Determination of 12 Mycotoxins in Seasoning Flour Products by QuEChERS-SPE-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

Abstract

A method was developed for the residual quantity determination of 12 mycotoxins in seasoning flour products by QuEChERS-SPE-ultra performance liquid chromatography-tandem mass spectrometry. The samples were extracted with formic acid acetonitrile aqueous solution and salted out by adding sodium chloride and anhydrous magnesium sulfate. The supernatant was taken and purified by Prime HLB column extraction. The purified liquid was further cleaned up by adding anhydrous magnesium sulfate, PSA, C18 and Al-N. The target compound, which was separated with Waters CORTECS C18+ column, was eluted by gradient elution. The electrospray ion source (ESI) positive ion mode and multiple reaction monitoring mode (MRM) were used for mass spectrometry. Take negative samples as ground substance whitespace along with matching standard curve. The quantification was achieved by external standard method. The results showed that within the scope of 0.3~1000 ng/mL, the linear relationships of 12 mycotoxins were very good, the determination coefficient (R2) of which were higher than 0.99. The limits of detection were 0.10~3.0 μg/kg, and the limits of quantity were 0.30~10.0 μg/kg. Under the adding levels of high and medium as well as low, the average adding standard recoveries of 12 mycotoxins were 84.2%~97.2% and the relative standard deviations (RSDs) were 3.25%~8.77% (n=6). This method with high recovery rate and high sensitivity was rapid and accurate, which would be used to simultaneously determinate the 12 mycotoxins in seasoning flour products.

Keywords

• ultra performance liquid chromatography-tandem mass spectrometry
• quechers
• solid phase extraction
• seasoning flour products
• mycotoxins