20.500.12556/DKUM-20538 DOLOČANJE ZEARALENONA Z METODO LC/MS/MS 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. tekočinska kromatografija masna spektrometrija mikotoksini zearalenon validacija liquid chromatography mass spectrometry mycotoxins zearalenone validation true true false [M. Škrobar] Slovenski jezik Angleški jezik Diplomsko delo 2011-09-21 16:41:27 2011-10-04 14:24:30 2022-04-14 08:00:58 2023-12-27 03:13:40 2011 0 Maribor 0 0000-00-00 NiDoloceno NiDoloceno NiDoloceno 0000-00-00 0000-00-00 0000-00-00 543.51/.544.5(043.2) 15771670 URN:SI:UM:DK:ZVB1NCUJ UNI_Skrobar_Masa_2011.pdf UNI_Skrobar_Masa_2011.pdf 1 B109F3ED1DCF14ADA7D9246BD67C8036 71d27206475db5f411e7ab934773d432e7f874a50d4411848fd2b19b2addc37f 9b0fb43e-7c05-11eb-bb7a-00155d0001ca 20.500.12556/dkum/2baac679-8d0e-474c-80d4-0b276728d1f7 https://dk.um.si/Dokument.php?lang=slv&id=25501 Fakulteta za kemijo in kemijsko tehnologijo 0 0 0