高效液相色谱法同时测定抗疲劳保健食品中的3种违禁成分

目的 建立抗疲劳类保健食品中违禁成分咖啡因、西地那非和他达那非的高效液相色谱法。方法 样品中的待测组分经甲醇超声提取、过滤后,采用Welch C18柱(4.6 mm×250 mm,5 μm)为分离柱,以三乙胺溶液(取三乙胺7 ml,加水至1 L,并用磷酸调节pH值至4.0)(A)-乙腈(B)为流动相,梯度洗脱流速为1.0 ml/min；检测波长为280 nm；柱温为40 ℃,标准曲线法定量。结果 3种化合物分离度良好,线性相关系数均大于0.999 9,回收率为93.2 %～103.7 %,检出限为3.0～4.4 μg/g,定量限为8.9～13.2 μg/g。结论 本法简便、准确,可用于抗疲劳类保健食品中非法添加化学药物的检测。

Determination of three illegally added chemicals in antifatigue health foods by high-performance liquid chromatography

Objective To establish a method for the determination of three chemicals (icariin;sildenafil;tadalafil) illegally added in the antifatigue health foods by high-performance liquid chromatography. Methods The target chemicals in samples were ultrasonically extracted with methanol and filtrated. The separation was performed on a,Welch C18 column (4.6mm×250mm,5μm) and the mixture of triethylamine solution (triethylamine 7ml in 1L water and the pH was adjusted to 4.0 with phosphoric acid) (A)-acetonitrile (B) was used as mobile phase using gradient elution. The flow rate was 1ml/min,and the detection wavelength was 280nm. The column temperature was set at 40℃. Results The correlation coefficients of the method were above 0.9999. The recoveries were 93.2%～103.7%. The limits of detection were in the ranges of 3.0～4.4μg/g,and the limits of quantification were in the ranges of 8.9～13.2μg/g. Conclusion The method is convenient and accurate,which can be used for determination of three chemicals illegally added in the antifatigue health foods.