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United States Department of Agriculture

Agricultural Research Service

Title: A dual validation approach to detect anthelmintic residues in bovine liver over an extended concentration range)

item Kinsella, Brian
item Whelan, Michelle
item Cantwell, Helen
item Mccormack, Martin
item Furey, Ambrose
item Lehotay, Steven
item Danaher, Martin

Submitted to: Talanta
Publication Type: Peer Reviewed Journal
Publication Acceptance Date: 8/17/2010
Publication Date: 11/1/2010
Citation: Kinsella, B., Whelan, M., Cantwell, H., Mccormack, M., Furey, A., Lehotay, S.J., Danaher, M. 2010. A dual validation approach to detect anthelmintic residues in bovine liver over an extended concentration range. Talanta. 83:14-24.

Interpretive Summary: The analysis of veterinary drug residues in animal-derived foods is an important function of regulatory bodies worldwide to ensure the proper usage of the chemicals by producers and to help ensure food safety. Currently, inefficient analytical monitoring methods are used by many regulatory agencies, which need updated using more efficient and effective modern approaches. In the case of worm controlling agents, known as anthelmintics, the previous analytical methods required multiple analyses to cover all 38 of them for monitoring purposes. This research demonstrated that a previous method could be extended to an additional matrix (beef liver) over a wide concentration range, which occurs in real-world practice. The fast and convenient method was validated thoroughly to demonstrate its satisfactory performance in regulatory applications. It is already being routinely used by regulatory laboratories in Ireland, and it will be transferred to U.S. monitoring labs in the near future.

Technical Abstract: This paper describes a method for the detection and quantification of 38 of the most widely used anthelmintics (including benzimidazoles, macrocyclic lactones and flukicides) in bovine liver at MRL and non-MRL level. A dual validation approach was adapted to reliably detect anthelmintic residues over an extended concentration range (1-3000 ug/kg). Sample extraction and purification was carried out using a modified QuEChERS method. A concentration step was included when analysing in the low ug/kg range. Rapid analysis was carried out by ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS), which was capable of detecting residues to <2 ug/kg. The method has been single-laboratory validated according to the 2002/657/EC guidelines and met acceptability criteria in all but a few cases. The inclusion of 19 internal standards, including 15 isotopically labelled internal standards, improved accuracy, precision, decision limit (CCa) and detection capability (CC beta).

Last Modified: 05/27/2017
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