Determination of Mycotoxin Biomarkers in Eggs by Liquid Chromatography-Tandem Mass Spectrometry Coupled with Matrix Solid Phase Dispersion / 分析化学

ABSTRACT

A matrix solid phase dispersion ( MSPD) method was developed for the simultaneous preparation of samples of 15 mycotoxin biomarkers including deoxynivalenol, aflatoxins and zearalenone from eggs, which were subsequently determined by liquid chromatography-electrospray ionization tandem mass spectrometry ( LC-ESI-MS/MS) under the multiple reaction monitoring ( MRM) mode. For the analysis, the samples were first mixed with C18 particles and loaded into an empty column, then 20 mL of acetonitrile/methanol (11, V/V) containing 1 mmol/L ammonium formate was used to elute the sample. The eluent was then dried with nitrogen flow and redissolved into the mobile phase. After filtration, samples were brought into vials and used for analysis. Different from other methods, no extra complicated purification and centrifugation steps were required in the procedure of MSPD. This method had good linearity in the range of 0. 2-100 ng/mL, with the correlation coefficient (r2) greater than 0. 9931. The limits of detection (LODs, S/N=3) and limits of quantification ( LOQs, S/N=3 ) of this method were 0. 05-2 μg/kg and 0. 2-4 μg/kg respectively. Comprehensive extraction recoveries of the 15 compounds ranged from 61% to 90%.