Determination of Mycotoxins in Brown Rice Using QuEChERS Sample Preparation and UHPLC-MS-MS

Abstract

QuEChERS sample preparation was optimized and validated using solvent extraction with 10% (v/v) acetic acid-containing acetonitrile in the presence of four salts (anh. MgSO4, NaCl, sodium citrate tribasic dihydrate and sodium citrate dibasic sesquihydrate) and dispersive solid-phase extraction with mixed sorbents (octadecylsilane, primary and secondary amine and silica sorbents) for an ultra high performance liquid chromatography-tandem mass spectrometric determination of nine mycotoxins in brown rice: aflatoxins (AFB1, AFB2, AFG1 and AFG2), fumonisins (FB1 and FB2), deoxynivalenol, ochratoxin A and zearalenone (ZON). Our developed method allows for the determination of trace levels of mycotoxins with method detection limits in the range of 1.4-25 μg/kg, below the maximum limits of EU regulations, and with an acceptable accuracy and precision, and recoveries in the range of 81-101% with relative standard deviations of 5-19% over a mycotoxin concentration range of 5.0-1,000 μg/kg. Six out of fourteen real samples of brown rice were found to be contaminated with at least one of these mycotoxins, ranging from 2.49-5.41 μg/kg of FB1, 4.33 ± 0.04 μg/kg of FB2 and 6.10-14.88 μg/kg of ZON.