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    催化动力学光度法测定奶制品中微量三聚氰胺

    Catalytic Kinetic Photometric Determination of Trace Amount of Melamine in Dairy Products

    • 摘要: 在磷酸-磷酸二氢钾缓冲溶液中,痕量三聚氰胺对铁氰化钾氧化4-氨基安替比林的显色反应有催化作用,在显色产物的吸收峰510 nm处测量时,所测得吸光度的增量ΔA与三聚氰胺的质量浓度在0.4~2.4 mg·L-1范围内呈线性关系。据此提出了催化动力学光度法测定痕量三聚氰胺的方法。优化的显色反应条件如下:① 20 g·L-1 4-氨基安替比林溶液用量为2.5 mL;② 反应温度为70 ℃;③ 反应时间为4 min。测得方法的检出限(3s)为0.313 mg·L-1。以纯鲜牛奶为基体用标准加入法进行回收试验,方法的回收率在98.6%~101%之间,测定值的相对标准偏差(n=6)在0.13%~0.69%之间。

       

      Abstract: It was found that in H3PO4-KH2PO4 buffer solution,the oxidative coloration of 4-amino antipyrine by potassium ferricyanide was catalyzed by the presence of trace amount of melamine, and that linear relationship was kept between the magnitude of increase in absorbance (ΔA) and mass concentration of melamine in the range of 0.4-2.4 mg·L-1 as measured at 510 nm, the absorption maximum of the colored product. Based on these facts, a catalytic kinetic photometric method for determination of trace amount of melamine in dairy products was proposed. The optimized conditions found for the color reaction were as follows: ① amount of 20 g·L-1 4-amino antipyrine solution used: 2.5 mL; ② temperature of reaction: 70 ℃; ③ time of reaction: 4 min. Detection limit (3s) found was 0.313 mg·L-1. Using pure fresh milk as matrix, test for recovery was made by standard addition method, giving values of recovery in the range of 98.6%-101% and RSD′s (n=6) in the range of 0.13%-0.69%.

       

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