Analytical Approaches in Official Food Safety Control: An LC-Orbitrap-HRMS Screening Method for the Multiresidue Determination of Antibiotics in Cow, Sheep, and Goat Milk

Abstract

The presence of unauthorized substances, such as residues of veterinary medicines or chemical contaminants, in food can represent a possible health concern. For this reason, a complete legislative framework has been established in the European Union (EU), which defines the maximum limits allowed in food and carries out surveillance programs to control the presence of these substances. Official food control laboratories, in order to ensure a high level of consumer protection, must respond to the challenge of improving and harmonizing the performance of the analytical methods used for the analysis of residues of authorized, unauthorized, or prohibited pharmacologically active substances. Laboratories must also consider the state of the art of the analytical methodologies and the performance requirements of current legislation. The aim of this work was to develop a multiresidue method for the determination of antibiotics in milk, compliant with the criteria and procedures established by Commission Implementing Regulation (EU) 2021/808. The method uses an LC-Orbitrap-HRMS for the determination of 57 molecules of antibiotic and active antibacterial substances belonging to different chemical classes (beta-lactams, tetracyclines, sulfonamides, quinolones, pleuromutilins, macrolides, and lincosamides) in bovine, ovine, and goat milk samples. It provides a simple and quick sample pretreatment and a subsequent identification phase of analytes, at concentrations equal to or lower than the maximum residual limit (MRL), in compliance with Commission Regulation (EU) 2010/37. The validation parameters: selectivity, stability, applicability, and detection capability (ccβ), are in agreement with the requirements of Commission Implementing Regulation (EU) 2021/808 and demonstrated the effectiveness of the method in detecting veterinary drug residues at the target screening concentration (at the MRL level or below), with a false positive rate of less than 5%. This method represents an effective solution for detecting antibiotics in milk, which can be successfully applied in routine analyses for official food control plans.

Colloidal Gold Immunochromatography and ELISA Traceability of Tetracycline Residues from Raw Milk to its Dairy Products

“…Antibiotic residues in milk represent a major public health concern. This research indicates that more than 40% of samples from household farmers exceeded the allowed TC amount (100 μg/kg), as has also been reported in other regions of the world including Italy (8), Poland (6), Serbia (44), or Iran (31). Inadequacies in the vaccination strategy may lead to the introduction of infectious diseases into herds of cattle, necessitating the administration of antibiotics.…”

“…Therefore, research in milk industry is an important current topic with many and various directions. The most recent scientific directions include: technological solutions for milk processing (1), food-monitoring technologies (2), sensors for antibiotic detection (3) or environmental monitoring (4,5), evaluation of bacterial diversity (6), developing methods for the determination of antibiotics in milk (7,8), food security (9), impact on the human health (10).…”