高效液相色谱法测定金枪鱼产品中的生物胺含量

Determination of biogenic amines in tuna products using high performance liquid chromatography

中文关键词:  生物胺  组胺  高效液相色谱法  金枪鱼  金枪鱼罐头  金枪鱼松  金枪鱼刺身

英文关键词:biogenic amine  histamine  high performance liquid chromatography  tuna  canned tuna  tuna pine  tuna sashimi

中文摘要:

      目的 建立高效液相色谱法检测金枪鱼产品中8种常见生物胺的含量。方法 样品经酸介质提取, 丹磺酰氯衍生, 0.22 μm有机膜过滤后, 采用CAPCELL Pak C18 MGⅡ色谱柱(150 mm×4.6 mm, 5 μm), 以甲醇-超纯水为流动相进行梯度洗脱, 流速0.8 mL/min, 柱温为室温。生物胺各组分以外标法进行定量。结果 采用0.4 mol/L高氯酸提取样品3次, 可以获得最优的生物胺提取效果。生物胺各组分浓度为0.17~2.25 mg/kg范围呈良好的线性关系(r>0.999), 平均加标回收率为86.6%~115.9%, 相对标准偏差为1.5%~13.7%。?80 ℃金枪鱼刺身的总生物胺含量低于10 mg/kg, 冰鲜金枪鱼刺身的总生物胺含量要高于?80 ℃金枪鱼刺身, 但低于 100 mg/kg; 金枪鱼罐头主要含有组胺、尸胺、腐胺和酪胺, 总生物胺含量范围为106.63~357.09 mg/kg; 金枪鱼松的总生物胺含量范围为111.20~751.54 mg/kg; 部分金枪鱼罐头和金枪鱼松的组胺含量超过50 mg/kg。 结论 建立的高效液相色谱法可以准确测定金枪鱼产品中的8种常见生物胺含量, 本文测定的金枪鱼刺身产品中生物胺含量较低, 不存在安全隐患, 部分金枪鱼罐头和金枪鱼松的生物胺(尤其是组胺)含量较高, 有出口退回风险, 应引起足够重视。

英文摘要:

      Objective To establish a method for the determination of 8 kinds of common biogenic amines in tuna products by high performance liquid chromatography (HPLC). Methods The sample was extracted from acid medium and derived by dansyl chloride, then the supernatant was filtered through 0.22 μm membrane microfilter for analysis. The samples were separated with a CAPCELL Pak C18 MGⅡ column (150 mm×4.6 mm, 5 μm) at the flow rate of 0.8 mL/min by gradient elution using methyl alcohol and water. The temperature of the column oven was maintained at room temperature, and the contents of 8 kinds of biogenic amine were quantitatively analyzed by external standard method. Results The optimal extraction effect of biogenic amines from tuna products was achieved by using 0.4 mol/L of perchloric acid for three times. Each compound of biogenic amines showed a good linear relationship between peak areas and concentrations in the concentration range of 0.17-2.25 mg/kg (r>0.999). The recoveries of 8 kinds of biogenic amines were 86.6%-115.9% with relative standard deviations (RSDs) of 1.5%-13.7%. Total biogenic amines contents of tuna sashimi products stored at ?80 ℃ were less than 10 mg/kg. Total biogenic amines contents of tuna sashimi products stored on ice were more than those stored at ?80 ℃, but less than 100 mg/kg. Canned tuna mainly contained histamine, resin amine, sapropine and tyramine, and the total biogenic amine content ranged from 106.63 to 357.09 mg/kg. Total biogenic amines contents of tuna pine products were between 111.20 mg/kg and 751.54 mg/kg. Some canned tuna products and tuna pine products contained more than 50 mg/kg of histamine. Conclusion The proposed high performance liquid chromatography method is accurate for detecting 8 kinds of biogenic amines in commercial tuna products. There is no safety risk in tuna sashimi products because of less biogenic amines content. However, attentions must be paid to some canned tuna products and tuna pine products because of higher biogenic amines (especially histamine) content.