Animal feeding stuffs: Methods of sampling and analysis - Determination of ergot alkaloids and tropane alkaloids in feed materials and compound feeds by LC-MS/MS
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 ??/kg to 250 ??/kg for individual alkaloids. Determination of concentrations above 250 ??/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 ??/kg to 221 ??/kg@ ergocorninine in the tested range of 9 ??/kg to 196 ??/kg@ ergocristine in the tested range of 14 ??/kg to 312 ??/kg@ ergocristinine in the tested range of 12 ??/kg to 258 ??/kg@ ??-ergocryptine in the tested range of 10 ??/kg to 184 ??/kg@ ??-ergocryptinine in the tested range of 8 ??/kg to 171 ??/kg@ ergometrine in the tested range of 12 ??/kg to 174 ??/kg@ ergometrinine in the tested range of 3 ??/kg to 172 ??/kg@ ergosine in the tested range of 12 ??/kg to 226 ??/kg@ ergosinine in the tested range of 9 ??/kg to 273 ??/kg@ ergotamine in the tested range of 11 ??/kg to 443 ??/kg@ ergotaminine in the tested range of 10 ??/kg to 273 ??/kg@ atropine in the tested range of 16 ??/kg to 252 ??/kg and scopolamine in the tested range of 15 ??/kg to 246 ??/kg.