高效液相色谱-四极杆/静电场轨道阱高分辨质谱检测葡萄酒中8种生物胺  

Determination of Eight Biogenic Amines in Red Wines by Liquid Chromatography-Quadrupole/Electrostatic Field Orbit Trap Mass Spectrometry

作　　者：丁涛[1] 吕辰[2] 柳菡[1] 郭玲[1] 吴斌[1] 陈国松[2] 沈崇钰[1] 张睿[1] 费晓庆[1] 张晓燕[1] 庾金良[2] 

机构地区：[1]江苏出入境检验检疫局食品实验室,江苏南京210001 [2]南京工业大学理学院,江苏南京211816

出　　处：《分析测试学报》2014年第1期27-32,共6页Journal of Instrumental Analysis

基　　金：江苏省局项目(2012KJ31)

摘　　要：利用分散固相萃取结合高效液相色谱-四极杆/静电场轨道阱高分辨质谱对进出口葡萄酒中组胺、酪胺、尸胺、腐胺、色胺、精胺、亚精胺和苯乙胺8种生物胺进行分析.葡萄酒样品用去离子水稀释,加入200 mg十八烷基硅烷粉（Octadecylsilyl,ODS）和50 mg N-丙基乙二胺粉（Primary secondary amine,PSA）吸附剂分散固相萃取净化后,以高效液相色谱-四极杆/静电场轨道阱高分辨质谱进行定性和定量分析.选择Phe-nomenex C18（100 mm ×4.6 mm ×2.6 μm）分析柱,乙腈-0.1‰七氟正丁酸水溶液作为流动相进行梯度洗脱分离.质谱采用正离子模式,通过高分辨质谱全扫描模式提取目标化合物精确质量数,利用阈值自动触发全扫描二级质谱功能提高了定性的准确性.8种生物胺在0.2～10.0 mg/L浓度范围内线性关系良好,相关系数均大于0.99.方法的定量下限可达1.0 mg/L.在1.0、5.0、10.0 mg/L 3个浓度加标水平下,葡萄酒中8种生物胺的平均回收率为83.7％～101.6％,相对标准偏差（RSDs）为3.1％～12.9％.此方法准确灵敏且前处理简单,可作为葡萄酒中生物胺筛选和确认的检测方法.A method for the determination of histamine,tyramine,cadaverine,putrescine,tryptamine,spermine,spermidine and phenylethylamine in wines by liquid chromatography-quadrupole/electrostatic field orbit trap mass spectrometry was developed.The samples were diluted with deionized water,followed by dispersive solid phase extraction （DSPE） clean-up procedure with 200 mg octadecylsilyl （ODS） and 50 mg primary secondary amine（PSA）.Chromatographic separation was performed on a Phenomenex C18 （100 mm × 4.6 mm × 2.6 μm） column with acetonitrile-0.1％o heptafluorobutyric acid（HFBA） solution as mobile phase by gradient elution.Eight biogenic amines were analyzed in positive mode with ESI interface by quadrurpole/electrostatic field orbit trap high-resolution mass spectrometry.Accurate mass extraction for the target analytes and two-stage threshold-triggered mass improved the accuracy during the analysis.The linearities of 8 biogenic amines ranged from 0.2 mg/L to 10.0 mg/L with correlation coefficients more than 0.99.The limits of quantitation for 8 biogenic amines were all 1.0 mg/L.The average recoveries at three spiked levels（1.0,5.0 and 10.0 mg/L） were between 83.7％ and 101.6％ with relative standard deviations（RSDs） not more than 12.9％.The developed method was simple and sensitive,and could be applied as a screen and confirmatory method for the analysis of biogenic amines in red wines.

关 键 词：生物胺 分散固相萃取 葡萄酒 静电场轨道阱高分辨质谱 

分 类 号：O657.63[理学—分析化学] O623.732[理学—化学]