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色谱

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高效毛细管电泳法测定牛奶和奶粉中残留的三聚氰胺

饶钦雄1，童敬2，郭平3，李海燕3，李晓薇2，丁双阳2   

  1. 1.Institute for Agri-food Standards and Testing Technology, Shanghai Academy of Agricultural Sciences, Shanghai 201106, China; 2.National Reference Laboratories for Veterinary Drug Residue, College of Veterinary Medicine, China Agricultural University, Beijing 100193, China; 3.Jiangxi Entry-Exit Inspection and Quarantine Bureau, Nanchang 330002, China
  • 收稿日期:2008-10-12 修回日期:2008-11-12 出版日期:2008-11-30 发布日期:1983-06-25
  • 通讯作者: 丁双阳
  • 基金资助:
    国家“十一五”科技支撑计划项目(项目号：2006BAD31B09-2)

Determination of melamine in milk and milk powder by high performance capillary electrophoresis

RAO Qinxiong1, TONG Jing2, GUO Ping3, LI Haiyan3, LI Xiaowei2, DING Shuangyang2   

  1. 1.Institute for Agri-food Standards and Testing Technology, Shanghai Academy of Agricultural Sciences, Shanghai 201106, China; 2.National Reference Laboratories for Veterinary Drug Residue, College of Veterinary Medicine, China Agricultural University, Beijing 100193, China; 3.Jiangxi Entry-Exit Inspection and Quarantine Bureau, Nanchang 330002, China
  • Received:2008-10-12 Revised:2008-11-12 Online:2008-11-30 Published:1983-06-25
  • Contact: DING Shuangyang

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摘要： 建立了牛奶和奶粉中三聚氰胺的高效毛细管电泳-二极管阵列检测器(HPCE-DAD)检测方法。使用长度58.5 cm、内径75 μm的毛细管柱，分离电压25 kV，进样量3.5 kPa (35 mbar)×8 s，分离温度25 ℃，缓冲溶液20 mmol/L 柠檬酸-40 mmol/L 磷酸氢二钠(pH 2.6)，检测波长232 nm。分析物在1~100 mg/L 范围内线性良好，r2>0.997；牛奶和奶粉的定量限分别为0.5 mg/kg和1.0 mg/kg。在添加水平为定量限浓度至50 mg/kg时的回收率为72.2%~97.3%，相对标准偏差为2.1%~3.9%。

关键词: 高效毛细管电泳, 奶粉 , 牛奶, 三聚氰胺

Abstract: A high performance capillary electrophoresis (HPCE) method has been established for the separation of melamine in milk and milk powder. The separation was carried out on a fused-silica uncoated capillary column （58.5 cm×75 μm）. The sample was injected by hydrodynamic injection (3.5 kPa (35 mbar)×8 s) at a temperature of 25 ℃. The analysis was completed in about 6 min in 40 mmol/L Na2HPO4-20 mmol/L citric acid buffer (pH 2.6) at 25 kV of separation voltage and 232 nm of detection wavelength. The linear range of melamine was 1-100 mg/kg, and the correlation coefficient was higher than 0.997. The limits of quantification (LOQs) in milk and milk powder were 0.5 mg/kg and 1.0 mg/kg, respectively. The average recoveries were in the range of 72.2%-97.3% in the spiked range of the concentration of LOQs and 50 mg/kg, and the relative standard deviations were between 2.1% and 3.9%.

Key words: melamine, milk, milk powder , high performance capillary electrophoresis (HPCE)