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液相色谱法快速测定乳制品中三聚氰胺含量
Studies on Quick Determination of Melamine of Dairy Products by HPLC
【摘要】 建立高效液相色谱法快速测定乳制品中三聚氰胺的分析方法。采用三氯乙酸溶液-乙腈提取乳制品中的三聚氰胺,用强阳离子交换色谱柱(SCX,250 mm×4.6 mm,5μm),在流动相配比为0.05 mol/L磷酸二氢钾缓冲液(pH=3.0)-乙腈(65+35,体积比)条件下分离,紫外检测器210 mm波长检测。结果表明:采用外标法定量,该方法在0.10 mg/L~10.0 mg/L浓度范围内有良好的线性关系,加标回收率均在91%以上,相关系数R2为0.999 9,相对标准偏差不大于1.2%,方法最低检出限为0.01 mg/L。通过实验室间能力验证证明,该方法具有快速、准确、灵敏度高,样品前处理简便易行等优点,可满足实验室日常快速检测乳制品中三聚氰胺的工作需求。
【Abstract】 An analysis method for quick determination of melamine from dairy products by HPLC has been developed.Trichloroacetic acid-acetonitrile was used to extract melamine from dairy products,and HPLC analyses were performed using the following operating parameters: strong cation exchange column(SCX,250 mm×4.6 mm,5 μm),mobile phase ratio: 0.05 mol/L KH2PO4(pH=3.0)/acetonitrile(65+35,volume ratio),UV detector wavelength 210 nm.This method with good linearity relation between 0.10 mg/L-10.0 mg/L adopted external standard method.The recovery was above 91 % and the coefficient of correlation R2 was 0.999 9.The relative standard deviation(RSD)was less than 1.2 %.The limit of detection was 0.01 mg/L.This method is quick,precise and sensitive,it also has good advantage of simple pretreatment,which satisfies the needs of routine testing melamine of dairy products.
【Key words】 liquid chromatography; strong cation exchange column; UV detector; dairy products; melamine;
- 【文献出处】 食品研究与开发 ,Food Research and Development , 编辑部邮箱 ,2010年11期
- 【分类号】TS252.7
- 【被引频次】4
- 【下载频次】239