Validation data for aflatoxin determination in maize by LC-MS/MS
2016
Vuković, Gorica (Institute of Public Health, Belgrade (Serbia)) | Bursić, Vojislava (Faculty of Agriculture, Novi Sad (Serbia)) | Kos, Jovana (Faculty of Agriculture, Novi Sad (Serbia)) | Čolović, Radmilo (Institute of Food Technology, Novi Sad (Serbia)) | Vukmirović, Đuro (Institute of Food Technology, Novi Sad (Serbia)) | Bagi, Ferenc (Faculty of Agriculture, Novi Sad (Serbia))
Aflatoxins B1 (AFB1), B2, (AFB2), G1 (AFG1), and G2 (AFG2) are toxic secondary metabolities produced by certain strains of the common moulds Aspergillus flavus and Aspergillus parasiticus. This study was designed to develop a sensitive liquid chromatography tandem mass spectrometry (LCMS/MS) method for the simultaneous detection and quantification of aflatoxins (AFB1, AFB2, AFG1 and AFG2) in maize samples with particular focus on the optimization of the sample preparation protocol and method validation. Spiked maize samples were extracted with 80% methanol followed by the Vicam AOZTM immunoaffinity column clean-up. The mycotoxins were eluted from the column with methanol and quantified using Selected Reaction Monitoring (SRM) mode in LC-MS/MS with an electrospray ionization (ESI) interface. A mobile phase of methanol-water with 0.1% HCOOH was used. The run time of the analisys was 5.5 min. Calibration level ranged from 1-20 ng/ml for all aflatoxins (AFs), with R2>0.998. The average recoveries of AFs spiked on two levels (5.0 µg/kg and 1.0 µg/kg) in maize were 79.0% for AFB1; 76.5% for AFB2; 83.7% for AFG1 and 67.2% for AFG2, with relative standard deviation (% RSD) of 4.55; 2.31; 7.2 and 19.7%, respectively. The good accuracy and precision results were also obtained in intra-day and inter-day analysis. The limit of detection (LOD) of AFB1, AFB2, AFG1 and AFG2, were below 0.1 μg/kg. The obtained validated LC-MS/MS method could be applied as a conformity method for AFs analysis.
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