超高效液相色谱-串联质谱法测定果蔬汁类及其饮料中22种镰刀菌属毒素  

Determination of 22 kinds of Fusarium toxins in fruit and vegetable juices and beverages by ultra performance liquid chromatography-tandem mass spectrometry

作　　者：邵瑞婷 丁学妍 姜洁 SHAO Rui-Ting;DING Xue-Yan;JIANG Jie(Beijing Institute of Food Inspection and Research,National Key Laboratory of Market Regulation(Key Technologies of Major Comprehensive Guarantee of Food Safety),Beijing 100041,China)

机构地区：[1]北京市食品检验研究院,国家市场监管重点实验室(食品安全重大综合保障关键技术),北京100041

出　　处：《食品安全质量检测学报》2024年第9期167-177,共11页Journal of Food Safety and Quality

基　　金：国家市场监督管理总局科技创新人才计划(CXTD202307)。

摘　　要：目的建立果蔬汁类及其饮料中22种镰刀菌属毒素的超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)检测的分析方法。方法样品经水和乙腈提取,QuEChERS净化,氮吹至近干,1mL80%乙腈水(体积分数)复溶,采用WatersACQUITYUPLCCSH Phenyl-Hexyl反相色谱柱(100 mm×2.1 mm,1.7μm)梯度分离,以乙腈和0.1%甲酸水(2 mmol/L甲酸铵)为流动相进行梯度洗脱,UPLC-MS/MS在正、负离子模式下多反应监测,基质配制外标法定量。结果22种镰刀菌属毒素在线性范围内,线性关系良好,决定系数(R2)均大于等于0.985,回收率在60.1%~119.7%之间,相对标准偏差在2.64%~15.53%之间。结论该分析方法具有前处理方式简单、分析时间短、灵敏度好、准确度高、杂质干扰小等特点,可以用于果蔬汁类及其饮料中22种镰刀菌属毒素的检测。Objective To establish an analytical method for the detection of 22 kinds of Fusarium toxins in fruit and vegetable juices and their beverages using ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).Methods The sample was extracted with water and acetonitrile,purified by QuEChERS,blown to near dry with nitrogen,redissolved with 1 mL of 80%acetonitrile water(volume fraction),separated by gradient on Waters ACQUITY UPLC CSH Phynyl-Hexyl reverse phase chromatographic column(100 mm×2.1 mm,1.7µm),gradient eluted with acetonitrile and 0.1%formic acid water(2 mmol/L ammonium formate)as mobile phase,multi-reaction monitoring by UPLC-MS/MS in positive and negative ion modes,and matrix preparation external standard method quantitative.Results The 22 kinds of Fusarium toxins were within a linear range,with a good linear relationship.Coefficient of determination(R2)was greater than or equal to 0.985,and the recovery rates were between 60.1%and 119.7%.The relative standard deviations were between 2.64%and 15.53%.Conclusion This analysis method has the characteristics of simple pre-treatment,short analysis time,good sensitivity,high accuracy,and low impurity interference.It can be used for the detection of 22 kinds of Fusarium toxins in fruit and vegetable juices and their beverages.

关 键 词：果蔬汁类及其饮料 QuEChERS净化 超高效液相色谱-串联质谱法 镰刀菌属毒素 

分 类 号：O657.63[理学—分析化学] TS255.44[理学—化学]