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目的:建立乳及乳制品中三聚氰胺的高效液相色谱测定方法。方法:样品用三氯乙酸-甲酸-甲醇提取,经阳离子交换固相萃取净化后,用高效液相色谱仪测定。结果:色谱条件:5μC8(2)100A 4.6 mm×250 mm柱,流动相:乙腈-离子对缓冲液(体积比15:85),流速1.0 ml/min;波长240 nm;柱温40℃;峰面积定量。该法相对标准偏差为1.5%~3.2%,检出限为0.035 mg/kg,回收率为98.1%~105.5%。结论:该法准确可靠,适用乳及乳制品中三聚氰胺的测定。
Objective: To establish a method for the determination of melamine in milk and dairy products by high performance liquid chromatography. Methods: Samples were extracted with trichloroacetic acid - formic acid - methanol, purified by cation exchange solid - phase extraction and then determined by high performance liquid chromatography. Results: The chromatographic conditions were as follows: 5μ C8 (2) 100A 4.6 mm × 250 mm column with mobile phase of acetonitrile-ion buffer (volume ratio 15:85) Area quantitative. The relative standard deviation (RSD) was 1.5% -3.2%. The detection limit was 0.035 mg / kg. The recoveries ranged from 98.1% to 105.5%. Conclusion: This method is accurate and reliable, suitable for the determination of melamine in milk and dairy products.