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研究了用四-(对甲基苯基)-卟啉柱前衍生,高效液相色谱法测定食品中痕量铅、镉、汞的方法。食品样品用湿法消化后,消化液中的铅、镉、汞用四-(对甲基苯基)-卟啉(T4MPP)柱前衍生,然后用甲醇(内含0.01mol/L四氢吡咯-醋酸缓冲盐)和四氢呋喃(内含0.01mol/L四氢吡咯-醋酸缓冲盐)为流动相梯度洗脱,WatersXterraTMRP18(3.9150mm,5μm)色谱柱为固定相分离铅、镉、汞的T4MPP络合物,用二极管矩阵检测器检测,铅、镉、汞含量在0.01～3mg/L范围内与峰面积成线性关系,根据信噪比(S/N=3),方法检测限为:铅2.3μg/L、镉1.8μg/L和汞2.5μg/L,方法相对标准偏差为2.1%～3.5%,标准回收率为93%～106%,该方法用于测定食品中的铅、镉、汞,结果令人满意。
A method for the determination of trace amounts of lead, cadmium and mercury in foods using tetra - (p - methylphenyl) - porphyrin precolumn derivatization and high performance liquid chromatography was studied. After wet digestion of food samples, lead, cadmium and mercury in the digestion solution were pre-column derivatized with tetrakis- (p-methylphenyl) -porphyrin (T4MPP) and then eluted with methanol (containing 0.01 mol / L tetrahydropyrrole - acetate buffer) and tetrahydrofuran (containing 0.01mol / L tetrahydropyrrole - acetate buffer) as the mobile phase. The WatersXterra TMRP18 (3.9150mm, 5μm) column was used to separate T4MPP The content of lead, cadmium and mercury in the range of 0.01 ~ 3 mg / L was linear with the peak area. The detection limit of the method was 2.3 for the signal to noise ratio (S / N = 3) μg / L, cadmium 1.8μg / L and mercury 2.5μg / L. The relative standard deviations were 2.1% ~ 3.5% and the standard recoveries were 93% -106% .The method was applied to the determination of lead, cadmium and mercury in food , The result is satisfactory.