反相高效液相色谱法同时检测海产品中8种生物胺
目的 建立一种可同时快速测定海产品中8种生物胺的丹磺酰氯柱前衍生反相高效液相色谱法。方法 样品经5%三氯乙酸提取, 丹磺酰氯柱前衍生后, 采用Agilent zorbax SB-C18色谱柱(4.6 mm×150 mm, 5 μm), 以甲醇和水作为流动相, 进行梯度洗脱。柱温30 ℃, 流速为1.5 mL/min, 采用UV紫外检测器, 检测波长254 nm, 对8种生物胺进行分离分析。结果 结果显示, 色胺、2-苯乙胺、腐胺、尸胺、组胺、酪胺、亚精胺和精胺在15 min内得到有效分离, 在1~100 mg/L范围内线性系数r2﹥0.999, 8种生物胺测定方法的检出限范围为0.02~0.17 mg/L, 定量限范围为0.067~0.57 mg/L, 且重复性良好, 向秋刀鱼中分别添加生物胺标准品20.0、50.0、100.0 mg/L 3个含量水平, 8种生物胺平均回收率介于79%~117%之间, 相对标准偏差为0.84%~12.57%。采用该方法测定了秋刀鱼等5类海产品中8种生物胺的含量, 结果显示生物胺总含量在23~208 mg/kg之间。结论 该方法简单、快速, 灵敏度和准确度符合要求, 适用于海产品中多种生物胺的同时检测。
Objective To establish a method for simultaneous determination of eight biogenic amines in seafood by reversed-phase high performance liquid chromatographic (RP-HPLC) with precolumn derivatization by dansylchloride. Methods Samples were extracted with trichloroacetic acid, and derivatized with dansylchloride. Using Agilent zorbax SB-C18 chromatography column (4.6 mm×150 mm, 5 μm), eight biogenic amines were separated and analyzed by RP-HPLC. The chromatographic conditions of RP-HPLC were as follows: the mobile phase for gradient elution consisted of methanol and water, the flow rate was 1.5 mL/min, the column temperature was 30 ℃, the UV detector was used and the detection wavelength was 254 nm. Results The results showed a good separation of eight biogenic amines (tryptamine, 2-phenylethylamine, putrescine, cadaverine, histamine, tyramine, spermidine, and spermine) within 15 min. It was linear in the range of 1~100 mg/L (r2﹥0. 999). The detection limits of eight biogenic amines were 0.02~0.17 mg/L, and the limits of quantification were 0.067~0.57 mg/L. The reproducibility of the method was good. The average recoveries of biogenic amines with different mass concentrations were 79%~117%, and the relative standard deviations (RSDs) ranged from 0.84% to 12.57%. The results showed that the total content of biogenic amines were between 23 and 208 mg/kg in five kinds of aquatic products. Conclusion The established method is simple, rapid, accurate, and sensitive, and can be used for simultaneous determination of biogenic amines in aquatic products.
标题：反相高效液相色谱法同时检测海产品中8种生物胺
英文标题：Simultaneous determination of eight biogenic amines in seafood by reversed-phase high performance liquid chromatography
作者：
田鑫 集美大学食品与生物工程学院,厦门市海洋功能食品重点实验室
刘红 集美大学食品与生物工程学院,厦门市海洋功能食品重点实验室
李传勇 厦门市农产品质量安全检验测试中心
张凌晶 集美大学食品与生物工程学院,厦门市海洋功能食品重点实验室
曹敏杰 集美大学食品与生物工程学院,厦门市海洋功能食品重点实验室
刘光明 集美大学食品与生物工程学院,厦门市海洋功能食品重点实验室
中文关键词:反相高效液相色谱法,生物胺,海产品,秋刀鱼,过敏反应,
英文关键词:reversed-phase high performance liquid chromatography,biogenic amines,seafood,Cololabis saira,allergic reactions,
发表日期：2016-12-28
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