超高效液相色谱法检测咸鸭蛋中苏丹红的含量

Determination of Sudan Red in salted duck eggs by UPLC

目的构建一种超高效液相色谱法测定咸鸭蛋中苏丹红(Ⅰ、Ⅱ、Ⅲ、Ⅳ)含量的分析方法,为食品中苏丹红含量的检测提供依据。方法随机采集市售咸鸭蛋,参照GB/T 19681-2005的方法,样品经溶剂提取、固相萃取净化后,以BEH C18(50 mm×2.1 mm,1.7μm)为色谱柱,乙腈-水为流动相,设定苏丹红Ⅰ检测波长478 nm,苏丹红Ⅱ、Ⅲ、Ⅳ检测波长520 nm,流速均为0.4 m L/min进行检测;并评价本方法的最低检出限、线性范围、精密度和回收率。结果空白检品无干扰,苏丹红Ⅰ、Ⅱ、Ⅲ、Ⅳ单标和混标均分离较好,且均在1.3 min内完全分离。本方法的最低检出限为3.28μg/kg,苏丹红Ⅰ、Ⅱ、Ⅲ、Ⅳ在1.6μg/m L～25.6μg/m L内浓度与峰面积呈良好的线性关系,相关系数均大于0.999;相对标准偏差在0.87%～1.97%;加标回收率在81.78%～88.32%。结论本方法具有快速、简便、准确度和灵敏度高等优点,适用于咸鸭蛋中苏丹红含量的检测。

Objective Objective To develop a method for determination of SudanⅠ,Ⅱ,Ⅲ and Ⅳ in salted duck eggs by ultra performance liquid chromatography (UPLC),which can provide a basis for the determination of Sudan in food. Methods The salted duck eggs were collected randomly in market. According to the method of GB/ T 19681-2005, the samples were extracted by the solvent and purified by solid phase. BEH C18(50 mm×2.1 mm,1.7 μm) was used as the chromatographic column,the acetonitrile-water was used as mobile phase for gradient elution. Sudan Ⅰ was detected by ultraviolet detector with 478 nm wavelength, Sudan Ⅱ,Ⅲ and Ⅳ was detected by ultraviolet detector with 520 nm wavelength. The flow rate of Sudan Ⅰ,Ⅱ,Ⅲ and Ⅳ was 0.4 mL/ min. The minimum detectability, linear range, precision and recovery were evaluated.Results There was no interference in the blank sample.The single standards and mixed standards of Sudan Ⅰ,Ⅱ,Ⅲ and Ⅳ have a good separation, which were separated completely in 1.3 min. The minimum detectability is 3.28 μg/ kg.Good linearity was obtained when the mass concentration of Sudan Ⅰ,Ⅱ,Ⅲ and Ⅳ among 1.6 μg/ mL ~ 25.6 μg/ mL.The correlation coefficients were all>0.999,the relative standard deviations were among 0.87%~1.97%, and the average recoveries were among 81.78%~88.32%. Conclusion This method is rapid, simple,accurate and has high sensitivity. Therefore, the method can be suitable for the determination of Sudan in salted duck eggs.