QuEChERS combined with ultra-high performance liquid chromatography-tandem mass spectrometry to determine acrylamide in Xinjiang Naan products
[Objective]This study aimed to establish a rapid and accurate analytical method for the determination of acrylamide in Xinjiang characteristic Naan products.[Methods]The methodology involved adding the internal standard 13C3-acrylamide isotope to the samples,followed by the sequential addition of 9 mL of water,10 mL of acetonitrile,6 mL of n-hexane,6 g of anhydrous magnesium sulfate,and 1.5 g of sodium acetate salting agent.The samples were then extracted using vortex oscillation and centrifugation,discarding the n-hexane layer.Take 4 mL of the acetonitrile layer was purify with 400 mg of anhydrous magnesium sulfate and 300 mg PSA.The supernatant was evaporated to near dryness using liquid and subsequently re-dissolved in water for measurement.The separation was performed using ACQUITY UPLC HSS T3(100 mm×2.1 mm,1.8 µm)column,with a mobile phase of water-methanol,in electrospray ionization positive ion mode and multi-reaction monitoring mode.[Results]The method demonstrated a strong linear relationship for acrylamide detection within the range of 1.0～100 ng/mL(R2>0.999 1),with detection and quantitation limits of 0.25 µg/kg and 0.82 µg/kg,respectively.Recovery tests at three different concentration levels in various sample matrices yielded an average recovery rate of 91.3%～97.6%,with RSD values ranging from 1.3%～4.6%.Analysis of 65 commercially available naan samples revealed acrylamide contents ranging from 17.4～207.5 µg/kg,with significant differences observed among different types of Naan(H=23.10,P<0.05).[Conclusion]The proposed method features minimal sampling volume and reagent consumption,along with a rapid and straightforward process that yields accurate results.It is applicable to various types of naan products,demonstrating its versatility and efficiency.
QuEChERSXinjiang Naan productsultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)acrylamide
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