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气相色谱-三重四极杆质谱法同时测定巴氏杀菌乳中9种香精成分
引用本文:刘通,王玉娇,王秀娟,崔东伟,张峰.气相色谱-三重四极杆质谱法同时测定巴氏杀菌乳中9种香精成分[J].色谱,2019,37(11):1215-1220.
作者姓名:刘通  王玉娇  王秀娟  崔东伟  张峰
作者单位:1.中国检验检疫科学研究院食品安全研究所, 北京 100176;2.天津科技大学生物工程学院, 天津 300000;3.中国医科大学药学院, 沈阳 110122
基金项目:国家重点研发计划(2017YFC1601600,2018YFC1603606);国家高层次人才特殊支持计划(检科2019-006).
摘    要:建立了气相色谱-三重四极杆质谱(GC-MS/MS)同时检测巴氏杀菌乳中9种香精成分(二氢香豆素、香兰素、香豆素、乙基香兰素、甲基香兰素、7-甲基香豆素、7-甲氧基香豆素、7-乙氧基-4甲基香豆素和环香豆素)的分析方法。巴氏杀菌乳样品用乙醇溶液萃取,低温涡旋离心,取上清液过0.22 μm滤膜,以DB-5MS色谱柱分离,在MRM模式下测定,基质曲线外标法定量。实验结果表明,9种香精成分在1~200 μg/L范围内呈良好线性,线性相关系数(R2)均大于0.997,方法的检出限为0.002~0.1 μg/kg,定量限为0.001~2 μg/kg,平均回收率为90.3%~110.6%,日内、日间精密度均小于10%。该方法前处理简单快速,检测准确度和灵敏度高,可用于巴氏杀菌乳中9种香精成分的同时检测。

关 键 词:气相色谱-三重四极杆质谱  香精成分  巴氏杀菌乳  
收稿时间:2019-04-21

Simultaneous determination of nine flavor compounds in pasteurized milk by gas chromatography- triple quadrupole mass spectrometry
LIU Tong,WANG Yujiao,WANG Xiujuan,CUI Dongwei,ZHANG Feng.Simultaneous determination of nine flavor compounds in pasteurized milk by gas chromatography- triple quadrupole mass spectrometry[J].Chinese Journal of Chromatography,2019,37(11):1215-1220.
Authors:LIU Tong  WANG Yujiao  WANG Xiujuan  CUI Dongwei  ZHANG Feng
Institution:1. Institute of Food Safety, Chinese Academy of Inspection and Quarantine, Beijing 100176, China;2. College of Bioengineering, Tianjin University of Science and Technology, Tianjin 300000, China;3. School of Pharmacy, China Medical University, Shenyang 110122, China
Abstract: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 (R2) 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.
Keywords:gas chromatography-tandem mass spectrometry (GC-MS/MS)  flavor compounds  pasteurized milk  
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