basic tool for risk assessment: A new method for the analysis of ergot alkaloids in rye and selected rye products

As a basis for the collection of occurrence and exposure data of ergot alkaloids in food, an HPLC method coupled with fluorimetric detection (HPLC-FLD) for the determination of 12 pharmacologically active ergot alkaloids in rye and rye products was developed. Samples were extracted with a mixture of...

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Bibliographic Details
Published in:Molecular nutrition & food research 2009-04, Vol.53 (4), p.500-507
Main Authors: Müller, Carola, Kemmlein, Sabine, Klaffke, Horst, Krauthause, Werner, Preiß-Weigert, Angelika, Wittkowski, Reiner
Format: Article
Language:English
Subjects:
Chromatography, High Pressure Liquid - methods
Claviceps
Ergot alkaloids
Ergot Alkaloids - analysis
Flour - analysis
Flour - microbiology
Fluorometry
HPLC-FLD
Risk Assessment
Rye
Secale - chemistry
Secale - microbiology
Validation
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Summary:As a basis for the collection of occurrence and exposure data of ergot alkaloids in food, an HPLC method coupled with fluorimetric detection (HPLC-FLD) for the determination of 12 pharmacologically active ergot alkaloids in rye and rye products was developed. Samples were extracted with a mixture of ethyl acetate, methanol, and aqueous ammonia, followed by centrifugation and purification by solid phase filtration (SPF) with basic alumina. After solvent adjustment, the samples were analyzed by HPLC-FLD using a phenyl-hexyl-column. Recoveries for five major alkaloids were between 89.3% (ergotamine) and 99.8% (α-ergokryptine) with a maximum LOQ of 3.3 μg/kg (ergometrine). Precision expressed as RSD ranged from 2.8% (ergocristine) to 12.4% (α-ergokryptine) for repeatability, and from 6.5% (ergocornine) to 14.9% (ergotamine) for within-laboratory reproducibility, respectively. In a survey of 39 rye product samples, ergocristine and ergotamine were found to be the major alkaloids in commercially available rye products with contents of 127 μg/kg (ergocristine), and 134 μg/kg (ergotamine) in rye flour, and 152.5 and 117.8 μg/kg in coarse meal, respectively.
ISSN:1613-4125
1613-4133
DOI:10.1002/mnfr.200800091