色谱

色谱

• 技术与应用 • 上一篇    下一篇

高效液相色谱法测定奶粉和液态奶中的三聚氰胺

何乔桑，刘敏芳，黄丽英，杨园园，廖上富   

  1. Zhejiang Test Academy of Quality and Technical Supervision, Hangzhou 310013, China
  • 收稿日期:2008-10-10 修回日期:2008-11-10 出版日期:2008-11-30 发布日期:1983-06-25
  • 通讯作者: 何乔桑
  • 基金资助:

Determination of melamine in milk powder and milk by high performance liquid chromatography

HE Qiaosang, LIU Minfang, HUANG Liying, YANG Yuanyuan, LIAO Shangfu   

  1. Zhejiang Test Academy of Quality and Technical Supervision, Hangzhou 310013, China
  • Received:2008-10-10 Revised:2008-11-10 Online:2008-11-30 Published:1983-06-25
  • Contact: HE Qiaosang

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摘要： 建立了奶粉和液态奶中三聚氰胺的高效液相色谱（HPLC）检测方法。经阳离子交换固相萃取柱净化后的样品采用HPLC测定。优化的色谱条件：C18柱（4.6 mm ×200 mm，5 μm），流动相为乙腈-0.01 mol/L庚烷磺酸钠（pH 3.3）（体积比为10∶90），流速为1.0 mL/min，检测波长为236 nm，柱温为40 ℃，进样量为20 μL。方法的线性范围为1~500 mg/L，检出限为0.2 mg/kg （S/N=3），定量限为1 mg/kg （S/N=15），回收率为81.4%~83.7%，相对标准偏差为3.3%~8.5%（n=6）。

关键词: 高效液相色谱法, 固相萃取, 奶粉, 三聚氰胺, 液态奶

Abstract: The analytical method of melamine in milk and milk powder by high performance liquid chromatography (HPLC) was established. The sample was purified by a cation exchange solid-phase extraction column, separated on a Diamonsil C18 column (4.6 mm×200 mm, 5 μm) with acetonitrile-0.01 mol/L sodium heptanesulfonate (pH 3.3) (10∶90, v/v) as mobile phase at a flow rate of 1.0 mL/min, and determined by a photodiode array detector. A linear calibration curve was obtained in the concentration range of 1-500 mg/L. The qualification limit was 0.2 mg/kg, and the quantification limit was 1 mg/kg. The recovery was 81.4%-83.7%.

Key words: high performance liquid chromatography (HPLC), melamine, milk , milk powder, solid-phase extraction（SPE）