摘要
目的建立发酵饮品中8种生物胺的柱前衍生-反相高效液相色谱测定方法。方法样品经酸化超声提取后,以饱和碳酸氢钠溶液为缓冲液,丹磺酰氯为衍生剂,调节p H值,于恒温水浴箱中反应,加入乙醚萃取,氮吹挥干后以初始流动相定容,反相高效液相色谱法测定。结果建立了最优衍生条件及色谱条件,8种生物胺在35 min内得到很好的分离,在0.20 mg/L^50 mg/L线性关系良好,相关系数>0.997 9,检出限:色胺为0.52 mg/L,苯乙胺为0.17 mg/L,腐胺为0.11 mg/L,尸胺为0.10 mg/L,组胺为0.75 mg/L,酪胺为0.32 mg/L,亚精胺为0.18 mg/L,精胺为0.21 mg/L。加标回收率在86.5%~103.0%,相对标准偏差为0.90%~2.95%,符合方法学要求。结论本方法操作简便、结果准确、实用性强,能够满足发酵饮品中8种生物胺的检测。
Objective To establish a method for the simultaneous determination of 8 biogenic amines in fermented drinks by reversed phase high performance liquid chromatography with precolumn derivatization. Methods The acidized samples were extracted by ultrasound,reacted in constant temperature water bath,with saturated sodium bicarbonate solution as buffer. The p H value was adjusted,and dansyl chloride was used as the derivatization reagent,then the samples was extracted by ether and dried by nitrogen. The residue was dissolved with the initial mobile phase,the biogenic amines in fermented drinks were separated on a high performance liquid chromatography instrument. Results Eight kinds of biogenic amines were separated well in 35 mins with optimal derivatization conditions and chromatographic conditions,showing good linearity in the range of 0. 20 mg/L-50 mg/L,with correlation coefficient 0. 997 9,and the detection limits of tryptamine,phenyl ethylamine,putrescine,cadaverine,histamine,tyrosamine,spermidine,spermine were 0. 52 mg/L,0. 17 mg/L,0. 11 mg/L,0. 10 mg/L,0. 75 mg/L,0. 32 mg/L,0. 18 mg/L,0. 21 mg/L. The recoveries were within 86. 5%-103. 0% and the relative standard deviation（ RSD）were within 0. 90%-2. 95%. Conclusion The method has the advantages of simple operation,accurate result and strong practicability,and can meet the detection of eight biogenic amines in the fermented beverage.
作者
张来颖
于秋红
张志荣
刘裕婷
王玉江
信振江
ZHANG Lai-ying;YU Qui-hong;ZHANG Zhi-rong;LIU Yu-ting;WANG Yu-jiang;XIN Zhen-jiang(Fengtai District Center for Disease Control and Prevention,Beijing 100071,China)
出处
《中国卫生检验杂志》
CAS
2018年第17期2057-2059,2063,共4页
Chinese Journal of Health Laboratory Technology
基金
北京市丰台区FETP骨干人才项目(丰台组织部)
关键词
生物胺
高效液相色谱法
柱前衍生
发酵饮品
Biogenic amines
High performance liquid chromatography
Precolumn derivatization
Fermented drinks
