Determination of pyrrolizidine alkaloids in honey from selected sites by solid phase extraction and HPLC-MS.

A method was developed for the determination in honey of the Ragwort (Senecio jacobaea) derived pyrrolizidine alkaloids jacoline, jacozine, jacobine, seneciphylline and senecionine, combining solid‐phase extraction with high performance liquid chromatography and atmospheric pressure chemical ionization mass spectrometric detection. The method allowed determination of individual alkaloids and offered a considerable improvement in terms of speed, sensitivity and specificity over previous approaches, but was not suitable for determination of jaconine, a minor alkaloid in Ragwort. Instrument calibrations were linear over the range 0.005 to 10.0 μg/ml, equivalent to approximately 0.001 to 2.0 mg/kg in honey with the extraction method used and allowing for observed recoveries. Detection limits in honey were 0.002 mg/kg. Recoveries for most of the alkaloids were between 57 and 70%. The alkaloids have been determined in a number of samples of honey selected after pollen identification and counting. The alkaloids ...