Target screening method for the quantitative determination of 118 pyrrolizidine alkaloids in food supplements, herbal infusions, honey and teas by liquid chromatography coupled to quadrupole orbitrap mass spectrometry.

An analytical procedure for the screening of 118 pyrrolizidine alkaloids (PAs) was successfully validated and applied to their quantitative determination in food supplements, herbal infusions, honey, and teas. It provides the reliable analyte identification by high-resolution tandem mass spectrometry (HRMS/MS), the accurate determination of 21 regulated PAs, and broad contamination profiles. 10% of 281 analyzed samples resulted contaminated at levels above the maximum levels (MLs) of European legislation. The contamination of herbal infusions of mixed plants can represent a possible health concern (23%; mean of PA sum above ML). A high number of PAs not included in the regulation was detected in honey and herbal food supplements, but their contribution was only relevant to the overall level in honey. The results indicate the need to continue collecting contamination data in food supplements and infusions of mixed herbs and to expand the PA-pool to be monitored in honey and related products.

An analytical platform for the screening and identification of pyrrolizidine alkaloids in food matrices with high risk of contamination.

An analytical platform for the detection of pyrrolizidine alkaloids (PAs) in honey, pollen, teas, herbal infusions, and dietary supplements is proposed; it includes a wide-scope suspect screening method, based on a diagnostic product ion filtering strategy for the characterization of PAs, and a target screening and identification method for the high-throughput detection of 118 PAs of a high-resolution mass spectral library. Salting-out assisted liquid-liquid extraction of aqueous extracts combined to ultra-high performance liquid chromatography-high-resolution tandem mass spectrometry was employed. The limit of identification (0.6-30 µg kg-1) of 28 standards were fit-for-purpose in PA-monitoring applications, with a false negative rate <1.3 % at 4 µg L-1. The wide-scope suspect screening method allowed the tentative identification of 88 compounds. The screening of 282 commercial samples revealed a broad contamination of the studied matrices, demonstrating the effectiveness of the platform in detecting and identifying both target and untarget PAs.