Total determination of triclabendazole and its metabolites in bovine tissues using liquid chromatography-tandem mass spectrometry.
J Chromatogr B Analyt Technol Biomed Life Sci
; 1109: 54-59, 2019 Mar 01.
Article
de En
| MEDLINE
| ID: mdl-30721796
ABSTRACT
A reliable LC-MS/MS analytical method for the determination of residual triclabendazole and its principal metabolites (triclabendazole sulfoxide, triclabendazole sulfone and keto-triclabendazole) in bovine tissues was developed, in which triclabendazole and its metabolites are oxidized to keto-triclabendazole as a marker residue. The method involves sample digestion with hot sodium hydroxide, thus releasing the bound residues of various triclabendazole metabolites in bovine tissues. The target compounds are extracted from the digest mixture with ethyl acetate, defatted by liquid-liquid partitioning using n-hexane and acetonitrile, then oxidized with hydrogen peroxide in a mixture of ethanol and acetic acid. The reaction mixture is cleaned up using a strong cation exchange cartridge (Oasis MCX) and the analytes are quantified using LC-MS/MS. The optimal conditions for the complete oxidation of triclabendazole and its metabolites to keto-triclabendazole are an incubation time of 16â¯h and a temperature of 90⯰C. The developed method was evaluated using three bovine samples muscle, fat, and liver. Samples were spiked with triclabendazole and its principal metabolites at 0.01â¯mg/kg and at the Japanese Maximum Residue Limits (MRLs) established for each sample. The validation results show excellent recoveries (81-102%) and precision (<10%) for all target compounds. The limit of quantification (S/Nâ¯≥â¯10) of the developed method is 0.01â¯mg/kg. These results suggest the developed method is applicable to quantifying residual triclabendazole in bovine tissues in compliance with the MRLs established by the Codex Alimentarius and EU and Japanese regulations, and thus the proposed method will be a useful tool for the regulatory monitoring of residual triclabendazole and its metabolites.
Mots clés
Texte intégral:
1
Collection:
01-internacional
Base de données:
MEDLINE
Sujet principal:
Sulfoxydes
/
Résidus de médicaments
/
Chromatographie en phase liquide
/
Spectrométrie de masse en tandem
/
Triclabendazole
Type d'étude:
Diagnostic_studies
/
Prognostic_studies
Limites:
Animals
Langue:
En
Journal:
J Chromatogr B Analyt Technol Biomed Life Sci
Sujet du journal:
ENGENHARIA BIOMEDICA
Année:
2019
Type de document:
Article