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[目的]建立一种牛乳中三聚氰胺的测定方法。[方法]导数极谱分析法。[结果]饱和硼砂介质下,三聚氰胺有很好的到数极谱峰,其峰电位-0.33V(vs.SEC)左右,其浓度在0～100μg/ml呈线性关系(r﹥0.999),方法定量限为1.5mg/kg,在添加浓度在2～150mg/kg范围内,回收率在87.2%～103.6%之间(RSD﹤10%),同一样品用该方法与GB/T22388-2008中“高效液相色谱法(第一法)”同时测定的结果差异无统计学意义(P﹥0.05),本方法与GB/T22388-2008中“高效液相色谱法(第一法)”相比较,对应指标均能达到要求。[结论]采用本方法可准确分析牛乳中低含量的三聚氰胺,整个方法具有操作简便、快速和灵敏的特点,适用于基层单位推广应用。
[Objective] To establish a method for the determination of melamine in milk. [Method] Derivative polarographic analysis. [Result] Melamine had a good number polarographic peak under saturated borax media with a peak potential of -0.33 V (vs.SEC) and a linear relationship (r> 0.999) with a concentration of 0-100 μg / ml The limit of quantification was 1.5mg / kg. The recoveries ranged from 87.2% to 103.6% (RSD <10%) at the concentration range of 2 ~ 150mg / kg. There was no significant difference between the results of simultaneous determination of high performance liquid chromatography (first method) and the method of GB / T22388-2008, “High Performance Liquid Chromatography (First Method) ”Compared with the corresponding indicators can meet the requirements. [Conclusion] This method can accurately analyze the low content of melamine in milk. The method is simple, rapid and sensitive. It is suitable for popularization and application of grassroots units.