高组胺鱼罐头中5种生物胺含量的LC-MS分析方法  

Determination of 5 Biogenic Amines in Canned Fish with High Histamine Content by LC-MS/MS

作　　者：杨清华[1] 史玉坤[1] 戴志英[1] 蔡秀丽[1] 施逸岚[1] 张卫兵[1] YANG Qinghua;SHI Yukun;DAI Zhiying;CAI Xiuli;SHI Yilan;ZHANG Weibing(Nantong Centers for Disease and Prevention,Nantong 226002)

机构地区：[1]南通市疾病预防控制中心,南通226002

出　　处：《食品工业》2022年第10期283-287,共5页The Food Industry

基　　金：南通市科技项目(JC2020111)。

摘　　要：建立高氯酸消解与三重四极杆串联液相色谱质谱仪(LC-MS/MS)联用检测鱼罐头中5种生物胺的含量。罐头中鱼肉样品粉碎后经5%高氯酸溶液进行消解提取,再由正己烷净化后进入LC-MS/MS分析。采用HILIC silica色谱柱进行分离,以含10 mmol/L甲酸铵的0.5%甲酸水溶液和0.5%甲酸的乙腈溶液为流动相进行梯度洗脱,电喷雾离子源正离子模式,多反应监测扫描,外标法定量。试验结果表明,在1.0~100μg/L范围内, 5种生物胺呈良好的线性关系,相关系数r均大于0.99,方法的检出限和定量限分别在0.31~4.1 mg/kg和1.0~13.6 mg/kg之间,基质效应在0.86~1.0之间。当样品加标质量分数为5.0, 50.0和100.0 mg/kg时,回收率和相对标准偏差(n=6)在76.0%~108%和2.89%~5.08%之间。与现有方法比较,该方法具有操作简单、灵敏度高、重现性好和有机试剂消耗少等优点,可以满足鱼罐头样品中生物胺的定性和定量分析。A perchloric acid digestion coupled with liquid chromatography mass spectrometer(LC-MS/MS) method for the determination of 5 biogenic amines in canned fish was established.The shattered fish meat from canned fish sample was extracted with 5% perchloric acid solution,and purified with n-hexane before being injected into the LC-MS/MS system.Hilic Silica column was used for separation,0.5% formic acid aqueous solution containing 10mmol/L ammonium formate and 0.5%formic acid acetonitrile solution were used as mobile phase for gradient elution,and the chromatographic peaks were detected by electrospray ionization(ESI) in the positive ion mode,using multiple reaction monitoring(MRM),and using external standard method of quantification.The results showed that there was a good linearity for 5 biogenic amines in the range of 1.0-100 μg/L with the correlation coefficient r more than 0.99.The detection limit and the quantitative limit of the method were 0.31-4.1 mg/kg and 1.0-13.6 mg/kg.The matrix efect rates of the method were 0.86-1.0.The recoveries of canned fish samples at the levels of 5.0,50.0 and 100.0 mg/kg were 76.0%-108%.Relative standard deviation(SRSD,n=6) were 2.89%-5.08%.Compared with the existing methods,the method had the advantages of simple operation,high sensitivity,good reproducibility and low consumption of organic reagents.The method was suitable for the confirmation and quantitive analysis of biogenic amines in the complex matrix of canned fish.

关 键 词：高氯酸 LC-MS/MS 鱼罐头 生物胺 

分 类 号：TS295.4[轻工技术与工程—农产品加工及贮藏工程] O657.63[轻工技术与工程—食品科学与工程]