色谱

色谱 ›› 2010, Vol. 28 ›› Issue (09): 859-862.DOI: 10.3724/SP.J.1123.2010.00859

• 研究论文 • 上一篇    下一篇

高效液相色谱-串联质谱法测定牛奶和奶粉中的三聚氰酸

桂茜雯*, 柳菡, 赵增运, 丁涛, 徐锦忠,沈伟健, 沈崇钰, 吴斌, 张睿   

  1. 江苏出入境检验检疫局动植物与食品检测中心, 江苏 南京 210001
  • 收稿日期:2010-05-27 修回日期:2010-08-10 出版日期:2010-09-28 发布日期:2010-09-28
  • 通讯作者: 桂茜雯,助理工程师,主要研究方向为食品检测.
  • 基金资助:

    无

Determination of cyanuric acid in milk and milk powder by high performance liquid chromatography-tandem mass spectrometry

GUI Qianwen*, LIU Han, ZHAO Zengyun, DING Tao, XU Jinzhong, SHEN Weijian, SHEN Chongyu, WU Bin, ZHANG Rui   

  1. Animal, Plant and Food Inspection Center of Jiangsu Entry-Exit Inspection and Quarantine Bureau, Nanjing 210001, China
  • Received:2010-05-27 Revised:2010-08-10 Online:2010-09-28 Published:2010-09-28

PDF

503

被引次数

17

摘要： 建立了牛奶和奶粉中三聚氰酸(CYA)的高效液相色谱-串联质谱(HPLC-MS/MS)测定方法。样品用乙腈提取并沉淀蛋白,经强阴离子交换柱富集和净化,AX色谱柱分离,HPLC-MS/MS法测定,内标法定量。50～2000 μg/L范围内CYA的线性关系良好(r≥0.999);在奶粉和牛奶基质中,添加200、500和1000 μg/kg 3个添加水平的回收率均在97%～121%之间,相对标准偏差(RSD)均小于4.8%;定量限(LOQ)为200 μg/kg。方法的前处理快速简便,净化效果好,准确度和精密度高,可用于牛奶和奶粉中CYA的测定。

关键词: 高效液相色谱-串联质谱, 奶粉, 牛奶, 三聚氰酸

Abstract: A method for the determination of cyanuric acid (CYA) in milk and milk powder was developed using high performance liquid chromatography-electrospray ionization tandem mass spectrometry (HPLC-ESI MS/MS). The target analyte was extracted from samples by acetonitrile, and the proteins were precipitated at the same time. The supernatant was cleaned up and enriched with a strong anion exchange column, analysed by HPLC-MS/MS with an AX column, and quantified by internal standard method. Good linearity was obtained in the range of 50~2000 μg/L. The recoveries were all ranged from 97% to 121% at three levels, 200, 500 and 1000 μg/kg, and the relative standard deviations (RSDs) were all below 4.8%. Limit of quantification (LOQ) was 200 μg/kg. The method has high accuracy and precision, the operation is fast, easy and suitable for the determination of CYA in milk and milk powder.

Key words: cyanuric acid, milk, milk powder, high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS)