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目的建立乳与乳制品中三聚氰胺的液相色谱-质谱/质谱(LC-MS/MS)测定方法。方法样品用三氯乙酸溶液和乙腈提取,经阳离子交换固相萃取柱(SPE)净化后,用液相色谱-质谱/质谱法测定和确证,外标法定量。结果在0.01～0.50μg/ml范围内呈线性相关,相关系数为0.999 2,方法测定低限(LOQ)为0.01 mg/kg。在0.01～0.10μg/ml添加浓度范围内,方法回收率为80.4%～107.4%,相对标准偏差(RSD)≤9.4%。结论本方法操作简便,灵敏度、准确度、精密度可满足乳与乳制品中三聚氰胺的检测要求。
Objective To establish a method for the determination of melamine in milk and dairy products by liquid chromatography-mass spectrometry / mass spectrometry (LC-MS / MS). Methods The samples were extracted with trichloroacetic acid solution and acetonitrile, purified by cation exchange SPE, and determined by liquid chromatography-mass spectrometry / mass spectrometry and quantified by external standard method. The results were linear in the range of 0.01-0.50 μg / ml with a correlation coefficient of 0.999 2. The LOQ of the method was 0.01 mg / kg. The method recoveries ranged from 80.4% to 107.4% and the relative standard deviations (RSDs) ≤9.4% in the range of 0.01 ~ 0.10μg / ml. Conclusion The method is simple, sensitive, accurate and precise to meet the detection requirements of melamine in milk and dairy products.