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

Simultaneous determination of nine flavor compounds in pasteurized milk by gas chromatography- triple quadrupole mass spectrometry

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0.22μm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1~200μg/L范围内呈良好线性,线性相关系数(R^2)均大于0.997,方法的检出限为0.002~0.1μg/kg,定量限为0.001~2μg/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。

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 1-200μg/L were observed for the nine flavor compounds.The linear correlation coefficients(R^2)were greater than 0.997.The limits of detection and limits of quantification were 0.002-0.1μg/kg and 0.001-2μg/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.