奶粉中三聚氰胺hplc-食品科学.pdfVIP

264 2010, Vol. 31, No. 14 食品科学 ※分析检测 刘 菊，郑 婷，常 诚，刘 霞，张薇薇，施超欧 * (华东理工大学分析测试中心，上海 200237) ：采用反相离子对色谱法、亲水相互作用色谱法及阳离子交换色谱法测定奶粉中三聚氰胺的含量。奶粉样 品前处理采用水- 乙酸提取后过RP 柱和甲酸提取后乙腈沉淀两种方法，反相离子对色谱法采用C18 柱和 10mmol/L庚 烷磺酸钠与 10mmol/L 柠檬酸的缓冲溶液 - 乙腈(85:15，V/V) 的流动相；亲水相互作用色谱法采用HILIC 柱和20mmol/L 甲酸胺- 乙腈(10:90，V/V) 的流动相；阳离子交换色谱法采用IonPac CS17 阳离子交换柱和6mmol/L 硫酸的流动相。 流速 1.0mL/min，检测波长240nm 。结果表明，3 种方法测定三聚氰胺在0.1～25.0mg/L 范围内线性均很好(r=1.0000) ， 样品加标回收率在 93.91%～99.96% 范围内。3 种方法中，反相离子对色谱法对三聚氰胺的响应值最高，阳离子交 换色谱法则能用最短的时间检测出三聚氰胺，而亲水相互作用色谱法在假阳性的判断上可作为其他两种方法的补充。 ：奶粉；三聚氰胺；反相离子对色谱；亲水相互作用色谱；阳离子交换色谱 Comparison of Three Chromatographic Methods for the Determination of Melamine in Powdered Milk LIU Ju ，ZHENG Ting ，CHANG Cheng ，LIU Xia ，ZHANG Wei-wei ，SHI Chao-ou* (Analysis and Testing Center, East China University of Science and Technology, Shanghai 200237, China) Abstract ：Three chromatographic methods, i.e., reversed-phase ion pair chromatography, hydrophilic interaction chromatog- raphy and cation exchange chromatography, were established to determine melamine in powered milk. Before hydrophilic interaction chromatographic analysis, samples were extracted with formic acid, precipitated with acetonitrile for the removal of proteins and centrifugated. While for other two methods, the sample pretreatment was based on extraction with aqueous acetic acid solution, precipitation, centrifugation and cleanup on a RP column. The chromatographic separation was performed on a C18 column using a mobile phase composed of a buffer solution containing 10 mmol/L sodium heptanesulfonate and 10 mmolL citric acid and acetonitrile (85:15, V/V) in reversed-phase ion pair chromatographic analysis. A HILIC column and 20 mmol/L ammonium f