氨基酸分析仪法测定动物性水产品中8种生物胺含量  

Quantification of eight biogenic amines in aquatic animal products with amino acid analyzer

作　　者：冯洪燕 夏永生 钱亮亮 陈小娟 周静 FENG Hongyan;XIA Yongsheng;QIAN Liangliang;CHEN Xiaojuan;ZHOU Jing(Lianyungang Comprehensive Inspection and Testing Center for Quality and Technology,Lianyungang,Jiangsu 222000,China;Seafood Quality Supervision and Inspection Center of Jiangsu Province,Lianyungang,Jiangsu 222000,China)

机构地区：[1]连云港市质量技术综合检验检测中心,江苏连云港222000 [2]江苏省海洋食品质量监督检验中心,江苏连云港222000

出　　处：《食品与机械》2025年第2期65-71,共7页Food and Machinery

基　　金：江苏省市场监管局科技计划项目(编号:KJ21125123,KJ2023065)。

摘　　要：[目的]解决传统色谱法在测定生物胺时所面临的繁琐手动柱前衍生步骤以及衍生物稳定性差的问题,以提升检测的效率和准确性。[方法]利用氨基酸分析仪测定动物性水产品中8种生物胺(腐胺、组胺、尸胺、亚精胺、章鱼胺、精胺、酪胺、苯乙胺)含量。动物性水产品试样经磺基水杨酸溶液提取,高速冷冻离心,钾盐缓冲液洗脱,钾离子型磺酸基强酸性阳离子交换色谱柱分离,130℃下茚三酮在线衍生,570 nm波长检测,8种生物胺采用外标法定量。[结果]8种生物胺线性范围为1.0~50.0 mg/L,相关系数R~2>0.9947,检出限为2.5~5.0 mg/kg、定量限为8.3~16.7 mg/kg,3种基质加标回收率为62.2%~119.2%,衍生条件和设备稳定性良好(峰面积RSD为0.43%~3.89%,保留时间RSD为0.050%~0.334%),有证质控样品考察结果为满意。[结论]该方法具有良好的稳定性、灵敏度、回收率和准确度,快速简便,适用于动物性水产品中8种生物胺含量的检测。[Objective]To address the cumbersome manual pre-column derivatization steps and poor derivative stability encountered in traditional chromatography when determining biogenic amines,so as to improve the efficiency and accuracy of detection.[Methods]In this study,an amino acid analyzer method is established for the simultaneous determination of eight biogenic amines(i.e.,putrescine,histamine,cadaverine,spermidine,octopamine,spermine,tyramine,and phenylethylamine)in aquatic animal products.The aquatic animal product samples are extracted using a sulfosalicylic acid solution,which is followed by high-speed refrigerated centrifugation,elution with potassium salt buffer,separation using a potassium ionic sulfonic acid based strong acid cation exchange chromatographic column,online derivatization with ninhydrin at 130℃,and detection at 570 nm.[Results]The linear ranges for the eight biogenic amines are 1.0~50.0 mg/L with correlation coefficients(R2)greater than 0.9947.The limits of detection range from 2.5 to 5.0 mg/kg,and the limits of quantification range from 8.3 to 16.7 mg/kg.The spike recovery rates for the three matrices range from 62.2%to 119.2%.The derivatization conditions and equipment stability are satisfactory,with relative standard deviations(RSD)of peak areas ranging from 0.43%to 3.89%and RSD of retention time ranging from 0.050%to 0.334%.[Conclusion]This developed method exhibits excellent stability,sensitivity,recovery,and accuracy.It is a rapid and simple approach for the detection of the eight biogenic amines in aquatic animal products.

关 键 词：氨基酸分析仪 生物胺 茚三酮 在线柱后衍生 水产品 

分 类 号：TS2[轻工技术与工程—食品科学与工程]