摘要
目的:为生物胺形成机制的研究和食品安全风险评估提供新的技术思路。方法:建立液相色谱-三重四极杆串联质谱同时检测奶酪中酪胺、2-苯乙胺、色胺、章鱼胺和尸胺的测定方法。采用超声辅助溶剂萃取生物胺,HILIC色谱柱分离,三重四极杆质谱正离子多反应监测模式进行测定,内标法定量;研究提取溶剂种类、超声时间选择和基质效应对峰面积的影响,进行方法学验证和评估。结果:以0.1%甲酸-乙腈-水溶液为提取溶剂,超声提取15 min,生物胺无需衍生化处理,以乙酸铵(甲酸调pH值为4)-乙腈为流动相,HPLC-MS/MS直接测定。5种生物胺的加标回收率为78.6%~113.8%,相对标准偏差为2.41%~7.12%(n=3);色胺、苯乙胺、酪胺和章鱼胺的检出限为0.75μg/kg,定量限为2.5μg/kg;尸胺的检出限为1.5μg/kg,定量限为5.0μg/kg;在各自线性范围内线性关系良好,相关系数均大于0.99。对市售奶酪样品进行测定,不同样品中不同的生物胺含量差异较大,含量范围为4.45~2863.00μg/kg,均在安全范围内。结论:试验所建方法适合奶酪中5种生物胺含量的快速检测。
Objective:A new technical idea was provided for the study of biogenic amine formation mechanism and food safety risk assessment.Methods:An analytical method was established for determination of tyramine,phenylethylamine,tryptamine,octopamine and cadaverine in cheeses with high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).Biogenic amines were extracted by ultrasonic-assisted solvent extraction from cheeses,and were separated by HILIC column,determined by positive electrospray ionization(ESI)with multiple reaction monitoring(MRM)mode,quantified by the internal standard method.The effect of extraction solvent type,ultrasonic time and matrix effect on the peak area was studied,and the performance of the method was validated and evaluated.Results:Using 0.1%formic acid(acetonitrile/water)as the extraction solvent,the samples were extracted by ultrasound for 15 min.Ammonium acetate of 5 mmol/L(pH value was adjusted to 4 by formic acid)and acetonitrile were used as the mobile phase,biogenic amines without derivatization were detected by HPLC-MS/MS.The recoveries of 5 biogenic amines were 78.6%~113.8%and relative standard deviations were 2.41%~7.12%at three spiked levels.The limit of detection of tryptamine,phenylethylamine,tyramine and octopamine was 0.75μg/kg and the limit of quantification was 2.5μg/kg;The limit of detection of cadaverine was 1.50μg/kg and the limit of quantification was 5.0μg/kg.The linear relationship was good in the respective linear ranges,and the correlation coefficient was greater than 0.99.The method was used for the determination of commercially available cheese samples.The contents of different biogenic amines in different samples varied greatly,ranging from 4.45 to 2863.00μg/kg,which was within the safe range.Conclusion:The proposed method was suitable for fast determination of 5 kinds of biogenic amines in cheese.
作者
张慧
曹慧
王瑾
肖功年
姜侃
ZHANG Hui;CAO Hui;WANG Jin;XIAO Gongnian;JIANG Kan(School of Biological and Chemical Engineering,ZheJiang University of Science&Technology,Hangzhou,Zhejiang 310023,China;Zhejiang Institute of Product Quality and Safety Science,Hangzhou,Zhejiang 310018,China)
出处
《食品与机械》
CSCD
北大核心
2023年第10期80-86,共7页
Food and Machinery
基金
浙江省基础公益研究计划项目(编号:LGN20C200011)。
关键词
液相色谱-三重四极杆串联质谱法
非衍生化
奶酪
生物胺
检测
high performance liquid chromatography-tandem mass spectrometry
without derivatization
cheese
biogenic amines
determination
