This document describes a method for the determination of individual ergot alkaloids and tropane alkaloids in unprocessed cereals and cereal-based compound feeds by high performance liquid chromatography with tandem mass spectrometry (LC-MS/MS). This method has been successfully validated by collaborative trial in the following matrices: rye, barley, wheat, complete feed for bovine, porcine and poultry. Validation in buckwheat produced acceptable results, but the relative standard reproducibility was higher for most analytes in comparison with the other matrices. This may be related to the matrix. The validated range of the method is approximately 10 ¼g/kg to 250 ¼g/kg for individual alkaloids. Determination of concentrations above 250 ¼g/kg is possible by applying a higher spiking level and dilution of the sample extract, but this has not been validated in the collaborative trial. The method is applicable for the determination, by means of one-point standard addition to the sample, of ergocornine in the tested range of 12 ¼g/kg to 221 ¼g/kg, ergocorninine in the tested range of 9 ¼g/kg to 196 ¼g/kg, ergocristine in the tested range of 14 ¼g/kg to 312 ¼g/kg, ergocristinine in the tested range of 12 ¼g/kg to 258 ¼g/kg, ±-ergocryptine in the tested range of 10 ¼g/kg to 184 ¼g/kg, ±-ergocryptinine in the tested range of 8 ¼g/kg to 171 ¼g/kg, ergometrine in the tested range of 12 ¼g/kg to 174 ¼g/kg, ergometrinine in the tested range of 3 ¼g/kg to 172 ¼g/kg, ergosine in the tested range of 12 ¼g/kg to 226 ¼g/kg, ergosinine in the tested range of 9 ¼g/kg to 273 ¼g/kg, ergotamine in the tested range of 11 ¼g/kg to 443 ¼g/kg, ergotaminine in the tested range of 10 ¼g/kg to 273 ¼g/kg, atropine in the tested range of 16 ¼g/kg to 252 ¼g/kg and scopolamine in the tested range of 15 ¼g/kg to 246 ¼g/kg.