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A basic tool for risk assessment: A new method for the analysis of ergot alkaloids in rye and selected rye products
Author(s) -
Müller Carola,
Kemmlein Sabine,
Klaffke Horst,
Krauthause Werner,
PreißWeigert Angelika,
Wittkowski Reiner
Publication year - 2009
Publication title -
molecular nutrition and food research
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 1.495
H-Index - 131
eISSN - 1613-4133
pISSN - 1613-4125
DOI - 10.1002/mnfr.200800091
Subject(s) - ergotamine , chromatography , high performance liquid chromatography , chemistry , repeatability , ergometrine , ammonium acetate , biology , medicine , pharmacology , migraine
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.