Development and validation of confirmatory LC–MS/MS method for multi-residue analysis of antibiotic drugs in bovine milk

Abstract

A confirmatory multi-class LC-MS/MS method have been developed for simultaneous determination of 23 antibiotic drugs from seven different classes in bovine milk. The method was validated in accordance with the criteria prescribed in Commission Decision 2002/657/EC. The linear regression analysis showed good correlation with R2 > 0.9800. LOD are in the range of 0.17-6.94 ng/ml, while the LOQ are in the range of 0.50-22.71 ng/ml. The CCα range from 4.43 to 122.33 ng/mL and CCβ was from 4.88 to 139.78 ng/mL. The recovery of the method ranged from 71.96 to 108.70%. The coefficient of variation for repeatability varied from 1.08 to 20.28% and the coefficient of reproducibility varied from 3.14 to 22.88%. In the present study, 189 bovine milk samples were collected from dairy farms and analyzed using confirmatory multi-class LC-MS/MS method. A total of 14 (7.41%) samples were found positive for antibiotics and sulfonamides. The concentrations of the residues were below the maximum levels established by EU.

A Universal LC-MS/MS Method for Simultaneous Detection of Antibiotic Residues in Animal and Environmental Samples

“…Different antibiotics have different chemical properties, and they may require different extraction and detection methods [ 19 , 20 ]. In our study, we used a single extraction and detection protocol to cover 30 antibiotics from 13 families, which makes it an improvement over existing methodologies in terms of efficiency and convenience [ 7 , 9 , 13 , 14 , 15 ]. To provide an insight into why we could make the aforementioned two improvements in detecting antibiotic residues, we provide an interpretation of the results after SPE and chemical extraction were conducted in our protocol.…”

“…In antibiotic residue testing, most of the fundamental laboratory detection methods involve an initial extraction followed by liquid chromatography tandem mass spectrometry (LC-MS/MS) (Figure 1). Although the fine details of the methodology differ between different studies, this fundamental approach has been used to detect the chemical composition of and antibiotic residues in different samples, including porcine muscle [6], duck meat [7], aquaculture products [8], bovine milk [9], milk [10], honey [11], natural water [12,13], swine manure [14], and distiller grains [15]. However, the common limitations of antibiotic residue testing in these studies are the lack of proven applicability of the testing protocol to detect different sample types and the wide number of antibiotic classes used in human and animals.…”

Contaminants in the cow's milk we consume? Pasteurization and other technologies in the elimination of contaminants

“…196 According to the literature, the presence of antibiotics in milk has been evidenced, highlighting tetracycline, oxytetracycline, penicillin, and amoxicillin. 103,124,197,198 While other antibiotics less reported in milk were rifamixin, gatifloxacin, spiramycin, and lomeflaxacin, with no indication in the studies of the purpose of their application in cattle. 101,112,126,127 The consumption of contaminated milk with antibiotic residues is an emerging public health problem worldwide.…”

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

“…Liquid chromatography tandem mass spectrometry (LC-MS/MS) is the most appropriate technique available today for the analysis of a wide range of antibiotics in food, including milk [ 21 , 22 , 23 , 24 , 25 ]. Furthermore, the use of HRMS instrumentation, operating in full-scan acquisition mode to an accurate mass, offers even greater possibilities for multiresidue analysis of antibiotics, as well as for the identification of unknown compounds using non-target analysis.…”

“…Furthermore, the use of HRMS instrumentation, operating in full-scan acquisition mode to an accurate mass, offers even greater possibilities for multiresidue analysis of antibiotics, as well as for the identification of unknown compounds using non-target analysis. However, these methods were mainly developed to quantify drug residues in bovine milk [ 21 , 22 , 23 , 24 , 25 ], very few analytical procedures are available for sheep and goat milk. In some regions, sheep and goat milk have a considerable production, distribution, consumption, and use, especially for typical products of the supply chain, such as pecorino romano.…”