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目的建立超高效液相色谱(ultra performance liquid chromatography,UPLC)同时测定动物源性食品中色胺、苯乙胺、腐胺、尸胺、组胺、章鱼胺、酪胺、亚精胺、精胺等9种生物胺的含量。方法样品经高氯酸溶液提取,丹磺酰氯柱前衍生化,加入氨水终止反应,乙腈定容。采用Acquity UPLC BEH C_(18)(2.1mm×100 mm,1.7μm)色谱柱,以5 mmol/L乙酸铵和乙腈作为流动相进行梯度洗脱,流速为0.4 mL/min,采用二极管阵列检测器在波长254 nm下检测。结果 9种生物胺在0.1~20μg/mL的范围内呈现良好的线性关系(r>0.999)。样品在20、50和100 mg/kg 3个浓度水平的加标回收率为75.6%~97.2%,相对标准偏差为0.12%~5.32%(n=6);9种生物胺的方法定量限均为10 mg/kg。结论该方法简便、快捷、准确,可以用于动物源性食品中9种生物胺的同时测定。
Objective To establish an ultra performance liquid chromatography (UPLC) for the simultaneous determination of tryptamine, phenethylamine, putrescine, cadaverine, histamine, octopamine, tyramine, 9 kinds of bio-amine content. Methods The samples were extracted with perchloric acid solution, derivatized with Dansyl chloride before column, and ammonia was added to terminate the reaction. The column was eluted with 5% ammonium acetate and acetonitrile as mobile phase using a mobile phase of Acquity UPLC BEH C 18 (2.1 mm × 100 mm, 1.7 μm) with a flow rate of 0.4 mL / min and a diode array detector Detection at a wavelength of 254 nm. Results Nine biogenic amines showed good linearity in the range of 0.1 ~ 20μg / mL (r> 0.999). The recoveries were 75.6% -97.2% with relative standard deviations (RSDs) of 0.12% -5.22% (n = 6) at the concentrations of 20, 50 and 100 mg / kg. 10 mg / kg. Conclusion The method is simple, rapid and accurate and can be used for the simultaneous determination of nine biogenic amines in animal-derived foods.