Determination of the New Illegal Additive Acetohydroxamic Acid in Wheat Flour, Wheat-flour Products and Wheat-flour Additives using UPLC-MS/MS
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Abstract:
An analytical method based on ultra-performance liquid-chromatography-tandem mass spectrometry was developed for the determination of a new illegal additive, acetohydroxamic acid (AHA), in wheat flour, wheat-flour products, and wheat-flour additives. Five representative samples (wheat flour, a wheat-flour additive, dough, noodles, and steamed bun) were selected as the study matrices. AHA was first extracted using ultrasonic and vortex oscillation with methanol as the extraction solvent, subjected to high-speed centrifugation and filtration, and then separated using a T3 column (2.1 mm×150 mm, 3 μm) with a mixture of 0.10% (volume fraction) aqueous formic acid and methanol as the eluting mobile phase. Finally, it was quantified using an external standard method using an atmospheric pressure chemical ionization source (APCI) and multiple reaction monitoring mode. The results showed that the solvent and matrix standard curves of AHA had good linearity in the 0.075~5.00 mg/L range, with correlation coefficients>0.999. The limit of detection was 0.25 mg/kg, the spike recovery rate was 78.49%~108.61%, and the relative standard deviation (RSD, n=6) was 1.67%~7.50%. This method is suitable for the determination of AHA in wheat flour, wheat-flour products and wheat-flour additives, exhibiting good anti-interference capacity and high accuracy.
