高效液相色谱法测定酱油中组胺的含量

Determination of histamine in soy sauce by high performance liquid chromatography

中文关键词:  高效液相色谱法  组胺  酱油

英文关键词:high performance liquid chromatography  histamine  soy sauce

中文摘要:

      目的 建立丹磺酰氯柱前衍生-高效液相色谱法测定酱油中组胺含量的方法。方法 样品酱油以1,7-二氨基庚烷作为内标, 用正丁醇:三氯甲烷(1:1, V:V)萃取净化, 经丹磺酰氯衍生, 乙醚萃取后氮气吹干, 用乙腈定容, 高效液相色谱仪测定, 内标法定量。结果 组胺含量在1~100 mg/L线性关系良好, 线性相关系数r=0.9999, 检出限为0.5 mg/kg。在精密度实验中, 其相对标准偏差为2.59%~6.48%, 在1.0、10.0、50.0 mg/kg的添加水平下, 加标回收率为88.0%~104.2%。结论 该方法线性关系好、检出限低、稳定性好、回收率高、测定结果准确, 适合酱油中组胺的测定。

英文摘要:

      Objective To establish a method for the determination of histamine in soy sauce by high performance liquid chromatography with dansyl chloride pre-column derivatization. Methods The sample soy sauce was extracted and purified with 1,7-diamino heptane by n-butanol-chloroform (1:1, V:V). After derivated by dansulfonyl chloride and extracted with ether, the sample soy sauce was dried by nitrogen gas, then dissolved in acetonitrile, and the content was determined with high performance liquid chromatography internal standard method. Results There was a good linear relationship between histamine content at 1?100 mg/L, the linear correlation coefficient r=0.9999, and the limit of detection was 0.5 mg/kg. In the precision experiment, the relative standard deviation was 2.59%?6.48%. At the addition level of 1.0, 10.0 and 50.0 mg/kg, the standard recovery was 88.0%?104.2%. Conclusion This method has the advantages of good linearity, low detection limit, good stability, high recovery, accurate results, and is suitable for the determination of histamine in soy sauce.