摘要
建立了固相支撑液液萃取-气相色谱-三重四极杆串联质谱法(solid phase supported liquid-liquid extraction-gas chromatography-triple quadrupole tandem mass spectrometry,SLE-GC-MS/MS)检测酒中人造食品香料环己基丙酸烯丙酯、乙基麦芽酚、反式杨梅醛、顺式杨梅醛、乙基香兰素含量的方法。样品经过硅藻土固相柱支撑液液萃取(SLE)净化,乙酸乙酯洗脱定容后,采用ZB-1701石英毛细管柱分离,多反应监测模式(MRM)检测,以保留时间和离子对定性,定量离子峰面积外标法定量。结果表明:5种人造食品香料在15 min内完成色谱分离,在5~1000μg·L^(-1)范围线性良好,相关系数R^(2)均大于0.99,检出限和定量限分别为1.2~3.0μg·kg^(-1)和4.0~10.0μg·kg^(-1),以三种阴性样品为基质,在不同添加水平下,5种人造食品香料平均回收率为85.7%~99.8%,相对标准偏差(RSD,n=6)在1.7%~7.3%之间。
a method for simultaneous determination of five kinds artificial flavours included(ethyl maltol、allylcyclxylpropionate、trans strawberry、cis strawberry、ethyl vanillin)in wine by solid supported liquid-liquid extraction-gas chromatography-triple quadrupole tandem mass spectrometry was established.The sample was purified by diatomite solid-phase column supported liquid-liquid extraction(SLE),eluted by ethyl acetate.separated with ZB-1701 capillary column(30 m×0.25 mm×0.25μm),The retention time and multiple reaction monitoring(MRM)ion pairs were used for qualitative analysis and peak area was used for quantification.The method showed that fieve kinds artificial flavours can be separated competely in fifteen minutes,in the range of 5.00~1000μg·L^(-1)there are good correlation coefficients(R^(2)≥0.99),The limits of determination(LODs)are 1.2~3.0μg·kg^(-1)and the limits of quantitation(LOQs)are 4.0~10.0μg·kg^(-1).The recoveries at three standards are 85.7%~99.8%,and the relative standard deviations(RSDs)are in the range of 1.7%and 7.3%(n=6).
作者
胡朝阳
林松
黄永辉
潘城
黄何何
林茂发
HU Chao-yang;LIN Song;HUANG Yong-hui;PAN Cheng;HUANG He-he;LIN Mao-fa(FuJian Inspection and Research Institute for Product Quality,Fuzhou 350015,China)
出处
《化学研究与应用》
北大核心
2025年第1期64-72,共9页
Chemical Research and Application
基金
福建省产品质量检验研究院科技项目(KY202324A)资助。
关键词
人造食品香料
酒
固相支撑液液萃取
气相色谱-三重四极杆串联质谱法
artificial food flavour
wine
solid supported liquid-liquid extraction
gas chromatography-triple quadrupole tandem mass spectrometry
作者简介
通信联系人:林茂发(1974-),男,高级工程师,主要从事食品安全分析。Email:lmf938@163.com。