液相色谱-质谱法测定熟肉制品中罗丹明B、碱性橙2和酸性橙Ⅱ

Simultaneous determination of Rhodamine B,Basic Orange 2 and Acid Orange Ⅱ in Deli meats by high perfoermance liquid chromatography coupled with tandem mass spectrometry

目的建立同时检测熟肉制品中3种非法添加工业染料罗丹明B、碱性橙2和酸性橙Ⅱ的液相色谱-质谱分析方法。方法使用Agilent Eclipse XDB-C_(18)分离柱(150 mm×3.0 mm,3.5μm),以0.1%甲酸水溶液-乙腈为流动相梯度洗脱,流速为0.3 ml/min。以电喷雾离子化源,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,罗丹明B和碱性橙2采用正离子模式检测。结果罗丹明B、碱性橙2和酸性橙Ⅱ的浓度为0μg/L^2.0μg/L时,线性关系良好,定量检出限分别为0.1 ng/g、0.5 ng/g、1.0 ng/g,方法保留时间和峰面积的相对标准偏差分别为0.06%~0.40%、1.37%~2.04%;加标回收率为91.0%~102.0%,相对标准偏差<6.0%。结论该方法操作简单高效,重现性较好,适合于烧卤食品、包装熟肉制品和火腿肠中3种非法添加工业染料的同时测定。

Objective To establish a method for the simultaneous determination of three illegally added industrial dyes（ Rhodamine B,Basic Orange 2 and Acid OrangeⅡ） in Deli meats by high performance liquid chromatography coupled with tandem mass spectrometry（ HPLC- MS）. Methods Separations were performed with an Agilent Eclipse XDB- C_（18） column at a flow rate of 0. 3 ml/min. The mobile phase was water（ containing 0. 1% formic acid）- acetonitrile. Using electrospray ionization source,the detection was conducted by MRM mode and quantified by matrix curve external standard method. Acid OrangeⅡadopted negative MRM mode while Rhodamine B and Basic Orange 2 adopted positive MRM mode for detection. Results Good linearity was obtained when the concentrations of Rhodamine B,Basic Orange 2 and Acid Orange Ⅱ were within 0 μg/L-2. 0 μg/L. The limits of quantification for Rhodamine B,Basic Orange 2and Acid Orange Ⅱ were 0. 1 ng/g,0. 5 ng/g,1. 0 ng/g,respectively. The relative standard deviations of reproducibility of this method for retention time and peak area were 0. 06%- 0. 40%,1. 37%- 2. 04%,respectively. The recoveries of adding standard were 91. 0%- 102. 0%,with the relative standard deviation of the method 〈 6. 0%. Conclusion The method is simple and high- efficient,repeatable and could be used for detecting 3 kinds of illegal industrial adding dyes simultaneously in unpacked marinated meats,packed cooked meats and sausage.