Direct determination of the estrogenic compounds 8-prenylnaringenin, zearalenone, α- and β-zearalenol in beer by liquid chromatography–mass spectrometry

• Published in: Journal of Chromatography A 2008-08, Vol.1202 (1), p.47-57
• Main Authors: Maragou, Niki C., Rosenberg, Erwin, Thomaidis, Nikolaos S., Koupparis, Michael A.
• Format: Article
• Language: English
• Subjects: 8-prenylnaringenin; alpha-zearalenol; Beer - analysis; Beers; beta-zearalenol; Biological and medical sciences; Chromatography, Liquid - methods; DOE (design of experiments); Endocrine-disrupting compounds; Estrogens - analysis; Estrogens - chemistry; Fermented food industries; Flavanones - analysis; Flavanones - chemistry; Food analysis; Food industries; Fundamental and applied biological sciences. Psychology; LC–ESI–MS; liquid chromatography; mass spectrometry; Molecular Structure; Mycotoxins; Phytoestrogens; plant estrogens; Reproducibility of Results; Spectrometry, Mass, Electrospray Ionization - methods; zearalenone; Zearalenone - analysis; Zearalenone - chemistry; Zeranol - analogs & derivatives; Zeranol - analysis; Zeranol - chemistry
• ISSN: 0021-9673
• DOI: 10.1016/j.chroma.2008.06.042

A novel LC–ESI–MS method for the simultaneous determination of four of the most significant estrogenic compounds naturally occurring in beer, 8-prenylnaringenin (8-PN), zearalenone (ZON), α-zearalenol (α-ZOL) and β-zearalenol (β-ZOL) which requires minimal sample preparation was developed using a chemometric approach. Experimental design was applied to assess the effects of the LC–ESI–MS parameters (mobile phase flow rate, drying gas flow, nebuliser pressure and capillary potential) on the obtained signal and to optimize the values in order to provide maximum sensitivity and detectability. The proposed method is simple, consisting only of degassing the beer and diluting with water (1:1, v/v) before injection. Comparison between the two internal standards used, zearalanone (ZAN) and 4,2′-dihydroxychalcone (4,2′-DHC), showed that ZAN performs better as internal standard not only for the mycotoxins but for 8-PN as well, giving lower % RSDs. Under inter-day conditions mean recoveries were 107% for ZON, 87.8% for α-ZOL, 72.8% for β-ZOL, and 77.5% for 8-PN. The corresponding % RSDs ranged between 5.0 and 8.0. The method limits of detection were 1.3, 1.4, 1.0 and 0.8 ng mL −1 for ZON, α-ZOL, β-ZOL and 8-PN, respectively. The method was applied to 15 beer samples obtained from local supermarkets and the concentration of the phytoestrogen 8-PN in beer ranged between