超高效液相色谱法同时快速测定多种动物源食品中9种生物胺的含量

摘要

Objective To establish a method for simultaneous determination of 9 kinds of biogenic amines including tryptamine,phenethylamine,putrescine,cadaverine,histamine,octopamine,tyramine,spermidine and sperminein in animal-derived foodstuffs by ultra performance liquid chromatography (UPLC).Methods Samples were extracted with perchloric acid solution,processed with pre-column derivatization with dansyl chloride,added ammonia water for termination reaction and then made up to the desired volume with acetonitrile.Chromatographic separation was performed on an Acquity UPLC BEH C18 column (2.1 mm×l00 mm,1.7 μm) using 5 mmol/L ammonium acetate and acetonitrile as mobile phase for gradient elution at the flow rate of 0.4 mL/min.Photo-diode array detector was used for detection at 254 nm.Results Nine kinds of biogenic amines had good linear relationships in the concentration range of 0.1～20 μg/mL with correlation coefficients larger than 0.999.The recoveries of samples spiked at levels of 20,50 and 100 mg/kg were 75.6％～97.2％ with the relative standard deviations (RSDs) of 0.12％～5.32％ (n=6).The limits of detection (LODs) of 9 kinds of biogenic amines were all 10 mg/kg.Conclusion The established method is simple,rapid and sensitive,which can be used for simultaneous determination of 9 kinds of biogenic amines residues in animal-derived foodstuffs.%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 C18(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0.1～20 μg/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.