QuEChERS结合超高效液相色谱—串联质谱法测定新疆馕制品中丙烯酰胺
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(1. 克拉玛依市疾病预防控制中心 ,新疆 克拉玛依 834000; 2. 新疆第二医学院 ,新疆 克拉玛依 834000)

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刘健(1966—),女,新疆第二医学院主任技师,硕士。E-mail:399720089@qq.com

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新疆维吾尔自治区卫生健康青科项目(编号:WJWY-202307)


QuEChERS combined with ultra-high performance liquid chromatography-tandem mass spectrometry to determine acrylamide in Xinjiang Naan products
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(1. Karamay City Center for Disease Control and Prevention , Karamay , Xinjiang 834000 , China; 2. Xinjiang Second Medical College , Karamay , Xinjiang 834000 , China)

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    摘要:

    [目的]建立一种快速、准确测定新疆特色馕制品中丙烯酰胺的分析方法。[方法]样品加入13C3-丙烯酰胺同位素内标后,依次加入 9 mL水、10 mL乙腈、6 mL正己烷、6 g无水硫酸镁和 1.5 g醋酸钠盐析剂,分别涡旋振荡提取,离心后弃去正己烷层。取4 mL乙腈层经 400 mg无水硫酸镁和 300 mg PSA 净化,上清液氮吹至近干,用水复溶后测定。采用水—甲醇作为流动相,经ACQUITY UPLC HSS T 3(100 mm ×2.1 mm,1.8 μm)柱分离,电喷雾电离正离子模式,多反应监测模式,内标法定量。[结果]丙烯酰胺在 1.0~100 ng/mL范围内线性关系良好 (R2>0.999 1),方法检出限和定量限分别为 0.25,0.82 μg/kg,3种不同基质的馕样品中进行 3个水平的加标试验,丙烯酰胺的平均回收率为 91.3%~97.6%,相对标准偏差为 1.3%~4.6%。对市售 65份馕样品进行分析,丙烯酰胺含量为 17.4~207.5 μg/kg,不同种类馕样品中的含量存在显著差异 (H=23.10,P<0.05)。[结论]该方法取样量和试剂消耗量小,过程快速简便,结果准确,对不同种类的馕制品具有普适性。

    Abstract:

    [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 T 3 (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.

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徐 曼,宋少龙,胡 俊,等. QuEChERS结合超高效液相色谱—串联质谱法测定新疆馕制品中丙烯酰胺[J].食品与机械,2024,40(11):61-68.
XU Man, SONG Shaolong, HU Jun, et al. QuEChERS combined with ultra-high performance liquid chromatography-tandem mass spectrometry to determine acrylamide in Xinjiang Naan products[J]. Food & Machinery,2024,40(11):61-68.

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  • 收稿日期:2024-01-24
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  • 在线发布日期: 2025-02-18
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