婴幼儿配方乳粉中三聚氰胺检测中前处理方法的优化

Optimization of pretreatment methods for determination of melamine in infant formula milk powder

中文关键词:  婴幼儿配方乳粉  高效液相色谱  三聚氰胺

英文关键词:infant formula milk powder  high performance liquid chromatography  melamine

中文摘要:

      目的 改进婴幼儿配方乳粉中三聚氰胺的检测方法。方法 样品经高浓度三氯乙酸溶液-乙腈提取过滤, 后经阳离子交换固相萃取柱净化, 用高效液相色谱法测定, 采用外标法定量。结果 改进方法的检测时间缩短4 h, 在0.5~10 μg/mL范围内检测结果线性关系良好, 方法检出限为0.5 mg/kg, 定量限为1.5 mg/kg, 回收率提高到99.3%~102%, 精密度为0.47%, 稳定性相对标准偏差为0.96%, 能力验证结果表明可靠性好。 结论 改进方法能快速有效对婴幼儿配方乳粉产品进行检测, 结果可靠, 具有实践应用价值。

英文摘要:

      Objective To improve the detection method of melamine in infant formula milk powder. Methods The samples were filtered by high concentration trichloroacetic acid solution and acetonitrile, and then purified by cation exchange solid phase extraction column. The samples were determined by high performance liquid chromatography and quantified by external standard method. Results The detection time of the improved method was shortened by 4 h, which had good linear relationships in the range of 0.5~10 μg/mL. The limit of detection was 0.5 mg/kg, and the limit of quantification was 1.5 mg/kg. The recovery rate increased to 99.3%~102%, with the precision of 0.47%, and the stability of the relative standard deviation was 0.96%. Ability verification results showed that the reliability was good. Conclusion The improved method can be used to detect the infant formula milk powder quickly and effectively, and the result is reliable and has practical application value.