白酒和黄酒中生物胺的高效液相色谱分析法

Determination of Biogenic Amines in Baijiu and Chinese Rice by High Performance Liquid Chromatography

本研究建立了1种检测某白酒与黄酒中常见的9种生物胺(尸胺、组胺、酪胺、色胺、盐酸吡哆胺、精胺、亚精胺、腐胺和2-苯乙胺)的柱前衍生-高效液相色谱法,并对其实际运用可行性进行验证与讨论。以丹磺酰氯(Dns-Cl)作为衍生试剂,采用Thermo Hypersil GOLD C18色谱柱(250 mm×4.6 mm,5μm)分离,以乙腈和含0.1%甲酸的0.01 mol/L乙酸铵水溶液作为流动相A与B,流速0.8 mL/min,紫外检测器波长254 nm。分析结果显示,9种生物胺在质量浓度0.5~50 mg/L范围,生物胺浓度与峰面积间线性相关性良好(R2>0.998)。选取1.0,5.0,10.0 mg/L 3个水平加标,得到加标回收率83.30%~114.7%,相对标准偏差均低于4.56%,9种生物胺检出限为0.07~0.22 mg/L。采用柱前衍生-高效液相色谱法分离、检测白酒与发酵酒——黄酒中的生物胺,实现了白酒与黄酒中生物胺含量的准确检测。

An analytical method for biogenic amines commonly(cadaverine,histamine,tyramine,tryptamine,pyridoxamine hydrochloride,spermine,spermidine,putrescine and 2-phenylethylamine)in Baijiu and Chinese rice wine by pre-column derivatization-HPLC was developed.The biogenic amines in Baijiu and Chinese rice wine were derived with dansyl chloride,separated by the C18 chromatographic column(250 mm×4.6 mm,5μm).The mixture of acetonitrile and water(0.01 mmol/L ammonium acetate,0.1%formic acid)were served as the mobile phase at a flow rate of 0.8 mL/min and the ultraviolet(UV)detection wavelength was 254 nm.The results showed that in the concentration range of 0.5-50 mg/L,each of the 9 biogenic amine presented good linear correlation(R2>0.998).After the addition of a mixed standard solution of biogenic amines to Chinese yellow wine,the recovery rates were 83.30%-114.7%,with relative standard deviations(RSDs)below 4.56%,and the limit of detection for each component was 0.07-0.22 mg/L.Hence,the pre-column derivatization-HPLC method in this experiment could be used to separate and detect the biogenic amines in Baijiu and Chinese rice wine accurately.