A Validated, Rapid HPLC-ESI-MS/MS Method for the Determination of Lycopsamine

The aim of the present work was to develop and validate an HPLC-MS/MS method for the determination of a major pyrrolizidine alkaloid of comfrey (lycopsamine) in aqueous samples as a basis for the development of a method for the determination of absorption of lycopsamine by human skin. A linear calibration curve was established in the range of 1.32-440 ng. The intraday precision during the 3-day validation period ranged between 0.57 and 2.48% while the interday precision was 1.70% and 1.95% for quality control samples. LOD was 0.014 ng and recovery was above 97%. The lycopsamine content of the samples stored for 9 and 25 days at 22 degrees C, 10 degrees C and -25 degrees C did not vary. These results underline the good repeatability and accuracy of our method and allow the analysis of samples with very low lycopsamine content.