Clavulanic acid is a molecule with antimicrobial effect used in several livestock species treatment. Its inclusion in the treatment of infectious diseases of broilers requires determination of pharmacokinetic and pharmacodynamic parameters in order to determine the appropriate dosage for broilers and ensure safety of chicken products for human health. The present study describes the optimisation of analytical LC-MS/MS method for identification and quantification of clavulanic acid in broiler chicken plasma and meat. The limit of detection and the limit of quantification for the developed method were 3.09 μg·L-1 and 10.21 μg·L-1 for plasma and 2.57 μg·kg-1 and 8.47 μg·kg-1 for meat. The recoveries of the developed plasma and tissue extraction procedure were > 105.7% and > 95.6%, respectively. The achieved coefficient of variation of within-run precision ranged from 2.8 to 10.9% for plasma and from 6.5 to 8.5% for meat. The pharmacokinetic experiment was performed in 112 Ross broiler chickens assigned into time interval groups ranging from 10 min to 24 h in accredited animal facilities. Administered dose of clavulanic acid was 2.5 mg·kg-1 according to the manufacturer's recommendations. The pharmacokinetic parameters obtained from the experiment are as follows: Cmax = 1.82 ± 0.91 mg·L-1, Tmax = 0.25 h, T1/2 = 0.87 h, Kel = 0.80 ± 0.04 h-1, AUC0-∞ = 2.17 mg·h ·L-1.

• Keywords
• Antibiotics, Clavulanic acid, Pharmacokinetics, Tandem mass spectrometry,
• MeSH
• Mass Spectrometry methods   MeSH
• beta-Lactamase Inhibitors blood   metabolism   pharmacokinetics   MeSH
• Chickens MeSH
• Clavulanic Acid blood   metabolism   pharmacokinetics   MeSH
• Limit of Detection MeSH
• Reference Standards MeSH
• Reproducibility of Results MeSH
• Chromatography, High Pressure Liquid methods   MeSH
• Animals MeSH
• Check Tag
• Animals MeSH
• Publication type
• Journal Article MeSH
• Names of Substances
• beta-Lactamase Inhibitors MeSH
• Clavulanic Acid MeSH

The use of anabolic steroid hormones as growth promoters in feed for farm animals has been banned in the European Union since 1988 on the basis of Council Directive 96/22/EC. However, there is still ongoing monitoring and reporting of positive findings of these banned substances in EU countries. The aim of this work was to investigate the efficacy and discriminatory ability of metabolic fingerprinting after the administration of 17β-testosterone esters to pigs. Plasma and urine samples were chromatographically separated on a Hypersil Gold C18 column. High resolution mass spectrometry metabolomic fingerprints were analysed on a hybrid mass spectrometer Q-Exactive. Three independent multivariate statistical methods, namely principal component analysis, clustre analysis, and orthogonal partial least squares discriminant analysis showed significant differences between the treated and control groups of pigs even 14 days after the administration of the hormonal drug. Plasma samples were also analysed by a conventional quantitative analysis using liquid chromatography with tandem mass spectrometry and a pharmacokinetic curve was constructed based on the results. In this case, no testosterone residue was detected 14 days after the administration. The results clearly showed that a metabolomics approach can be a useful and effective tool for the detection and monitoring of banned anabolic steroids used illegally in pig fattening.

• Keywords
• anabolic practices, metabolomic, pigs, plasma, testosterone, urine,
• Publication type
• Journal Article MeSH

Liquid chromatography (LC) coupled with mass spectrometry (MS) is widely used for the determination of mycotoxins in cereals and cereal-based products. In addition to the regulated mycotoxins, for which official control is required, LC-MS is often used for the screening of a large range of mycotoxins and/or for the identification and characterization of novel metabolites. This review provides insight into the LC-MS methods used for the determination of co-occurring mycotoxins with special emphasis on multiple-analyte applications. The first part of the review is focused on targeted LC-MS approaches using cleanup methods such as solid-phase extraction and immunoaffinity chromatography, as well as on methods based on minimum cleanup (quick, easy, cheap, effective, rugged, and safe; QuEChERS) and dilute and shoot. The second part of the review deals with the untargeted determination of mycotoxins by LC coupled with high-resolution MS, which includes also metabolomics techniques to study the fate of mycotoxins in plants.

• Keywords
• Fungal secondary metabolites, Liquid chromatography–high-resolution mass spectrometry, Liquid chromatography–tandem mass spectrometry, Metabolomics, Validation,
• MeSH
• Food Analysis methods   MeSH
• Chromatography, Affinity methods   MeSH
• Solid Phase Extraction methods   MeSH
• Fungi isolation & purification   metabolism   MeSH
• Edible Grain chemistry   metabolism   microbiology   MeSH
• Metabolomics methods   MeSH
• Mycotoxins analysis   metabolism   MeSH
• Tandem Mass Spectrometry methods   MeSH
• Chromatography, High Pressure Liquid methods   MeSH
• Publication type
• Journal Article MeSH
• Review MeSH
• Names of Substances
• Mycotoxins MeSH