05 February 2003

Development of a reliable and sensitive HPLC method for the determination of citrinin in cereals and cereal products

As ochratoxin A (OTA) also the mycotoxin citrinin has a kidney injurious and possibly cancerogenic effect to humans. Nephritic tumors were observed in animal tests. Citrinin together with OTA is produced by mold fungi (penicillia, aspergilli) on numerous agricultural products and can endanger the health of humans and animals.

Till recently, little attention was paid to citrinin as against OTA, which fact possibly is due to the poorer analytical determinability. Therefore, the project was aimed at the development of a reliable and sensitive HPLC method for the determination of citrinin preferably in cereals and cereal products. A new method was developed and validated which is based on the solid phase extraction with polyamide columns and a gradient HPLC method with fluorescence detection. The intensive consideration of the problem of citrinin analytics has resulted in a method according to which citrinin can be determined in cereal samples with satisfactory recovery rate and good detection sensitivity and precision. Sufficient skill and experience with the method given, precise results, i.e. variation coefficients <10 %, will be achieved. The mean recovery rates were in the range 74-90 %. The detection limits of the new method determined according to DIN 32645, at good precision (process standard deviation 4-7 %) amounted to 1 µg/kg for wheat, rye, barley, maize, and oats.

The analysis of several OTA containing samples according to the new method has shown that citrinin is contained relatively frequently in brans, wheatings and shorts containing a higher ratio of the outer layers of the grain kernel; beside OTA citrinin also is contained in cocoa shells and raisins. Citrinin was detected in 14 of 35 OTA containing samples. Further, it was demonstrated that citrinin also can be determined in red mold rice according to the new method.

The method can be used for collecting data on the frequency of occurrence of citrinin and consequently for increasing the consumer safety. The accreditated test laboratory of IGV Ltd. is experienced and available for citrinin analyses.

IGV Institut für Getreideverarbeitung GmbH
Arthur-Scheunert-Allee 40/41
14558 Bergholz-Rehbrücke

Contact: Ines Gromes
Fon.:        03 32 00/89-107
Fax:        03 32 00/89-220
e-mail:    igv-transfer@institut-fuer-getreideverarbeitung.net