高效液相色谱-串联质谱法测定果汁中恩镰孢菌素和白僵菌素  

Determination of enniatins and beauvericin in fruit juice by high performance liquid chromatography-tandem mass spectrometry

作　　者：邓涛 吉小凤[2] 肖英平[2] 汪雯[2] 吕文涛 王小骊[2] 吴振[1] 杨华[2] DENG Tao;JI Xiaofeng;XIAO Yingping;WANG Wen;LÜWentao;WANG Xiaoli;WU Zhen;YANG Hua(College of Food and Pharmaceutical Sciences,Ningbo University,Ningbo 315832,China;Institute of Agro-Product Safety and Nutrition,Zhejiang Academy of Agricultural Sciences,Hangzhou 310021,China)

机构地区：[1]宁波大学食品与药学学院,浙江宁波315832 [2]浙江省农业科学院农产品质量安全与营养研究所,浙江杭州310021

出　　处：《宁波大学学报（理工版）》2023年第6期50-56,共7页Journal of Ningbo University：Natural Science and Engineering Edition

基　　金：科技部国家重点研发计划政府间合作项目(2019YFE0103900).

摘　　要：建立高效液相色谱-串联质谱法测定果汁中恩镰孢菌素和白僵菌素检测方法.样品用V(乙腈):V(水):V(甲酸)混合液(79:20:1)提取,QuEChERS填料包(4 g无水MgSO_(4)、0.5 g无水CH_(3)COONa和0.5 g NaCl)盐析,100 mg C18净化,经过液相色谱柱分离,2 mmol·L^(-1)乙酸铵水溶液-甲醇为流动相梯度洗脱,由ESI源扫描,多反应监测模式,基质外标法定量分析.该方法中,恩镰孢菌素A(ENA)、恩镰孢菌素B(ENB)和白僵菌素(BEA)在0.1~200μg·L^(-1)以及恩镰孢菌素A1(ENA1)和恩镰孢菌素B1(ENB1)在1~200μg·L^(-1)范围内线性关系良好,且线性相关系数(R^(2))均大于0.9989,相对标准偏差范围为1.7%~11.7%.3个不同加标浓度的添加回收率为88.0%~114.1%,样品检测限为1.5μg·kg^(-1),样品定量限为5μg·kg^(-1).本文建立的方法简单、高效、准确,满足果汁中恩镰孢菌素和白僵菌素污染筛查需求.A high performance liquid chromatography-tandem mass spectrometry method was developed for the simultaneous determination of enniatins and beauvericin in fruit juices.Samples were extracted with V(acetonitrile):V(water):V(formic acid)mixture solution(79:20:1),salted out extraction by QuEChERS packed packages(4 g anhydrous MgSO_(4),0.5 g anhydrous CH_(3)COONa and 0.5 g NaCl),purified by 100 mg C18,and separated by liquid chromatography column with 2 mmol·L^(-1)ammonium acetate aqueous solution-methanol as mobile phase gradient elution.ESI positive ion mode scanning,multiple response monitoring mode detection,and matrix external standard method quantitative analysis were employed.The linearity was in the range of 0.1-200μg·L^(-1)for ENA、ENB and BEA,and the linearity was in the range of 1-200μg·L^(-1)for ENA1 and ENB1,with the correlation coefficients(R^(2))greater than 0.9989 and relative standard deviations ranging from 1.7%to 11.7%.The recoveries were ranged from 88.0%to 114.1%.The samples’limits of detection were 1.5μg·kg^(-1),and their limits of quantitation were 5μg·kg^(-1).The method established in this study is demonstrated as being simple,efficient,and accurate,which can satisfy the requirements of screening tests for enniatins and beauvericin in fruit juice samples.

关 键 词：果汁 恩镰孢菌素 白僵菌素 食品安全 

分 类 号：O675.63[理学—化学] TS201.6[轻工技术与工程—食品科学]