食品科学 ›› 2014, Vol. 35 ›› Issue (6): 172-175.doi: 10.7506/spkx1002-6630-201406037

• 分析检测 • 上一篇    下一篇

高效液相色谱法快速测定乳粉中的三聚氰胺与双氰胺

杨 嘉1,丁娟芳2,周元元1,徐 秋1,朱 姜1,王 帅1   

  1. 1.扬州市产品质量监督检验所,江苏 扬州 225111;2.扬州职业大学生物与化工工程学院,江苏 扬州 225009
  • 收稿日期:2013-07-03 修回日期:2014-03-13 出版日期:2014-03-25 发布日期:2014-04-04
  • 通讯作者: 杨嘉 E-mail:jiajia82112001@163.com

Rapid Determination of Melamine and Dicyandiamide in Milk Powder by High Performance Liquid Chromatography

YANG Jia1, DING Juan-fang2, ZHOU Yuan-yuan1, XU Qiu1, ZHU Jiang1, WANG Shuai1   

  1. 1. Yangzhou Products Quality Supervision and Inspection Institute, Yangzhou 225111, China;
    2. College of Biological and Chemical Engineering, Yangzhou Polytechnic College, Yangzhou 225009, China
  • Received:2013-07-03 Revised:2014-03-13 Online:2014-03-25 Published:2014-04-04
  • Contact: YANG Jia E-mail:jiajia82112001@163.com

摘要:

建立高效液相色谱-二极管阵列检测器同时检测乳粉中三聚氰胺和双氰胺的分析方法。采用1%三氯乙酸溶液提取样品中的三聚氰胺和双氰胺,氨基柱为分析柱,流动相为乙腈-水(75∶25,V/V),流速1.0 mL/min,检测波长233 nm。2 种物质在0.005~60 mg/L范围内与其峰面积线性关系良好,不同添加水平的回收率在83.2%~102.6%,三聚氰胺和双氰胺的方法定量限分别为0.17、0.15 mg/kg,方法变异系数为2.3%~7.2%(n=6)。此方法操作简便、快速、成本低,适用于乳粉中三聚氰胺和双氰胺的同时检测。

关键词: 高效液相色谱, 二极管阵列检测器, 乳粉, 三聚氰胺, 双氰胺

Abstract:

A high performance liquid chromatography-diode array detector (DAD) method was developed for rapid
and simultaneous determination of melamine and dicyandiamide in milk powder. Melamine and dicyandiamide were
extracted with 1% trichloroacetic acid solution. The chromatographic separation was performed on an amino column using
acetonitrile-water (75:25, V/V) as mobile phase at a flow rate of 1.0 mL/min, and the analytes were detected with a DAD
detector at 233 nm. The two compounds were well separated with a good linear relationship in the wide range of 0.005–60 mg/L.
The average recoveries in milk powder were in the range of 83.2%–102.6% at several spiked levels. The lowest limits of
quantification for melamine and dicyandiamide were 0.17 and 0.15 mg/kg, respectively, and the precision of the method
expressed as coefficient of variance (CV) was in the range of 2.3%–7.2% (n = 6). This method is simple, rapid, low-cost and
suitable for the simultaneous determination of melamine and dicyandiamide in milk powder.

Key words: high performance liquid chromatography, diode array detector, milk powder, melamine, dicyandiamide

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