摘要
为快速检测水产品中精胺、亚精胺、腐胺、尸胺、组胺、色胺、章鱼胺、酪胺、2-苯乙胺9种生物胺含量,本研究以小黄花鱼为基质,优化了流动相组成和样品提取溶剂,建立了超高效液相色谱-串联三重四极杆质谱同时检测方法。样品经0.1%三氯乙酸水溶液重复提取两遍,合并上清液过0.22μm聚四氟乙烯滤膜。以HSS T3为色谱柱,流动相A为0.1%甲酸乙腈,流动相B为10 mmol/L甲酸铵水溶液含0.2%甲酸,在电喷雾正离子电离、多反应监测模式下,9种生物胺在4 min内得到分离。根据响应强度不同,9种生物胺分成酪胺、2-苯乙胺,腐胺、尸胺、组胺、色胺、章鱼胺,精胺、亚精胺三组,以1:5:25浓度比配制多浓度混合标准中间液。该方法对三组生物胺的线性范围分别为1~40 ng/mL、5~200 ng/mL和25~1000 ng/mL;方法定量限依次为0.01、0.05和0.25 mg/kg。低、中、高三个浓度水平加标回收率分别为81.7%~111.2%、80.0%~110.3%、80.0%~99.0%;精密度(n=6)依次为1.7%~7.3%、1.3%~9.1%、0.7%~4.6%。总体而言,该方法简便、快速,具有良好的灵敏度、回收率和精密度,适用于小黄花鱼中生物胺的测定。
To rapidly determine 9 biogenic amines including spermine,spermidine,putrescine,cadaverine,histamine,tryptamine,octopamine,tyramine andβ-phenethylamine in aquatic products,the ultra high-performance liquid chromatographytandem mass spectrometry method was established with Larimichthys polyactis using as matrix sample,and mobile phase and extract solvents were optimized.Matrix sample was extracted by 0.1%trichloroacetic acid(TCA)in duplicate,the supernatant was combined and filtered by 0.22μm PTFE filters,and separated by HSS T3 column in 4 min.The mobile phase A was acetonitrile containing 0.1%formic acid,while mobile phase B was 10 mmol/L ammonium formate containing0.2%formic acid.Nine biogenic amines were divided into three groups based on their different response intensity,with a concentration range of 1 to 40 ng/mL(tyramine andβ-phenethylamine),5 to 200 ng/mL(putrescine,cadaverine,histamine,tryptamine and octopamine),and 25 to 1000 ng/mL(spermine and spermidine).Their method quantification limits(LOQs)were 0.01,0.05 and 0.25 mg/kg,respectively.The recovery rate of low,medium and high concentrations was 81.7%~111.2%,80.0%~110.3%and 80.0%~99.0%,respectively,with the corresponding degree of precision(n=6)of 1.7%~7.3%,1.3%~9.1%and 0.7%~4.6%.This method is simple,fast and with good sensitivity,recovery and precision,which is suitable for the determination of biogenic amines in Larimichthys polyactis.
作者
罗振玲
高海波
杨挺
付余
LUO Zhenling;GAO Haibo;YANG Ting;FU Yu(Taizhou Food Inspection Centre,Taizhou 318100,China;College of Food Science,Southwest University,Chongqing 400715,China)
出处
《食品工业科技》
CAS
北大核心
2023年第5期251-257,共7页
Science and Technology of Food Industry
基金
台州市科技计划项目(20ny06)。
关键词
生物胺
超高效液相色谱-串联质谱
小黄花鱼
biogenic amines
ultra high-performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS)
Larimichthys polyactis
