全自动固相萃取结合UPLC-MS/MS同时测定蜂蜜中26种内源性组分  

Simultaneous Determination of 26 Endogenous Components in Honey by Automated Solid Phase Extraction Coupled with Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：李静 张居舟 刘毅 余晓娟 王欣 LI Jing;ZHANG Juzhou;LIU Yi;YU Xiaojuan;WANG Xin(China National Center for Quality Supervision and Test of Agricultural-Avocation Processed Food,Anhui Provincial Institute for Food and Drug Control,Hefei 230051,China)

机构地区：[1]安徽省食品药品检验研究院,国家农副加工食品质量监督检验中心,安徽合肥230051

出　　处：《食品科学》2023年第10期265-272,共8页Food Science

基　　金：“十三五”国家重点研发计划重点专项(2017YFC1601705);安徽省重点研究与开发计划项目(202004a07020024)。

摘　　要：采用全自动固相萃取-超高效液相色谱-串联质谱(ultra-high performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)法同时测定荆条蜜、油菜蜜、洋槐蜜中脱落酸、酚酸和黄酮类等26种内源性组分。样品用磷酸盐缓冲溶液提取,经HLB固相萃取柱净化,用Agilent Eclipse Plus RRHD C_(18)柱(2.1 mm×100 mm,1.8μm)分离,以0.03%甲酸溶液-乙腈为流动相进行梯度洗脱。在电喷雾离子源负离子模式下,结合动态多反应监测模式,外标法定量。26种待测组分在各自的质量浓度范围内均呈良好线性关系,相关系数(r^(2))均大于0.996,检出限和定量限范围分别为1.0~10.0μg/kg和2.5~25.0μg/kg,在各加标水平,平均回收率为81.9%~101%,相对标准偏差为3.4%~9.8%。UPLC-MS/MS是一种高效、快捷、精准的内源性组分含量的定量分析方法,可为蜂蜜品质控制和鉴别提供技术支持。An automated solid phase extraction coupled with ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method was developed for the determination of 26 endogenous components in chaste,acacia and rape honey.The samples were extracted with phosphate buffer solution,purified by solid-phase extraction using an Oasis HLB cartridge,and separated on an Agilent Eclipse Plus RRHD C_(18) column(2.1 mm×100 mm,1.8μm)by gradient elution using a mobile phase comprising of 0.03% formic acid in water and acetonitrile.The analytes were detected by using an electrospray ion source in the negative ion mode with dynamic multiple reaction monitoring(dMRM),and quantified by an external standard method.Results showed that good linear relationships were obtained for the 26 analytes in their respective concentration ranges with correlation coefficients(r^(2))greater than 0.996.The limits of detection(LOD)and quantitation(LOQ)ranged from 1.0 to 10.0 and 2.5 to 25.0μg/kg,respectively.The average recoveries from spiked samples were between 81.9% and 101%,with relative standard deviations(RSD)of 3.4%-9.8%.The UPLC-MS/MS method has the advantages of rapidity as well as high efficiency and accuracy,which can provide technical support for the quality control and identification of honey.

关 键 词：超高效液相色谱-串联质谱法 荆条蜜 油菜蜜 洋槐蜜 脱落酸 酚酸 黄酮类 内源性组分 

分 类 号：O657.7[理学—分析化学] TS207.3[理学—化学]