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凌睿, 胡文彦, 乔玲. 高分辨快速液相色谱-串联质谱法测定肉制品中的刚果红[J]. 分析测试学报, 2012,31(6):730-733.
Determination of Congo Red in Meat Products by Rapid Resolution Liquid Chromatography-Tandem Mass Spectrometry[J]. 2012,31(6):730-733.
建立了肉制品中刚果红的高分辨快速液相色谱-串联质谱(RRLC-MS/MS)测定方法。均质后的样品经乙腈与正己烷混合溶剂(1∶1)提取,乙腈提取层离心后直接上机测试。使用Agilent XDB C18色谱柱,以乙腈和10 mmol/L甲酸铵水溶液为流动相梯度洗脱,采用多反应监测方式(MRM)负离子模式检测,定量离子对与定性离子对分别为m/z 325.0/416.0与m/z 651.0/152.0,外标法定量。结果表明,刚果红在0.1~10 mg/L范围内线性关系良好(r2>0.999),加标回收率为91%~102%,RSD为1.2%~4.0%,检出限与定量下限分别为0.07 mg/kg和0.18 mg/kg。该方法准确、高效,可用于肉制品中刚果红染料的快速检测。
A rapid resolution liquid chromatography-tandem mass spectrometric(RRLC-MS/MS) method was firstly developed for the determination of Congo red in meat products.Homogenized samples were extracted with acetonitrile-n-hexane mixture(1∶1) and the acetonitrile extraction were transferred for immediate testing after centrifugated by 15 000 r/min for 10 min.The target compound was separated on an Agilent XDB C18 column with acetonitrile-10 mmol/L ammonium formate as mobile phase by gradient elution,and determined by tandem mass spectrometry with multiple reaction monitoring(MRM) mode under negative electrospray ionization mode.The two precursor-product ion pairs,m/z 325.0/416.0 and m/z 651.0/152.0,were used as the quantizative and qualificative ions,respectively.The external standard method was used for quantitative analysis.The results showed a good linearity in range of 0.1-10 mg/L with correlation coefficients higher than 0.999.The average recoveries of three spiked levels including high,medium and low concentrations were between 91% and 102%,with relative standard deviations(RSDs) of 1.2%-4.0%.The limits of detection(LODs) and limits of quantitation(LOQs) were 0.07 mg/kg and 0.18 mg/kg,respectively.The proposed method was accurate and high efficient,and could meet the requirements for the rapid detection of Congo red in meat products.
刚果红高分辨快速液相色谱-串联四极杆质谱肉制品
Congo redRRLC-MS/MSmeat products
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