Detection of pyrrolizidine alkaloids in milk and honey on the Belgian market using UHPLC-MS/MS.

The objective of the research is to report occurrence levels of pyrrolizidine alkaloids (PAs) and N-oxide (PANOs) in targeted food items on the Belgian market to perform a dietary exposure assessment to those contaminants and evaluate if they can pose a health problem, hampering a data gap at Belgium's level. Diverse cases of human poisoning are documented and are mainly related to consumption of traditional herbal remedy, milk, dairy products or honey. As PAs are biosynthesized by a wide variety of plant species, intoxication could occur worldwide. Therefore, the development of efficient analytical methods is required to detect PAs at (very) low levels.Analytical methods based on UPLC separation and MS/MS detection were developed for the analysis of 16 PAs and 13 PANOs in honey and milk matrices at WIV-ISP. The sample preparation involves acidic extraction of the analytes followed by SCX-SPE purification to avoid loss of sensitivity due to matrix effect. Several parameters were optimized in order to obtain the best method sensitivity. The separation of PAs/PANOs was performed on a C18 stationary phase LC column. The analytical methods were validated in-house and the validation parameters met the critical validation criteria allowed by Directive 2002/657/CE. Moreover, the LOQs achieved (0.05 ng.g