ABSTRACT
Pyrrolizidine alkaloids (PAs) and related N-oxides (PANOs) are secondary plant metabolites thought to be found in approximately 3% of the flowering plants worldwide and exhibiting hepatotoxic properties to humans. As a consequence, beehive products are prone to be contaminated with those compounds by bees foraging PA-producing plants. Downstream contamination can also occur through food items containing honey. Analytical methods based on UHPLC separation and MS/MS detection were developed with a focus on very low LOQs and validated for the analysis of 16 PAs and 14 PANOs in honey, honey-based candies and snacks, as well as beehive product-based food supplements. A maximum level of 182 ng/g of PAs was detected in a Mediterranean honey, and high levels of heliotrine-type compounds were reported for the first time. An extensive sampling of honeys harvested in Belgium was performed (N = 374), the concentration levels were more limited with a maximum of 60 ng/g, and the contamination pattern was dominated by senecionine-type PAs. The PA levels in honey-based candies and snacks were very low, with respective maxima of 7.61 ng/g and 0.36 ng/g. Seventy-five percent among the pre-dosed food supplements based on beehive products were contaminated, with a maximum of 43 ng/g. The highest level was detected in a bee-collected pollen sample (1672 ng/g). The analytical results were consistent with the previously reported data for beehive products and confirmed that PA/PANO contamination in these food commodities is recurrent.
Subject(s)
Honey , Pyrrolizidine Alkaloids , Animals , Bees , Belgium , Food Contamination , Humans , Pyrrolizidine Alkaloids/analysis , Tandem Mass SpectrometryABSTRACT
Two sample preparation methods were developed (graphitised carbon and C18 solid phase extraction clean-up) and validated in house using liquid chromatography and tandem mass spectrometry (MS/MS) for the determination of 30 pyrrolizidine alkaloids (PAs) in salads, herbs, tea, herbals teas as well as tea infusion and ice-tea beverages. Total PAs concentration of samples purchased on the Belgian market varied greatly with matrix type ranging from Subject(s)
Beverages/analysis
, Pyrrolizidine Alkaloids/analysis
, Tandem Mass Spectrometry
, Teas, Herbal/analysis
, Chromatography, High Pressure Liquid
, Food Analysis
, Graphite/chemistry
, Limit of Detection
, Pyrrolizidine Alkaloids/chemistry
, Pyrrolizidine Alkaloids/isolation & purification
, Solid Phase Extraction