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HPLC/MS/MS method for the determination of ergot alkaloids in cereals
Project Code: C03057
Central Science Laboratory
Crews, C ; Krska, R
Note: Final Report was agreed and finalised in March 2009.
A method has been developed and validated which enables the quantification of the six major ergot alkaloids in a number of cereals and cereal based food products. The six ergot alkaloids studied (ergometrine, ergotamine, ergosine, ergocristine, ergocryptine and ergocornine) have been defined by EFSA as of the major importance. In addition the method can determine the epimer isomers (-inines) corresponding to the major ergot alkaloids. This is of considerable importance in terms of the differences in toxicity of the isomeric forms.
The method was developed and validated using 10 different cereal and food samples. The extraction and clean-up procedure is simple and the analysis time short. The limits of quantification were 0.17 to 2.78 µg/kg depending on the analyte and matrix. Recovery values for the 12 ergot alkaloids spiked into 10 different matrices at levels of 5, 50 and 100 µg/kg were between 70 and 105% for 85 of 90 recovery measurements made over six days.
Measurement uncertainty values were highly satisfactory. At a concentration level of 5 µg/kg the expanded measurement uncertainty ranged from ± 0.56 to ± 1.49 µg/kg, at a concentration level of 100 µg/kg the expanded measurement uncertainty ranged from ± 8.9 to ± 20 µg/kg. Both LOQs and measurement uncertainties were dependent on the analyte but almost independent of the matrix.
The method performance was satisfactory when tested in a mini-intercomparison studywith two other laboratories that used alternative methods.
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