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
QuEChERS combined with ultra-high performance liquid chromatography-tandem mass spectrometry to determine acrylamide in Xinjiang Naan products
徐曼 1宋少龙 1胡俊 1施海云 1刘健2
作者信息
- 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
- 折叠
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 T3(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 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.
关键词
QuEChERS/馕/超高效液相色谱—串联质谱法/丙烯酰胺Key words
QuEChERS/Xinjiang Naan products/ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)/acrylamide引用本文复制引用
出版年
2024
国家科技期刊平台
NSTL
万方数据