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 C18Rapid Resolution HD色谱柱(50mm×2.1mm,1.8μm)进行分离,流动相为95%(体积分数)甲醇,流速为0.2mL/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0.03～1mg/L浓度范围内,线性关系良好(相关系数为0.999 8),精密度良好(RSD小于5%),回收率为88%～91%,检出限约为0.01mg/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。
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 liq- uid 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 C）8 Rapid Resolution HD UPLC column （50 mm x2. 1 ram, 1.8 ~m） HPLC , using 95% （vol- ume 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. 999 8. 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.
出处
《色谱》
CAS
CSCD
北大核心
2013年第9期914-919,共6页
Chinese Journal of Chromatography
基金
江苏省质量技术监督局科技项目(KJ112501)
关键词
高效液相色谱-串联四极杆飞行时间质谱
超高效液相色谱-串联三重四极杆质谱
刚果红
牛肉
high performance liquid chromatography-tandem quadrupole time of flight massspectrometry （LC-QTOF MS）
ultra-high performance liquid chromatography-tandem triplequadrupole mass spectrometry （UPLC-MS/MS）
congo red
beef
