液相色谱-串联质谱法测定葡萄酒中7种生物胺含量  

LC-MS/MS Determination of 7 Bio-amines in the Grape

作　　者：孙骥[1] 施瑛[2] 陈树兵[1] 房科腾[1] 贺小雨[1] 章再婷[1] 

机构地区：[1]宁波出入境检验检疫局技术中心,宁波315012 [2]南京农业大学理学院,南京225001

出　　处：《理化检验（化学分册）》2013年第6期697-700,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：国家质检总局科技计划项目(2009IK172)

摘　　要：提出了液相色谱-串联质谱法测定葡萄酒中2-苯乙胺、色胺、尸胺、组胺、腐胺、精胺、亚精胺等7种生物胺含量的方法。样品经0.45μm滤膜过滤后,直接通过Zorbax Eclipse XDB C8色谱柱(4.6mm×150mm,5μm)进行分离,以不同体积5mmol·L-1乙酸铵-10mmol·L-1全氟己酸甲醇溶液(A)和5mmol·L-1乙酸铵-10mmol·L-1全氟己酸水溶液(B)的混合液为流动相梯度洗脱,串联质谱法进行测定。7种生物胺的质量浓度均在0.1～5.0mg·L-1范围内与其峰面积呈线性关系,检出限(3S/N)在0.005～0.02mg·L-1之间。以空白葡萄酒样品为基体进行加标回收试验,测得回收率在84.1%～97.5%之间;测定值的相对标准偏差(n=5)在6.3%～13%之间。A method of LC-MS/MS for the determination of 7 bio-amines,including 2-phenylethylamine,tryptamine,cadaverine,histamine,putrescine,spermine and spermidine,in the grape was proposed.The sample was filtered on 0.45 μm filtering membrane,the filtrate obtained was taken for separation on Zorbax Eclipse XDB C8（4.6 mm×150 mm,5 μm） column,using mixtures of A（methanol solution containing 5 mmol·L-1 ammonium acetate and 10 mmol·L-1 perfluorohexanoic acid） and B（water solution containing ammonium acetate and perfluorohexanoic acid of same concentrations as in A） in various ratios as mobile phase in the gradient elution.Linear relationships between values of peak area and mass concentration of the 7 bio-amines were kept in the same range of 0.1-5.0 mg·L-1,with detection limit（3S/N） in the range of 0.005-0.02 mg·L-1.Tests for recovery and precision were made by addition of standard solution of the 7 bio-amines to blank samples of the grape which was then analyzed by the proposed method.Values of recovery and RSD′s（n=5） obtained were in the ranges of 84.1%-97.5% and 6.3%-13% respectively.

关 键 词：液相色谱-串联质谱法 葡萄酒 生物胺 

分 类 号：O657.63[理学—分析化学]