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 extrac-tion-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5~1000 μg·L-1范围线性良好,相关系数R2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。
Determination of artificial flavours in wine by solid phase supported liquid-liquid extraction-gas chromatography-triple quadrupole tandem mass spectrometry
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 quadru-pole 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 mmx0.25 μm),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 5.00~1000 μg·L-1 there are good correlation coefficients(R2≥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 de-viations(RSDs)are in the range of 1.7%and 7.3%(n=6).
artificial food flavourwinesolid supported liquid-liquid extractiongas chromatography-triple quadrupole tandem mass spectrometry