全自动固相萃取-超高效液相色谱-串联质谱法同时测定大米中香兰素、甲基香兰素、乙基香兰素、香豆素  

Simultaneous Determination of Vanillin,Methyl Vanillin,Ethyl Vanillin and Coumarin in Rice by Fully Automatic Solid Phase Extraction-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：张树权 周瑞铮 易华娟 林秋凤[1] 郑耀林 ZHANG Shuquan;ZHOU Ruizheng;YI Huajuan;LIN Qiufeng;ZHENG Yaolin(Dongguan Institutes for Food and Drug Control,Dongguan 523808,China)

机构地区：[1]东莞市食品药品检验所,广东东莞523808

出　　处：《现代食品》2022年第21期134-138,144,共6页Modern Food

基　　金：东莞市社会科学技术发展一般项目(2019507101508)。

摘　　要：建立全自动固相萃取-超高效液相色谱-串联质谱法同时测定大米中4种香精的分析方法。选用甲醇作为提取溶剂,经涡旋振荡和超声提取后,上清液加一级水稀释通过亲水亲脂平衡型固相萃取柱HLB净化,氮吹近干后补液过膜上机,使用Atlantis T3色谱柱分离,以甲醇-0.1%甲酸水为流动相。结果表明,4种香精在质量浓度为1~500 ng·mL^(-1)时线性关系良好,相关系数R均大于0.999,平均加标回收率在80.1%~89.3%,RSD为1.7%~3.9%。该方法具有前处理简便、自动化、检测速度快等优点,适用于大米的批量检测。A method for the simultaneous determination of four essence in rice by automatic solid phase extraction ultra performance liquid chromatography tandem mass spectrometry was established.Methanol was selected as the extraction solvent.After vortex oscillation and ultrasonic extraction,the supernatant was diluted with primary water and purified by the hydrophilic lipophilic equilibrium solid phase extraction column HLB.After nitrogen blowing was nearly dry,the solution was added to the membrane and put on the machine.Atlantis T3 chromatographic column was used for separation.Methanol-0.1%formic acid water was used as the mobile phase.The results showed that when the mass concentration of the four essence was 1~500 ng·mL^(-1),the linear relationship was good,and the correlation coefficient R was greater than 0.999.The average recovery rate of spiking was 80.1%~89.3%,and the RSD was 1.7%~3.9%.This method has the advantages of simple pretreatment,automation and fast detection speed,and is suitable for batch detection of rice.

关 键 词：香兰素 甲基香兰素 乙基香兰素 香豆素 大米 全自动固相萃取 超高效液相色谱-串联质谱法 

分 类 号：O657.7[理学—分析化学]