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

✍ Scribed by Carola Müller; Sabine Kemmlein; Horst Klaffke; Werner Krauthause; Angelika Preiß-Weigert; Reiner Wittkowski

• Publisher: John Wiley and Sons
• Year: 2009
• Tongue: English
• Weight: 686 KB
• Volume: 53
• Category: Article
• ISSN: 1613-4125
• DOI: 10.1002/mnfr.200800091

✦ Synopsis

Abstract

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.