色谱

色谱 ›› 2010, Vol. 28 ›› Issue (11): 1026-1030.DOI: 10.3724/SP.J.1123.2010.01026

• 研究论文 • 上一篇    下一篇

柱后氨化-超高效液相色谱-串联质谱法测定牛奶和奶粉中的三聚氰酸

云环*, 张朝晖, 高洋洋, 何悦   

  1. 北京出入境检验检疫局技术中心, 北京 100026
  • 收稿日期:2010-08-09 修回日期:2010-09-19 出版日期:2010-11-28 发布日期:2010-11-28
  • 通讯作者: 云环,工程师,主要研究方向为食品中药物残留的分析.
  • 基金资助:

    无

Determination of cyanuric acid in milk and milk powder by ultra performance liquid chromatography-tandem mass spectrometry with post-column ammoniation

YUN Huan*, ZHANG Zhaohui, GAO Yangyang, HE Yue   

  1. Technology Center of Beijing Entry-Exit Inspection and Quarantine Bureau, Beijing 100026, China
  • Received:2010-08-09 Revised:2010-09-19 Online:2010-11-28 Published:2010-11-28

PDF

597

被引次数

9

摘要： 建立了一种柱后氨化-超高效液相色谱-串联质谱法(UPLC-MS/MS)测定牛奶和奶粉中三聚氰酸的分析方法。样品用5%三氯乙酸溶液提取,无需净化和浓缩,用Acquity UPLC HSS T3色谱柱(50 mm×2.1 mm, 1.8 μm)进行分离,以乙腈和水作为流动相进行梯度洗脱,柱后氨化,电喷雾负离子(ESI~)模式电离,多反应监测(MRM)模式进行检测。结果表明: 三聚氰酸在10.0～160.0 μg/L范围内线性关系良好(r≥0.99)。牛奶在0.05、0.10、0.20 mg/kg的添加浓度的回收率为60%～118.5%,相对标准偏差(RSD, n=6)为8.2%～12.6%;奶粉在0.25、0.50、1.00 mg/kg的添加浓度的回收率为88%～108%, RSD(n=6)为2.5%～5.7%。牛奶中方法的定量限(信噪比为10)为0.05 mg/kg,奶粉中为0.25 mg/kg。该方法快速、灵敏、准确,适合于牛奶、奶粉等乳及乳制品中三聚氰酸的快速、高灵敏度的分析检测。

关键词: 超高效液相色谱-串联质谱, 奶粉, 牛奶, 三聚氰酸, 柱后氨化

Abstract: A method for the determination of cyanuric acid in milk and milk powder has been developed by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) with post-column ammoniation. After extracted by 5% trichloroacetic acid, the samples were loaded onto an Acquity UPLC HSS T3 column (50 mm×2.1 mm, 1.8 μm) and separated with a gradient elution. The electrospray was operated in the negative mode and monitored by the multiple reaction monitoring (MRM) mode. The calibration curves showed a good linearity in the range of 10.0~160.0 μg/L, and the correlation coefficients (r) were higher than 0.99. When the spiked levels were 0.05, 0.10, and 0.20 mg/kg, the recoveries of cyanuric acid in milk ranged from 60% to 118.5%, with the relative standard deviations (RSDs) of 8.2%~12.6%; while the spiked levels were 0.25, 0.50, and 1.00 mg/kg in the milk powder, the recoveries ranged from 88% to 108% and the RSDs ranged from 2.5%~5.7%. The limits of quantification (LOQs, S/N=10) of cyanuric acid were 0.05 mg/kg in milk sample and 0.25 mg/kg in milk powder. The results indicate that the method is simple, rapid, sensitive and suitable for the qualitative and quantitative analyses of cyanuric acid in milk and milk powder samples.

Key words: cyanuric acid, milk, milk powder, ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), post-column ammoniation