摘要
研究了用四 (对甲基苯基 ) 卟啉柱前衍生、固相萃取富集、高效液相色谱法测定烟草中痕量Pb、Cd、Hg的方法。烟草样品用微波消化后 ,用四 (对甲基苯基 ) 卟啉 (T4MPP)柱前衍生 ,用WatersSep Park C1 8固相萃取微柱萃取富集Pb、Cd、Hg的T4MPP络合物 ,富集倍数为 5 0倍 ;然后用甲醇 (内含 0 .0 1mol L四氢吡咯 醋酸缓冲盐 (pH =1 0 ) )和四氢呋喃 (内含 0 .0 1mol L四氢吡咯 醋酸缓冲盐 (pH =1 0 ) )梯度洗脱为流动相 ,WatersXterraTMRP1 8(3 .9(1 5 0 )色谱柱为固定相分离 ,用二极管矩阵检测器检测 ;Pb、Cd、Hg的含量在 1～ 1 2 0 μg L范围内与峰面积呈线性关系 ,根据信噪比 (S N =3 ) ,方法检测限为 :Pd 0 .3 μg L、Cd 0 .5 μg L和Hg0 .3 μg L ,方法相对标准偏差为 2 .6%～ 4 .1 % ,标准回收率为 91 %～1 0 7% ,该方法用于测定烟草中的Pb、Cd、Hg。
A new method for the solid phase extraction followed by high performance liquid chromatographic determination of lead, cadmium and mercury was studied. Lead, cadmium and mercury were pre-column derived by Tera-(4-Methylphenyl)-porphine (T4MPP). These chelates can be extracted by Waters Sep-Park-C-18 cartridge and eluted by terahydrofuran (THF) (contain 0.01 mol/L prolidine-acetic acid buffer (pH = 10)). The chelates can be separated on a Waters Xterra(TM).RP18 chromatographic column (5 mum, 3.9 x 150) with methanol (contain 0.01 mol/L prolidine-acetic acid buffer (pH = 10)) and THF (contain 0.01 mol/L prolidineacetic acid buffer (pH = 10)) binary mixture gardient elution as mobile phase, and monitored with photodiode array dector. The linearity range of lead, cadmium and mercury is 1 similar to 120 mug/L. The detection limit (S/N = 3) is 0.5 mug/L for lead, 0.3 mug/L for cadmium and 0.5 mug/L for mercury. The relative standard dervaitions are 2.6% similar to 4.1%, and the recoveries are 91% similar to 107%. This method can be applied to the determination of microamount of lead, cadmium and mercury in tobacco with satisfactory results.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2003年第4期463-466,共4页
Chinese Journal of Analytical Chemistry
