A 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 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% (alpha-ergokryptine) with a maximum LOQ of 3.3 microg/kg (ergometrine). Precision expressed as RSD ranged from 2.8% (ergocristine) to 12.4% (alpha-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 microg/kg (ergocristine), and 134 microg/kg (ergotamine) in rye flour, and 152.5 and 117.8 microg/kg in coarse meal, respectively.
Müller
Carola
C
Federal Office of Consumer Protection and Food Safety, Berlin, Germany. carola.mueller@bvl.bund.de
Kemmlein
Sabine
S
Klaffke
Horst
H
Krauthause
Werner
W
Preiss-Weigert
Angelika
A
Wittkowski
Reiner
R
D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D004876:Ergot Alkaloids / Q000032:analysis*; D005433:Flour / Q000032:analysis / Q000382:microbiology; D005470:Fluorometry; D018570:Risk Assessment; D012434:Secale / Q000737:chemistry / Q000382:microbiology*
D004876:Ergot Alkaloids