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New method of citrinin determination by HPLC after polyamide column clean-up

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Abstract

In the past, various analytical methods of citrinin determination have been published; their application is not unproblematic. In this article, a HPLC method for sensitive fluorescence detection, based on solid phase extraction in combination with a HPLC gradient, is described. The samples are extracted with dichloromethane with the addition of phosphoric acid, and the extract is cleaned up on polyamide columns. According to this method, citrinin is detectable in cereals and milling products up to a detection limit of ~1–2 μg/kg (limit of quantification: 3–5 μg/kg). The mean recovery rates amounted to 74–90%. Analyses of some samples containing ochratoxin A (OTA) show that citrinin is especially detectable in cereal products, such as brans, wheatings and shorts, which contain increased amounts of the outer layers of the kernel. Citrinin, as well as OTA, was also detected in cocoa shells and raisins. 14 OTA-containing samples had citrinin contents of 1–8 μg/kg. Further, it was demonstrated that the new method is also applicable for citrinin determination in red-fermented rice.

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Acknowledgements

The project was supported by the Federal Ministry of Consumer Protection, Nutrition and Agriculture. Thanks are also expressed to Dr. Dietrich of the University of Munich for rapid analyses of some citrinin-containing samples by EIA, and to Dr. Richter of Bayrische Landesanstalt für Landwirtschaft in Poing for providing some samples (wheat inoculated with Penicillium verrucosum, kernel peas) from storage tests.

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  1. IGV Institut für Getreideverarbeitung GmbH, Arthur-Scheunert-Allee 40–41, 14558, Bergholz-Rehbrücke, Germany

    Ute Meister

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  1. Ute Meister
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Correspondence to Ute Meister.

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Meister, U. New method of citrinin determination by HPLC after polyamide column clean-up. Eur Food Res Technol 218, 394–399 (2004). https://doi.org/10.1007/s00217-003-0858-1

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  • DOI: https://doi.org/10.1007/s00217-003-0858-1

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