超高效液相色谱-串联质谱法测定鲣鱼中的生物胺  

The detection of biogenic amines in skipjack tuna by using the ultrahigh performance liquid chromatography-tandem mass spectrometry method

作　　者：刘洋帆 李绪鹏 冯阳 王迪[2,4] 陈胜军[2,4] 杨贤庆[2,4] 吴燕燕 邓建朝[2,4] LIU Yangfan;LI Xupeng;FENG Yang;WANG Di;CHEN Shengjun;YANG Xianqing;WU Yanyan;DENG Jianchao(College of Food Science and Technology,Shanghai Ocean University,Shanghai 201306,China;Key Laboratory of Aquatic Product Processing,Ministry of Agriculture and Rural Affairs,South China Sea Fisheries Research Institute,Chinese Academy of Fishery Sciences,Guangzhou 510300,China;Guangdong Agricultural Technology Extension Center,Guangzhou 510300,China;Collaborative Innovation Center of Seafood Deep Processing,Dalian Polytechnic University,Dalian 116034,China)

机构地区：[1]上海海洋大学食品学院,上海201306 [2]中国水产科学研究院南海水产研究所,国家水产品加工技术研发中心,农业农村部水产品加工重点实验室,广东广州510300 [3]广东省农业技术推广中心,广东广州510300 [4]大连工业大学,海洋食品精深加工关键技术省部共建协同创新中心,辽宁大连116034

出　　处：《食品与发酵工业》2022年第20期225-230,共6页Food and Fermentation Industries

基　　金：广东省重点领域研发计划资助(2020B1111030004);国家重点研发计划(2017YFC1600706,2018YFF0213605);中国水产科学研究院南海水产研究所中央级公益性科研院所基本科研业务费(2020TS05);财政部和农业农村部财政专项(NFZX2021);国家现代农业产业技术体系资助(CARS-47);广东省现代农业产业技术体系创新团队建设专项资金(2021KJ151);海水产品品质评价与调控创新团队项目(2020TD73)。

摘　　要：建立了鲣鱼中精胺、亚精胺、酪胺、色胺、组胺、β-苯乙胺、腐胺、尸胺8种生物胺的超高效液相色谱-串联质谱(ultrahigh performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)方法。样品依次使用0.2%(体积分数)酸化乙腈和二氯甲烷提取除杂,随后经C18色谱柱进行分离,采用甲醇和0.5%(体积分数)甲酸水溶液作为流动相进行梯度洗脱,通过电喷雾正离子(electrospray ionization,ESI+)扫描,在多反应监测(multiple reaction monitoring,MRM)模式下获得质谱数据,并采用内标法进行定量分析。结果表明,8种生物胺可在6 min内分离,且在各自浓度范围内线性良好,相关性系数R为0.9956~0.9996,检出限为75~150μg/kg,定量限为250~500μg/kg,样品平均回收率为82%~113%,相对标准偏差为2.3%~9.7%。该方法简单、快速,具有良好的灵敏度、回收率和精密度,适用于鲣鱼中生物胺的测定。This study established a detection method for spermine,spermidine,tyramine,tryptamine,histamine,β-phenylethylamine,putrescine and cadaverine for 8 kinds of biogenic amines by utilizing ultrahigh performance liquid chromatography-tandem mass spectrometry method(UPLC-MS/MS).The sample was extracted and decontaminated by 0.2%acidified acetonitrile and dichloromethane separately,and then separated using a C18 column.Methanol and 0.5%formic acid in water were used as the mobile phase for gradient elution.Mass spectrometry data were obtained by electrospray positive ion(ESI+)scanning in multiple reaction monitoring(MRM)mode,and an internal standard method was used for quantification.Results showed that 8 kinds of biogenic amines could be separated within 6 minutes,and the linearity was good with the correlation coefficient R between 0.9956 and 0.9996.The detection limit was in the range of 75-150μg/kg and the quantification limit was in the range of 250-500μg/kg.Moreover,the average recovery rate of the sample was between 82%-113%and the relative standard deviation was between 2.3%and 9.7%.This method developed here was simple,fast,and had good sensitivity,recovery,and precision,which was suitable for the determination of biogenic amines in skipjack tuna.

关 键 词：鲣鱼 生物胺 超高效液相色谱-串联质谱 

分 类 号：O657.63[理学—分析化学] TS254.7[理学—化学]