国标法测定鱼肉中组胺的方法改进
Improvement of the Method in Chinese National Standards for the Determination of Histamine in Fish Meat
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摘要: 为简化GB 5009.208-2016第二法中组胺测定的实验步骤,提高实验准确度与精密度,本文在国标法的基础上进行方法改进。结果表明,将对硝基苯胺溶液的配制溶剂改为浓盐酸;选择60 ℃水浴保温0.5 h代替室温浸泡;采用旋涡振荡法对样品进行提取,并在此基础上将盐酸提取次数改为2次;在测定环节改取盐酸提取液为1.0 mL。改进法线性方程相关系数r=0.9991,加标回收率分别为92.90%~94.70%、91.50%~94.10%和100.20%~102.20%,RSD在1.84%~2.32%。该改进法操作简单、快速,可以更好地用于鱼类中组胺的测定。Abstract: In order to simplify the experimental steps of histamine determination in GB 5009.208-2016 and improve the accuracy and precision of the experiment, the paper ameliorated the method on the basis of the Chinese national standard. The results showed that, changed the solvent of P-nitroaniline solution to concentrated hydrochloric acid, and selected 60℃ to keep warm for 0.5 h instead of room temperature soaking. The samples were extracted by vortex oscillating. And the extraction times of hydrochloric acid were changed to 2 times on this basis. The extraction solution of hydrochloric acid was changed to 1.0 mL. The correlation coefficient of the improved linear equation was 0.9991.The recovery rate of the improved method were 92.90%~94.70%, 91.50%~94.10% and 100.20%~102.20%, and the RSD was 1.84%~2.32%. The method was simple and rapid. It could be used for the determination of histamine in fish better.