高效液相色谱-串联质谱法同时测定豆制品中6种违禁偶氮染料

Simultaneous Determination of Six Banned Azo-Dyes in Soybean Products by HPLC-MS/MS

  • 摘要: 为了快速、高效的检测豆制品中非法添加的偶氮染料,建立了高效液相色谱-串联质谱(HPLC-MS/MS)同时分析豆制品中6种偶氮染料(碱性橙Ⅱ、对位红、苏丹红Ⅰ~Ⅳ)的方法。样品用乙腈超声提取、取离心后的上清液直接进样分析,经Waters C18色谱柱分离,电喷雾串联质谱多反应监测(MRM)模式检测,空白基质曲线外标法定量。结果表明:6种染料在2~100 μg/L范围内呈良好的线性关系,线性相关系数R2均大于0.99;提取回收率为93.9%~110.6%,相对标准偏差为3.1%~14.8%;检测限(LOD)和定量限(LOQ)分别为0.03~0.75 μg/kg和0.1~2.0 μg/kg。该方法操作简单、灵敏度高、结果准确可靠,适用于豆制品中6种违禁偶氮染料的定量分析。

     

    Abstract: A sensitive and efficient method was developed for the simultaneous determination of six azo-dyes (Chrysoidin, Para Red, Sudan I, SudanⅡ, SudanⅢ and Sudan Ⅳ) in soybean products using high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The samples were extracted with a simple procedure using acetonitrile. The supernatant was directly analyzed by LC-MS/MS after centrifugation. The sample was separated on a Waters XTerra C18 column, and detected by MS/MS with the multiple reaction monitoring (MRM) mode. Matrix calibration was used for quantitative testing of the method. Good linearity is obtained over the range of 2-100 μg/L with a correlation coefficient R2>0.99. The recoveries are 93.9%-110.6% with good coefficients of variation of 3.1%-14.8%. Limit of detection (LOD) and limit of quantification (LOQ) for the six dyes are in the ranges of 0.03-0.75 μg/kg and 0.1-2.0 μg/kg, respectively. This method has been applied successfully for the determination of the six azo dyes in soybean products.

     

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