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目的建立发酵酒中色胺、2-苯乙胺、腐胺、组胺、尸胺、酪胺、精胺、亚精胺的柱后衍生-液相色谱分析方法,并探讨其在实际检测中的适用性。方法取2 ml样品经高氯酸涡旋提取,以离子对试剂和乙腈为流动相,高效液相色谱梯度洗脱,Atlantis-C_(18)柱分离,采用邻苯二甲醛(OPA)为柱后衍生试剂,二极管阵列检测器254 nm检测,以1,7-二氨基庚烷为内标进行定量。结果本法8种生物胺在1.0 mg/L~50 mg/L内线性关系良好,相关系数均≥0.998 2,在1.0 mg/L、5.0 mg/L、10.0 mg/L的3个添加水平的平均回收率为81.2%~106.0%,相对标准偏差为2.79%~5.21%,方法定量限为0.2 mg/L。结论采用柱后衍生-高效液相色谱法对发酵酒中的生物胺进行分离检测,方法快速、简便、灵敏度高,适用于批量实际样品检测。
Objective To establish a post-column derivatization-liquid chromatographic method for the determination of tryptamine, 2-phenylethylamine, putrescine, histamine, cadaverine, tyramine, spermine and spermidine in fermented wine Applicability. Methods Two ml samples were vortexed by perchloric acid and separated by Atlantis-C_ (18) column using ion-pair reagent and acetonitrile as mobile phases. High performance liquid chromatography (HPLC) Post-derivatization reagent, diode array detector detection 254 nm, 1,7-diaminoheptane as an internal standard for quantitative. Results The linearity of the eight biogenic amines in the range of 1.0 mg / L ~ 50 mg / L was good with the correlation coefficients ≥0.998 2. At the three addition levels of 1.0 mg / L, 5.0 mg / L and 10.0 mg / L, The average recoveries ranged from 81.2% to 106.0%, with relative standard deviations from 2.79% to 5.21%. The limit of quantification was 0.2 mg / L. Conclusion Post-column derivatization-high performance liquid chromatography (HPLC) is used to separate and detect biogenic amines in the fermented liquor. The method is rapid, simple and sensitive, and is suitable for the detection of batch actual samples.