液相色谱-质谱／质谱法测定乳与乳制品中的三聚氰胺  

Determination of Melamine in Milk and Dairy Products by Liquid Chromatography-Tandem Mass Spectrometry

作　　者：陈冬东[1] 彭涛[1] 李晓娟[1] 李淑娟[1] 邵兵[2] 徐娇[3] 

机构地区：[1]中国检验检疫科学研究院,北京100123 [2]北京市疾病预防控制中心,北京100013 [3]卫生部卫生监督中心,北京100007

出　　处：《中国食品卫生杂志》2009年第3期253-255,共3页Chinese Journal of Food Hygiene

摘　　要：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 develop a method of Liquid chromatography-tandem mass spectrometry （LC - MS/MS ） for determination of melamine in milk and dairy products. Method Melamines were extracted from samples with trichloracetic acid solution and acetonitrile, and then cleaned up by cation ion exchange SPE cartridge. The analytes were determined by LC- MS/ MS, and quantified by the external standard curve. Results The linearity was good between 0.01 and 0.5μg/ml. Correlation coefficient was 0.999 2. The limit of quantization （LOQ） was 0.01 mg/kg. Recoveries of melamine ranged from 80.4% to 107.4 %, in spiked level from 0.01 to 0. 1μg/ml, with relative standard deviations （ RSDs ） ≤ 9.4 %. Conclusion This method was easy to operate. And the sensitivity, accuracy, precision of the method could satisfy the requirements for the identification and quantification of melamine in milk and dairy products.

关 键 词：三聚氰胺 色谱法 液相 光谱分析 质量 食品分析 乳 

分 类 号：R155.5[医药卫生—营养与食品卫生学]