基于UPLC-MS/MS测定烘焙咖啡豆中美拉德产物F3-A含量

Analysis of the Maillard reaction product F3-A of roasted coffee beans by UPLC-MS/MS

为建立超高效液质联用法(ultra-performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)检测烘焙咖啡豆中美拉德产物[5-(5,6-dihydro-4H-pyridin-3-ylidenemethyl)furan-2-yl]methanol(F3-A)含量的分析方法,并基于该方法检测不同烘焙模式下烘焙咖啡豆中F3-A含量,样品采用1 mol/L HCl溶液超声提取,MCX固相萃取小柱纯化,经Waters ACQUITY UPLC BEH C 18色谱柱分离后,在串联质谱负离子多反应监测模式下检测,外标法定量。结果表明,F3-A在10~2000μg/kg线性关系良好,决定系数达到0.999,加标回收率在85.7%~93.3%,相对标准偏差为2.56%~3.97%。烘焙咖啡豆样品检测显示,随烘焙程度增加,F3-A含量先升后降,其中轻度烘焙F3-A含量最高。咖啡豆品种、烘焙时间和温度是F3-A形成主要影响因素,F3-A形成最佳条件为:肯尼亚AA++咖啡豆200℃烘焙10 min,F3-A含量达到329.5μg/kg。

A ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method for the determination of maillard reaction product[5-(5,6-Dihydro-4H-pyridin-3-ylidenemethyl)furan-2-yl]methanol(F3-A)in roasted coffee beans was constructed,and the contents of F3-A in coffee beans roasted to different degrees were detected by using this method.The sample was extracted with 1 mol/L HCl in an ultrasonic bath,purified by MCX solid phase extraction column.The separation of F3-A was performed on a Waters ACQUITY UPLC BEH C 18 column(100 mm×2.1 mm,1.7μm),and determined in the positive MRM modes by MS/MS using external standard method.The method showed a good linearity over the range of 10-2000μg/kg with r 2=0.999.Recovery rates of F3-A were 85.7%-93.3%at three spiked levels in roasted coffee beans and the relative standard deviations were 2.56%-3.97%.The roasted coffee bean samples results showed that with increasing roasting degree,the formation of F3-A was found and the contents of F3-A first increased and then decreased,light roasting degree showed the maximum F3-A content.The types of coffee bean,the roasting temperature and the roasting time were the major factors in the formation of F3-A during roasting coffee beans,the optimum conditions for the formation of F3-A were Kenya++coffee beans roasted at 200℃for 10 min,and the content of F3-A was 329.5μg/kg.