Kemisk analys

Ämnesområden: Djurfoder; Kemisk analys
Kommittébeteckning: SIS/TK 435 (Livsmedel och foder)
Källa: CEN
Svarsdatum: den 13 sep 2018
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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 μg/kg to 250 μg/kg for individual alkaloids. Determination of concentrations above 250 μg/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 μg/kg to 221 μg/kg, ergocorninine in the tested range of 9 μg/kg to 196 μg/kg, ergocristine in the tested range of 14 μg/kg to 312 μg/kg, ergocristinine in the tested range of 12 μg/kg to 258 μg/kg, α-ergocryptine in the tested range of 10 μg/kg to 184 μg/kg, α-ergocryptinine in the tested range of 8 μg/kg to 171 μg/kg, ergometrine in the tested range of 12 μg/kg to 174 μg/kg, ergometrinine in the tested range of 3 μg/kg to 172 μg/kg, ergosine in the tested range of 12 μg/kg to 226 μg/kg, ergosinine in the tested range of 9 μg/kg to 273 μg/kg, ergotamine in the tested range of 11 μg/kg to 443 μg/kg, ergotaminine in the tested range of 10 μg/kg to 273 μg/kg, atropine in the tested range of 16 μg/kg to 252 μg/kg and scopolamine in the tested range of 15 μg/kg to 246 μg/kg.