首页> 中文期刊>分析化学 >固相萃取结合超高效液相色谱-串联质谱法同时检测食品中的6种工业染料

固相萃取结合超高效液相色谱-串联质谱法同时检测食品中的6种工业染料

     

摘要

An ultra high performance liquid chromatography-tandem mass spectrometric method was established for the simultaneous determination of the residues of six industrial dyes in foods. The samples were extracted with 50 mmol/L ammonium acetate solution containing 50% methanol and 1% formic acid, cleaned up by WAX solid phase extraction column, and then analyzed in multiple reaction monitoring (MRM) mode. Sample matrix-matched calibration was used to determine the residue contents by external standard. Orange Ⅱ was detected with negative ion model, and the other five dyes were detected with positive ion model. Limit of quantitation (LOQ) of Chrysoidine Ⅱ , Rho-damine B , Auramine O , Rhodamine 6G and Safranine T was 1. 6 ug/kg,and LOQ of orange II was 6.0 ug/kg. The linear range of chrysoidine Ⅱ, rhodamine B, auramine O, rhodamine 6G and safranine T was 1. 0-100. 0 μg/L and that of orange Ⅱ was 5. 0-100. 0 μg/L, the linear correlation coefficients were all more than 0. 999. The recoveries of 6 dyes ranged from 70. 3% to 109. 2% with relative standard deviations (RSD) of 2. 6% -14.1%. This method was simple, effective and sensitive, and was suitable for the determination and confirmation of six industrial dyes added in the foods illegally.%建立了超高效液相色谱-串联质谱(UPLC-MS/MS)同时检测食品中6种工业染料含量的方法.样品用含50%甲醇和1%甲酸的50 mmol/L乙酸铵溶液进行提取、WAX弱阴离子交换固相萃取柱进行净化后,采用多反应监测(MRM)模式进行检测,基质曲线外标法定量.其中酸性橙Ⅱ采用负离子模式检测,其余5种染料采用正离子模式检测.碱性橙Ⅱ、罗丹明B、碱性嫩黄O、罗丹明6G、碱性桃红T的定量限为1.6 μg/kg,酸性橙Ⅱ为6.0 μg/kg;碱性橙Ⅱ、罗丹明B、碱性嫩黄O、罗丹明6G、碱性桃红T的线性范围为1.0~100.0 μg/L;酸性橙Ⅱ的线性范围为5.0~100μg/L,线性相关系数均大于0.999.6种染料的回收率为70.3%~109.2%;相对标准偏差(RSD)为2.6%~14.1%.本方法灵敏度高,操作简单高效,适合于食品中6种非法添加工业染料的定量及确证分析.

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