Simultaneous Determination of Four Individual Alternaria Toxins by Ultra-high Performance Liquid Chromatography-tandem Mass Spectrometry in Flour
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Abstract:
A sensitive and rapid method based on solid phase extraction (SPE) and ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS /MS) was developed for the determination of four individual Alternaria toxins in the wheat flour. The samples were extracted with the mixture of 0.05 mol/L NaH2PO4 (pH3.0)-acetonitrile-methanol (450+450+100, V/V) by ultrasound, and then purified by HLB solid-phase extraction column. The separation used Waters CORTECS C18 (4.6×100 mm, 2.7 μm) column gradient elution with 1.0 mmol/L ammonia solution (pH 8.3) and methanol as the mobile phase. The electrospray negative ion (ESI-) and multiple reaction monitoring mode (MRM) pattern were used to detect and the matrix additive standard was used toquantify the Alternaria Toxins. The tenuazonic acid(TeA) and alternariol (AOH) in concentration range of 2.0~100 μg/L, as well as tentoxin (TEN) and alternariol methyl ether (AME) in concentration range of 0.2~10.0 μg/L, had a good linear relationship with the correlation coefficient (R2) of > 0.998. The average recovery was 76.3%~107.5%. The detection limit and the quantitative limit of TeA, AOH, TeA and AME were 1.0 μg/kg and 3.0 μg/kg, respectively. The detection limit and the quantitative limit were 0.1 μg/kg and 0.3 μg /kg, respectively. Therefore, the method is suitable for the determination of Alternaria toxins in flour.
