Wang Yujiao, Liu Tong, Deng Yamei, Wang Jiaqi, Chen Hong, Hua Erbing, Zhang Feng
College of Bioengineering, Tianjin University of Science and Technology, Tianjin 300000, China.
Institute of Food Safety, Chinese Academy of Inspection and Quarantine, Beijing 100176, China.
Se Pu. 2019 Jul 8;37(7):766-772. doi: 10.3724/SP.J.1123.2019.01032.
QuEChERS purification was established as a sample pretreatment method and combined with gas chromatography-tandem mass spectrometry (GC-MS/MS) for the simultaneous detection of six banned fragrance components in tea (coumarin, thujone, 2-exylthiophene, -beta-acacene, -mentha-1,8(10)diene-9-ethyl acetate, and butyl cinnamate). Tea samples were extracted with ethyl acetate and subjected to whirlpool oscillation, following which anhydrous magnesium sulfate, primary secondary amine (PSA), and octadecylsilyl silica gel (C18) were added to the supernatant. After centrifugation, the supernatant was filtered over a membrane and separated on a DB-5MS column. The six compounds were determined by GC-MS/MS in MRM mode, and quantified by a matrix-matched external standard method. The six banned flavor compounds exhibited good linearity over the range of 1-200 μg/L, and the linear correlation coefficients () were greater than 0.999. The limits of detection were 0.005-1 μg/kg and the limits of quantification were 0.02-2 μg/kg, the average recoveries were 82.3%-93.1%, and the intra-day and inter-day RSDs were each less than 10%. The method is simple, rapid, accurate, and sensitive, and can be used for the simultaneous detection of six banned fragrance components in tea.
建立了QuEChERS净化作为样品预处理方法，并与气相色谱 - 串联质谱法（GC-MS/MS）相结合，用于同时检测茶叶中的六种禁用香料成分（香豆素、侧柏酮、2-己基噻吩、β-刺苞菊烯、薄荷-1,8(10)二烯-9-乙酸乙酯和肉桂酸丁酯）。茶叶样品用乙酸乙酯提取并进行涡旋振荡，然后向上清液中加入无水硫酸镁、伯仲胺（PSA）和十八烷基硅烷硅胶（C18）。离心后，将上清液通过膜过滤，并在DB-5MS柱上进行分离。六种化合物通过GC-MS/MS在多反应监测（MRM）模式下测定，并采用基质匹配外标法进行定量。六种禁用香料化合物在1 - 200 μg/L范围内呈现良好的线性，线性相关系数（）大于0.999。检测限为0.005 - 1 μg/kg，定量限为0.02 - 2 μg/kg，平均回收率为82.3% - 93.1%，日内和日间相对标准偏差均小于10%。该方法简便、快速、准确、灵敏，可用于同时检测茶叶中的六种禁用香料成分。
