【摘要】 研究了用固相萃取富集,快速分离柱高效液相色谱法测定中草药中4种重金属元素:镍、铅、镉、汞的方法.中草药样品用微波消化,样品消化液中的镍、铅、镉、汞用四-(间氨基苯基)-卟啉(T2APP)柱前衍生,然后用ZORBAX RP18固相萃取小柱萃取富集镍、铅、镉、汞的T2-APP络合物,富集倍数为50倍;经富集后的络合物用乙腈和0.05 mol.L-1pH=10.0四氢吡咯-醋酸缓冲液(92/8)为流动相,ZORBAX Stab le Bound(4.6mm×50 mm,1.8μm)快速分离柱为固定相分离,用二极管矩阵检测器检测.镍、铅、镉、汞的检测限分别为:4,4,3,2 ng.L-1,分离4种重金属元素络合物的时间只需2.0 m in.方法相对标准偏差为1.8%~3.4%,标准回收率为88%~103%.更多还原

【Abstract】 A new method for determination of nickel,lead,cadmium and mercury by solid phase extraction and high performance liquid chromatography was studied.The nickel,lead,cadmium and mercury ions were pre-column derived by tera-（2-aminophenyl）-porphine（T₂APP）.These chelates were enriched by solid phase extraction with C₁₈ cartridge and the enrichment factor of 50 was achieved. The chelates were separated on a ZORBAX Stable Bound（4.6mm×50 mm,1.8 μm） by gradient elution with methanol and THF as mobile phase at a flow rate of 2.0 mL/min and detected with photodiode array detector from 350 600 nm.The detection limits of nickel,lead,cadmium and mercury are 4,4,3 and 2 ng·L^-1,respectively.This method had been applied to the determination of nickel,lead,cadmium and mercury in Chinese herb with good results.更多还原