Multi-residue methodology for quantification of antiparasitics in hen eggs by LC-MS/MS: development, validation and application to 348 samples from Brazil

Abstract

Analytical methodology for quantification of 15 antiparasitic drugs and their respective metabolites in laying hen eggs was optimized and validated. The method uses acetonitrile as solvent extraction, sodium chloride for salting-out, low-temperature purification and analysis by LC-MS/MS. A total of 348 egg samples were collected in 11 states of Brazil and 50% of the total samples presented antiparasitic residues, which were albendazole, fipronil, fenbendazole, ivermectin, oxibendazole and mebendazole. A total of 12.4% of the samples were considered non-compliant, and residues quantified in these samples were albendazole, fipronil, and mebendazole. Albendazole was always identified as albendazole sulfone. Only one sample presented fipronil and fipronil sulfone; all others exclusively the sulfone metabolite. Fenbendazole was characterized by the presence of both metabolites: sulfone and sulfoxide. Maximum limits adopted are based on the Normative Instruction 51/2019 of the Brazilian Health Regulatory Agency (ANVISA), but albendazole, fipronil, oxibendazole, ivermectin, and mebendazole do not have their maximum residue level established. In addition, metabolites of albendazole, fipronil and fenbendazole in eggs are not considered in this Instruction.

Keywords:

• LC-MS/MS
• eggs
• antiparasitic
• residues
• metabolites

Acknowledgments

The Federal Laboratory of Animal and Plant Health and Inspection – LFDA/RS of the Ministry of Agriculture, Livestock and Supply and the Chemistry Institute of the Federal University of Rio Grande do Sul (UFRGS) supported this study.

Author contributions

CT – Methodology, writing original draft, review & editing, project administration; FB – Investigation, writing – review & editing; LB– Methodology, writing – review & editing; LJ – Methodology, writing – review & editing; TMP –Writing – review & editing

Disclosure statement

The authors declare no competing financial interest.