Guangzhou Quality Supervision and Testing Institute, Research Center of Risk Dynamic Detection and Early Warning for Food Safety of Guangzhou City, Key Laboratory of Detection Technology for Food Safety of Guangzhou City, Guangzhou 511447, China.
College of Light Industry and Food Sciences, Zhongkai University of Agriculture and Engineering, Guangzhou 510225, China.
Food Chem. 2019 Jul 1;285:77-85. doi: 10.1016/j.foodchem.2019.01.132. Epub 2019 Jan 30.
Based on QuEChERS dispersed purification, FeO nanoparticle decoloration and UHPLC-MS/MS, a robust and sensitive method was established for simultaneous analysis of 14 heterocyclic aromatic amines (HAAs) and acrylamide (AA) in coffee products. Sample was extracted by 90% acetonitrile water (v/v), dispersed with primary secondary amine (PSA) and further purified with FeO nanoparticle. Then, 15 analytes were detected using ESI positive ion under MRM mode. Good linearity was observed for all analytes in the range of 0.2-100 μg/L with the determination coefficients being above 0.996. Limits of detection (S/N ≥ 3) and limits of quantification (S/N ≥ 10) were in the range of 0.02-0.15 µg/L and 0.2-0.7 µg/L, respectively. The intra-day average recoveries were between 81.6% and 100%, and the intra-day precisions ranged from 4.3% to 9.0%. The inter-day average recoveries were in the range of 81.0-101% with precisions ranging from 5.0% to 7.8%. Results indicated that the combination of PSA and FeO exhibited superior purification and adsorption effects for removing pigments and acid compounds. Real samples analysis indicated that coffee products were widely contaminated with AA, harman and norharman.
基于 QuEChERS 分散净化、FeO 纳米粒子脱色和 UHPLC-MS/MS,建立了一种同时分析咖啡产品中 14 种杂环芳香胺(HAAs)和丙烯酰胺(AA)的灵敏、稳健方法。样品用 90%乙腈-水(v/v)提取,用初级/次级胺(PSA)分散,然后用 FeO 纳米粒子进一步纯化。然后,在 MRM 模式下,ESI 正离子检测 15 种分析物。所有分析物在 0.2-100μg/L 范围内均表现出良好的线性关系,相关系数均大于 0.996。检出限(S/N≥3)和定量限(S/N≥10)分别为 0.02-0.15μg/L 和 0.2-0.7μg/L。日内平均回收率在 81.6%-100%之间,日内精密度在 4.3%-9.0%之间。日间平均回收率在 81.0%-101%之间,精密度在 5.0%-7.8%之间。结果表明,PSA 和 FeO 的组合对去除色素和酸类化合物具有优越的净化和吸附效果。实际样品分析表明,咖啡产品广泛受到 AA、哈尔曼和诺哈尔曼的污染。