Liu Tong, Wang Yujiao, Wang Xiujuan, Cui Dongwei, Zhang Feng
Institute of Food Safety, Chinese Academy of Inspection and Quarantine, Beijing 100176, China.
College of Bioengineering, Tianjin University of Science and Technology, Tianjin 300000, China.
Se Pu. 2019 Nov 8;37(11):1215-1220. doi: 10.3724/SP.J.1123.2019.04033.
A gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS) method was established for the simultaneous determination of nine flavor compounds (hydrocoumarin, vanillin, coumarin, ethyl vanillin, methyl vanillin, 7-methylcoumarin, 7-methyoxycoumarin, 7-ethoxy-4-mrthyl coumarin, pyranocoumarin) in pasteurized milk. The samples were extracted with ethanol and subjected to whirlpool oscillation. After centrifugation, the supernatant was filtered through a membrane, and the components were separated on a DB-5MS column. The nine analytes were detected by GC-MS/MS in the multiple reaction monitoring (MRM) mode and quantified by a matrix-matched external standard method. Good linearities in the range of 1-200 μg/L were observed for the nine flavor compounds. The linear correlation coefficients () were greater than 0.997. The limits of detection and limits of quantification were 0.002-0.1 μg/kg and 0.001-2 μg/kg, respectively. The average recoveries were 90.3%-110.6%. Both the intra-day and inter-day RSDs were less than 10%. The developed method is simple, rapid, accurate and sensitive, and can be used for the simultaneous determination of the nine flavor compounds in pasteurized milk.
建立了一种气相色谱 - 三重四极杆质谱法（GC-MS/MS），用于同时测定巴氏杀菌乳中的9种风味化合物（氢化香豆素、香草醛、香豆素、乙基香草醛、甲基香草醛、7-甲基香豆素、7-甲氧基香豆素、7-乙氧基-4-甲基香豆素、吡喃香豆素）。样品用乙醇提取并进行涡旋振荡。离心后，上清液通过膜过滤，各组分在DB-5MS柱上分离。采用GC-MS/MS在多反应监测（MRM）模式下对9种分析物进行检测，并采用基质匹配外标法进行定量。9种风味化合物在1 - 200 μg/L范围内具有良好的线性关系。线性相关系数（）大于0.997。检测限和定量限分别为0.002 - 0.1 μg/kg和0.001 - 2 μg/kg。平均回收率为90.3% - 110.6%。日内和日间相对标准偏差均小于10%。所建立的方法简便、快速、准确、灵敏，可用于同时测定巴氏杀菌乳中的9种风味化合物。
