色谱 ›› 2012, Vol. 30 ›› Issue (07): 716-720.DOI: 10.3724/SP.J.1123.2012.02011

• 研究论文 • 上一篇    下一篇

应用亲水作用色谱检测鸡蛋和肉中三聚氰胺及三聚氰酸二酰胺

李延昭1, 郝卫强2*, 王余波1, 陈强2, 李锦春1, 孙小丽1   

  1. 1. 常州大学材料科学与工程学院, 江苏 常州 213164; 2. 南京大学常州高新技术研究院, 江苏 常州 213164
  • 收稿日期:2012-02-04 修回日期:2012-03-01 出版日期:2012-07-28 发布日期:2012-07-19
  • 通讯作者: 郝卫强,博士,副研究员,主要研究方向为色谱分析. E-mail: hao_w_q@163.com.
  • 基金资助:

    国家自然科学基金项目(21005009)和常州市应用基础研究计划项目(CJ20115002).

Determination of melamine and ammeline in eggs and meat using hydrophilic interaction liquid chromatography

LI Yanzhao1, HAO Weiqiang2*, WANG Yubo1, CHEN Qiang2, LI Jinchun1, SUN Xiaoli1   

  1. 1. School of Materials Science and Engineering, Changzhou University, Changzhou 213164, China; 2. High-Tech Research Institute of Nanjing University, Changzhou 213164, China
  • Received:2012-02-04 Revised:2012-03-01 Online:2012-07-28 Published:2012-07-19

摘要: 应用亲水作用色谱(HILIC)对从市场上购买的鸡蛋和肉中的三聚氰胺及三聚氰胺降解产物三聚氰酸二酰胺进行了检测。采用的色谱柱为ZIC-HILIC柱,流动相为3 mmol/L磷酸二氢铵溶液(pH 6.9)-乙腈(20:80, v/v),流速为0.8 mL/min,检测波长为220 nm。在该体系下,三聚氰胺和三聚氰酸二酰胺的保留时间适中,与样品中的内源性物质有良好的分离。样品经0.1%磷酸提取,偏磷酸及乙腈沉淀蛋白质和糖类物质,以及P-SCX固相萃取柱净化。三聚氰胺和三聚氰酸二酰胺在0.4~40 mg/L范围内与峰面积呈良好的线性关系,样品定量限(按信噪比(S/N)不小于10计)为2 mg/kg,在2~10 mg/kg添加水平下的平均回收率为80%~105%,相对标准偏差小于10%。该方法具有良好的分离选择性,可用于鸡蛋和肉中三聚氰胺和三聚氰酸二酰胺的同时检测。

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关键词: 鸡蛋, 亲水作用色谱, 肉, 三聚氰胺, 三聚氰酸二酰胺, 液相色谱

Abstract: A hydrophilic interaction liquid chromatographic (HILIC) method for the determination of melamine and its degradation product ammeline in eggs and meat has been developed. The separation was carried out on a ZIC-HILIC column with 3 mmol/L NH4H2PO4 (pH 6.9)-acetonitrile (20:80, v/v) as mobile phase at the flow rate of 0.8 mL/min, and detected at 220 nm. Compared with the reversed-phase liquid chromatography, this method can avoid the use of ion pair reagents and thus simplify the composition of mobile phase. Under the above chromatographic conditions, melamine and ammeline had good peak shapes and moderate retention times. Good separation between these compounds and the substances that were naturally contained in the samples can be achieved. For the sample preparation, the analytes were first extracted with 0.1% phosphoric acid due to the basicity of melamine and ammeline. Then, metaphosphoric acid and acetonitrile were used to remove proteins and saccharides by precipitation. After the filtration and removal of acetonitrile by rotary evaporation under vacuum, the filtrate was cleaned-up by solid-phase extraction (SPE) technique in which a cation exchange column was used. The SPE column was activated by using methanol and 0.1% phosphoric acid. A solution of 5% ammonia methanol was chosen as eluent. The residues obtained from the eluant by evaporating the solvent were resolved in the mobile phase. It was found that there was a good linear relationship between concentration and detector response within the range of 0.4~40 mg/L. The limits of detection were 2 mg/kg for both melamine and ammeline. The average recoveries were between 80% and 105% in the spiked range of 2~10 mg/kg. The relative standard deviations were not more than 10%. The solutions of melamine and ammeline were stable in a month. The established method can be used in practice to determine melamine and ammeline simultaneously in egg and meat samples.

Key words: ammeline, eggs, liquid chromatography (LC), meat, melamine, hydrophilic interaction liquid chromatography (HILIC)

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