de Oliveira LG, Barreto F, Hoff R, Rübensam G, Scherer Kurz MH, Galle G, Gonçalves FF. (2016). Validation of a method for sedatives and β-blockers determination in swine, bovine and equine kidney using liquid chromatography coupled with tandem mass spectrometry. Food Addit Contam Part A Chem Anal Control Expo Risk Assess, 34(1), 32-39. https://doi.org/10.1080/19440049.2016.1252468

Publication

ISSN: 1944-0057
NlmUniqueID: 101485040
Country: England
Language: English
Volume: 34
Issue: 1
Pages: 32-39

Researcher Affiliations

de Oliveira, Lenise Guimarães
  • a Escola de Química e Alimentos , Universidade Federal do Rio Grande - FURG, Rua Barão do Caí , 125 Santo Antônio da Patrulha , Brazil.
Barreto, Fabiano
  • b Laboratório Nacional Agropecuário - LANAGRO/RS , Ministério da Agricultura, Pecuária e Abastecimento , Porto Alegre , Brazil.
Hoff, Rodrigo
  • b Laboratório Nacional Agropecuário - LANAGRO/RS , Ministério da Agricultura, Pecuária e Abastecimento , Porto Alegre , Brazil.
Rübensam, Gabriel
  • b Laboratório Nacional Agropecuário - LANAGRO/RS , Ministério da Agricultura, Pecuária e Abastecimento , Porto Alegre , Brazil.
Scherer Kurz, Marcia Helena
  • a Escola de Química e Alimentos , Universidade Federal do Rio Grande - FURG, Rua Barão do Caí , 125 Santo Antônio da Patrulha , Brazil.
Galle, Gabriela
  • a Escola de Química e Alimentos , Universidade Federal do Rio Grande - FURG, Rua Barão do Caí , 125 Santo Antônio da Patrulha , Brazil.
Gonçalves, Fábio Ferreira
  • a Escola de Química e Alimentos , Universidade Federal do Rio Grande - FURG, Rua Barão do Caí , 125 Santo Antônio da Patrulha , Brazil.

MeSH Terms

  • Adrenergic beta-Antagonists / metabolism
  • Animals
  • Cattle
  • Chromatography, Liquid / methods
  • Horses
  • Hypnotics and Sedatives / metabolism
  • Kidney / metabolism
  • Swine
  • Tandem Mass Spectrometry / methods

Citations

This article has been cited 3 times.
  1. Kośka I, Kubalczyk P, Cichomski M, Kisielewska A. The Use of Extraction on C18-Silica-Modified Magnetic Nanoparticles for the Determination of Ciprofloxacin and Ofloxacin in Meat Tissues.. Molecules 2023 Aug 18;28(16).
    doi: 10.3390/molecules28166123pubmed: 37630375google scholar: lookup
  2. Kośka I, Kubalczyk P. Development of the Chromatographic Method for Simultaneous Determination of Azaperone and Azaperol in Animal Kidneys and Livers.. Int J Mol Sci 2022 Dec 21;24(1).
    doi: 10.3390/ijms24010100pubmed: 36613536google scholar: lookup
  3. Chen L, Hu X, Xing Y, Sun Y, Hu M, Zhang G. Highly sensitive immunochromatographic assay for simultaneous determination of azaperone and azaperol in pork.. Food Chem X 2023 Mar 30;17:100525.
    doi: 10.1016/j.fochx.2022.100525pubmed: 36478711google scholar: lookup