DETERMINATION OF ZEARALENONE WITH LIQUID CHROMATOGRAPHY TANDEM MASS SPECTROMETRY

Za določanje mikotoksina zearalenona v ţitaricah smo uvedli in validirali metodo tekočinske kromatografije s tandemsko masno spektrometrijo (LC/MS/MS). Vzorec po dodatku internega standarda zearalenona homogeniziramo z raztopino acetonitrila in vode. Po filtriranju in redčenju ekstrakt analiziramo s tekočinsko kromatografijo in tandemsko masno spektrometrijo z ionizacijo z negativnim električnim razprševanjem. Rezultate vzorcev smo ovrednotili s pomočjo umeritvene krivulje v koncentracijah od 40 μg/kg do 640 μg/kg. Mejna oziroma dovoljena vsebnost zearalenona je 100 μg/kg. Rezultate smo statistično ovrednotili glede na zahteve analizne metode (linearnost kalibracijske funkcije, meja zaznavanja, meja določanja, pravilnost, izkoristek metode, ponovljivost, obnovljivost, stabilnost v ekstraktu, stabilnost med hranjenjem vzorca, merilna negotovost). Metoda določanja vsebnosti zearalenona v ţitaricah s tekočinsko kromatografijo in masno spektrometrijo je primerna in uporabna zaradi enostavne in hitre priprave vzorcev. Rezultati analiz so v merilnem območju od 40 μg/kg do 640 μg/kg natančni in pravilni.For determination of mycotoxin zearalenone in cereals validated analytical method using liquid chromatography and tandem mass spectrometry (LC/MS/MS) was used. The samples were homogenized with acetonitrile and water after addition of internal standard zearalenone . After filtration and dilution the extracts were analyzed using liquid chromatography tandem mass spectrometry by negative electrospray (ESI) ionization. The results of the samples were evaluated using calibration curve in concentration range from 40 μg/kg to 640 μg/kg. The limit of zearalenone is 100 μg/kg. The results were statistically evaluated according to demands of the analytical method (linearity , limit of detection, limit of quantification, accuracy, efficiency of the method, repeatability, reproducibility, stability in the extract, the stability during storage of the sample, measurement uncertainty). The method for determination of zearalenone in cereals by liquid chromatography and mass spectrometry is suitable and useful because of simple and rapid preparation of samples. Results within a measurement range from 40 μg/kg to 640 μg/kg are precise and accurate