首页> 中文期刊>分析测试学报 >高分辨快速液相色谱-串联质谱法测定肉制品中的刚果红

高分辨快速液相色谱-串联质谱法测定肉制品中的刚果红

     

摘要

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0.1-10mg/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 sam-ples 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 i-ons, 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.

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