UPLC-MS/MS同时测定固体饮料中9种甜味剂及筛查数据库的建立

Simultaneous Determination of 9 Sweetener in Solid Drinks by UPLC-MS/MS and the Establishment of Screening Database

为保障进出口食品安全,提升固体饮料中常用甜味剂的筛查效率,为口岸监管执法提供快速、准确的实验结果,保证贸易和供应顺畅,本研究建立了固体饮料中9种甜味剂的超高效液相色谱-串联质谱测定方法(UPLC-MS/MS)。试样经甲醇-水(1∶1,体积比)提取后,采用HLB固相萃取小柱净化,采用ACQUITY UPLC BEH C18柱(2.1×100mm,1.7μm)进行分离,多反应选择离子检测。本实验利用超高效液相串联质谱仪的动态多重反应监控模式,在同一分析时间下快速扫描完成9种甜味剂的筛选,针对疑似检出的阳性物质以触发式多重反应监控模式,得到二级质谱图,通过自建数据库的比对得到匹配相似度值以作为定性确认。方法学验证结果表明,所有化合物均得到良好的线性关系,标准曲线回归系数(r)均大于0.9995,回收率范围为72.4%~103.4%,精密度在0.8%~5.4%之间。本方法简单、快速、灵敏度高,并具有良好的精密度与准确度,能满足固体饮料中甜味剂测定的要求。

In order to ensure the safety of imported and exported food,improve the screening efficiency of commonly used sweeteners in solid drinks,provide rapid and accurate experimental results for port supervision and law enforcement,and ensure the smooth trade and supply,this study established an ultra-high performance liquid chromatography tandem mass spectrometry method for the determination of nine sweeteners in solid drinks.The samples were extracted by methanol-water(1∶1),purified by HLB solid-phase extraction column,separated by acquity UPLC BEH C18 column(2.1×100 mm,1.7μm),and detected by multi reaction selective ion.In this experiment,the dynamic multiple reaction monitoring mode of ultra-high performance liquid-phase tandem mass spectrometer was used to quickly scan nine sweeteners at the same analysis time.For the suspected positive substances,the trigger multiple reaction monitoring mode was used to obtain the secondary mass spectrum,and the matching similarity value was obtained through the comparison of self-built database for qualitative confirmation.The results of methodological validation showed that all the compounds had good linear relationship.The regression coefficient(R)of standard curve was more than 0.9995,the recovery range was 72.4%-103.4%,and the precision was between 0.8%~5.4%.The method is simple,rapid,sensitive,and has good precision and accuracy.It can meet the requirements of the determination of sweetener in solid drinks.