Development, Validation and Application of Isotope Based Chromatographic/Spectrometric Techniques for Mixed Contaminants Including Some Veterinary Drug Residues in Bovine Meat
Date Issued
2019-10-27
Author(s)
Zehra Hajrulai-Musliu
Risto Uzunov
Stefan Jovanov
Elizabeta Dimitrieska-Stojkovikj
Biljana Stojanovska-Dimzoska
Velimir Stojkovski
Abstract
The aim of this study was optimization of solid phase extraction method and optimization and
validation of LC-MS/MS method for detection of β-agonists, antibiotics and organophosphorus
pesticides using isotopically labeled internal standards in bovine meat. In the method were
included total of 30 veterinary drugs from which 10 β-agonists, 15 antibiotics (cephalosporines,
fluoroquinolones, β-lactams and sulfonamides) and 5 organophosphorus pesticides. Also in the
method were included 12 isotopically labeled internal standards.The extraction of the residues
from meat samples is with double extraction with acetonitrile:ethilacetate:acetic acid
(49.5:49.5:1, v/v/v) and after first extraction, the solid phase extraction with Oasis HLB
cartridges was used. For identification and quantification of the residue liquid chromatograph
tandem mass spectrometer was used. With injections of standards of all veterinary drugs
included in this study in MS/MS detector and ESI+ ionization the precursor and product ions
were determined. After optimization of the chromatographic conditions (mobile phase,
gradient) the method was validated. In the validation study were included following validation
parameters: linearity, determination of CCα, CCβ, LOD and LOQ, accuracy and precision
(interday and intraday reproducibility). From total of 30 veterinary drugs with this method were
extracted 22. The results from linearity, accuracy and precision of the method for the extracted
veterinary drugs were in accordance with criteria in the 2002/657/EC and the guidance for
validation of analytical methods. The CCα, CCβ, LOD and LOQ were lower than recommended
concentration of β-agonists and MRL values for antibiotics and pesticides. According of the
results of the validation study, this method can be used in routine analysis of 22 residues in
bovine meat.
validation of LC-MS/MS method for detection of β-agonists, antibiotics and organophosphorus
pesticides using isotopically labeled internal standards in bovine meat. In the method were
included total of 30 veterinary drugs from which 10 β-agonists, 15 antibiotics (cephalosporines,
fluoroquinolones, β-lactams and sulfonamides) and 5 organophosphorus pesticides. Also in the
method were included 12 isotopically labeled internal standards.The extraction of the residues
from meat samples is with double extraction with acetonitrile:ethilacetate:acetic acid
(49.5:49.5:1, v/v/v) and after first extraction, the solid phase extraction with Oasis HLB
cartridges was used. For identification and quantification of the residue liquid chromatograph
tandem mass spectrometer was used. With injections of standards of all veterinary drugs
included in this study in MS/MS detector and ESI+ ionization the precursor and product ions
were determined. After optimization of the chromatographic conditions (mobile phase,
gradient) the method was validated. In the validation study were included following validation
parameters: linearity, determination of CCα, CCβ, LOD and LOQ, accuracy and precision
(interday and intraday reproducibility). From total of 30 veterinary drugs with this method were
extracted 22. The results from linearity, accuracy and precision of the method for the extracted
veterinary drugs were in accordance with criteria in the 2002/657/EC and the guidance for
validation of analytical methods. The CCα, CCβ, LOD and LOQ were lower than recommended
concentration of β-agonists and MRL values for antibiotics and pesticides. According of the
results of the validation study, this method can be used in routine analysis of 22 residues in
bovine meat.
Subjects
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