高效液相色谱法测定白酒中6种生物胺的含量  

Determination of Six Biogenic Amines in Light Flavor and Luzhou Flavor Baijiu by High Performance Liquid Chromatography

作　　者：董孝元 冯小进 李斯琳 陈周 刘占奇 李俊薇 DONG Xiaoyuan;FENG Xiaojin;LI Silin;CHEN Zhou;LIU Zhanqi;LI Junwei(Huanghelou Distillery(Xianning)Co.,Ltd.,Wuhan 430070,Hubei,China])

机构地区：[1]黄鹤楼酒业(咸宁)有限公司,湖北武汉430070 [2]武汉雅仕博科技有限公司,湖北武汉430070

出　　处：《酿酒》2023年第3期106-109,共4页Liquor Making

摘　　要：建立了采用高效液相快速准确的检测白酒中6种生物胺(腐胺、亚精胺、精胺、色胺、盐酸吡哆胺、对羟基苯乙胺)含量的方法。此方法特征在于采用正丁醇-二氯甲烷萃取酒样,并优化了萃取步骤,保证萃取效率最高及各样品萃取效率一致。以丹磺酰氯作为衍生剂,衍生条件为60℃、30 min、2 mL衍生剂(浓度为10 mg/mL),采用Agilent Polaris C18-A色谱柱(4.6 mm×250 mm,5μm)分离,以乙腈和水作为流动相A和B,采用梯度洗脱,洗脱程序如表1,流速为1 mL/min,柱温为35℃,检测波长为254 nm。6种生物胺如表2所示浓度范围内具有良好的线性关系(R2>98.643%),6种生物胺的检出限0.04~0.09 mg/L,定量限0.10~0.32,选取3.000 mg/L、5.000 mg/L 2个水平加标,平均加标回收率为92.20%~108.86%。A rapid and accurate method for the determination of six kinds of biogenic amines(putrescine,spermidine,spermine,tryptamine,pyridoxamine hydrochloride,and p-hydroxyphenylethylamine)in Baijiu was established by HPLC.This method is characterized in that n-butanol dichloromethane is used to extract wine samples,and the extraction steps are optimized to ensure the highest extraction efficiency and the same extraction efficiency of each sample.Take dansyl chloride as the derivatization agent,and the derivatization conditions are 60℃,30min,2mL of derivatization agent(the concentration is 10mg/mL).The Agilent Polaris C18-A chromatographic column(4.6mm×250mm,5μm)Separation:acetonitrile and water are used as mobile phases A and B,and gradient elution is adopted.The elution procedure is shown in Table 1.The flow rate is 1mL/min,the column temperature is 35℃,and the detection wavelength is 254nm.Six kinds of biogenic amines have good linear relationship within the concentration range shown in Table 2(R2>98.575%).The detection limit of six kinds of biogenic amines is 0.04~0.09mg/L.Two levels of 3.0,5.0mg/L are selected for spiking,and the average spiking recovery rate is 92.2%~108.86%.

关 键 词：高效液相色谱(HPLC) 白酒 生物胺 

分 类 号：TS262.3[轻工技术与工程—发酵工程] TS207.3[轻工技术与工程—食品科学与工程]