食品科学 ›› 2003, Vol. 24 ›› Issue (4): 125-128.

• 分析检测 • 上一篇    下一篇

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

 台希, 胡秋芬, 尹家元, 杨光宇   

  1. 玉溪师范学院化学系,云南大学化学系
  • 出版日期:2003-04-15 发布日期:2011-12-13

Studies on Determination of Lead, Cadmium and Mercury in Foodstuff with High Performance Liquid Chromatography

 TAI  Xi, HU  Qiu-Fen, YIN  Jia-Yuan, YANG  Guang-Yu   

  • Online:2003-04-15 Published:2011-12-13

摘要: 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。

关键词: 四-(对甲基苯基)-卟啉, 铅, 镉, 汞, 高效液相色谱法

Abstract: A new method for the determination of lead, cadmium and mercury wi th high performance liquid chromatography was studied. The lead, cadmium and mercu ry was pre-column derived with tera-(4-methylphenyl)-porphine (T4MPP). The c haletes can be separated on a Waters XterraTM RP18 chromatographic column (5m, 3 .9×150, 5) with methanol (containing 0.01 mol/L prolidine-acetic acid bu ff er salt) and THF (containing 0.01 mol/L prolidine-acetic acid buffer salt) b ina ry mobile phase gardient elution as mobile phase, and monitored with photodi ode array detector. The linearity range of lead, cadmium and mercury are 0.01~ 3 mg/ L. The detection limits (S/N=3) are lead 2.3/L and m ercur y 2.5/L. The relative standard deviations are 2.1%~3.5%, and the rec overie s are 93%~106%. This method was applied to the determination of lead, cadmium and mercury in food with good results.

Key words: tera-(4-methylphenyl)-porphine, lead, cadmium, mercury, high per fo rmance liquid chromatography