LC-HRMS analysis of 13 classes of pharmaceutical substances in food supplements.

Food supplements should not contain substances considered unsafe or pose a health risk to consumers. In recent years illegal adulterants have been found in various functional foods without notification of their presence or amount in the labelling. In this study, a validated method was developed and applied as a screening method to detect 124 forbidden substances belonging to 13 classes of compounds in food supplements. Liquid chromatography coupled with high-resolution mass spectrometry (LC-HRMS) and a simple and rapid extraction protocol was applied to 110 food supplements collected from the internet market or during official controls in Italy. The percentage of non-compliant samples was 4.5%, relatively high compared with the official control results for these substances usually obtained on other food matrices. The results suggested the need to strengthen controls in this field to detect food supplement adulteration, which represents a potential health risk for the consumer.

Analysis of beta-agonist residues in bovine hair: Development of a UPLC-MS/MS method and stability study.

Beta-sympathomimetic compounds are widely used in therapy because of the bronchodilator, smooth muscle-relaxant and tocolytic properties. However, their growth promoting and performance enhancing effects are often subject to illegal use. The present work describes the development of a fast and reliable analytical multiresidue method for the confirmation 20 ß-agonist compounds in animal hair. The procedure is based on alkaline digestion, LLE with organic solvents, SPE clean up and liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) analysis, and is suitable for the public Official control of ß-agonist residues in hair sample. Validation was performed according to Commission Decision 2002/657/EC requirements. Independent samples spiked with the investigated compounds in the range 0.2-10.0µgkg-1 are showing intra-day and inter-day precision (RSD) lower than 17.8% and 19.7%, respectively. Linearity, measured in the range of 0.1-10.0µgkg-1, resulted with a Pearson's r>0.996. The decision limits (CCα) for the all investigated beta agonists resulted in the range 0.2-1.0µgkg-1. Furthermore, the method was tested on real hair samples obtained from cattle, known as positive to clenbuterol, in order to check its effectiveness and the ß-agonists stability.