色谱

色谱 ›› 2013, Vol. 31 ›› Issue (9): 914-919.DOI: 10.3724/SP.J.1123.2013.03043

• 技术与应用 • 上一篇    下一篇

液相色谱-串联四极杆飞行时间质谱和超高效液相色谱-串联三重四极杆质谱用于检测牛肉中的刚果红

林慧1,2, 徐春祥1, 颜春荣1, 张征1, 王岁楼2   

  1. 1. 江苏省产品质量监督检验研究院, 江苏 南京 210007;
    2. 中国药科大学, 江苏 南京 210009
  • 收稿日期:2013-03-22 修回日期:2013-04-24 出版日期:2013-09-28 发布日期:2013-09-02
  • 通讯作者: 徐春祥, 王岁楼
  • 基金资助:

    江苏省质量技术监督局科技项目(KJ112501).

Determination of congo red in beef by high performance liquid chromatography-tandem quadrupole time of flight mass spectrometry and ultra-high performance liquid chromatography-tandem triple quadrupole mass spectrometry

LIN Hui1,2, XU Chunxiang1, YAN Chunrong1, ZHANG Zheng1, WANG Suilou2   

  1. 1. Jiangsu Product Quality Testing and Inspection Institute, Nanjing 210007, China;
    2. China Pharmaceutical University, Nanjing 210009, China
  • Received:2013-03-22 Revised:2013-04-24 Online:2013-09-28 Published:2013-09-02

PDF

315

被引次数

10

摘要：

建立了牛肉中刚果红的检测方法。定性方法采用液相色谱-串联四极杆飞行时间质谱对未知物进行质谱谱图库匹配,定量分析采用超高效液相色谱-串联三重四极杆质谱。牛肉样品中的刚果红经液液萃取净化后,采用Agilent ZORBAX Eclipse Plus C18 Rapid Resolution HD色谱柱(50 mm×2.1 mm, 1.8 μm)进行分离,流动相为95%(体积分数)甲醇,流速为0.2 mL/min。AB 4000+三重四极杆质谱仪在电喷雾负离子化(ESI)及MRM模式下定量。结果显示,刚果红在0.03~1 mg/L浓度范围内,线性关系良好(相关系数为0.9998),精密度良好(RSD小于5%),回收率为88%~91%,检出限约为0.01 mg/L。本方法快速简便,重现性好,可以为牛肉及其他肉制品中刚果红的定量提供良好的解决方案。

关键词: 超高效液相色谱-串联三重四极杆质谱, 刚果红, 高效液相色谱-串联四极杆飞行时间质谱, 牛肉

Abstract:

A method was developed for the determination of congo red in beef. The analyte was identified by high performance liquid chromatography-tandem quadrupole time of flight mass spectrometry (LC-QTOF MS) and quantitatively determined by ultra-high performance liquid chromatography-tandem triple quadrupole mass spectrometry. After purified by liquid-liquid extraction, the congo red in the beef sample was separated on an Agilent ZORBAX Eclipse Plus C18 Rapid Resolution HD UPLC column (50 mm×2.1 mm, 1.8 μm) HPLC, using 95% (volume percentage) methanol as the mobile phase at 0.2 mL/min. The detection was performed on an AB 4000+ triple quadrupole mass spectrometer utilizing electrospray ionization (ESI) interface operated in negative ion mode and multiple-reaction monitoring (MRM) mode. The results showed that the linear range of congo red mass concentration was 0.03-1 mg/L with the correlation coefficient of 0.9998. The method had a good precision with the RSDs lower than 5% and the recoveries ranging from 88% to 91%. The limit of detection (LOD) of congo red was 0.01 mg/L. With good reproducibility, the method is simple, fast and effective for the determination of the illegally added congo red in beef and other meat products.

Key words: beef, congo red, high performance liquid chromatography-tandem quadrupole time of flight mass spectrometry (LC-QTOF MS), ultra-high performance liquid chromatography-tandem triple quadrupole mass spectrometry (UPLC-MS/MS)

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