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在线柱富集-反相高效液相色谱法分离金属四-(4-溴苯基)卟啉螯合物测定痕量铅、镉和汞。

Determination of trace lead, cadmium and mercury by on-line column enrichment followed by RP-HPLC as metal-tetra-(4-bromophenyl)-porphyrin chelates.

机构信息

Department of Chemistry, Yunnan University, 650091, Kunming, People's Republic of China; Department of Chemistry, Yuxi Normal College, 653100, Yuxi, People's Republic of China.

出版信息

Talanta. 2002 Jun 10;57(4):751-6.

PMID:18968677
Abstract

This paper reports the utilization of tetra-(4-bromophenyl)-porphyrin (T(4)BPP) as a chelating reagent using Waters Xterratrade mark RP(18) column for the on-line column enrichment and the separation of trace lead, cadmium and mercury ions by reversed-phase high-performance liquid chromatography (RP-HPLC) with photodiode array detector. When the Hg-T(4)BPP, Pb-T(4)BPP and Cd-T(4)BPP chelates were injected into the injector and sent to the enrichment column with 0.05 mol l(-1) of pH 10.0 pyrrolidine-phosphoric acid buffer solution (containing 10% of tetrahydrofuran (THF)) as mobile phase. The chelates were retained on the top of the enrichment column. After the enrichment is finished, by switching the valve of six-ports switching valve, the retained metal-T(4)BPP chelates will be eluted by mobile phase in reverse direction and will travel towards analytical column. With THF (containing 0.05 mol l(-1), pH 10.0 pyrrolidine-phosphoric acid buffer salt) and 0.05 mol l(-1), pH 10.0 pyrrolidine-phosphoric acid buffer solution (containinging 10% THF) gradient elution as mobile phase, the chelates separation on the analytical column was satisfactory. The linearity ranges are 0.01-120 mug l(-1) for each metal ion. The detection limits (S/N=3) of lead, cadmium and mercury are 1.0, 0.5 and 1.0 ng l(-1), respectively. This method can be applied to the determination (mug l(-1)) level of lead, cadmium and mercury in drinking water with satisfactory results.

摘要

本文报道了利用四-(4-溴苯基)卟啉(T(4)BPP)作为螯合试剂,采用 Waters Xterratrade 商标 RP(18)柱,通过反相高效液相色谱(RP-HPLC)与光电二极管阵列检测器,对痕量铅、镉和汞离子进行在线柱富集和分离。当 Hg-T(4)BPP、Pb-T(4)BPP 和 Cd-T(4)BPP 螯合物注入进样器并以 0.05 mol l(-1) pH 10.0 吡咯烷-磷酸缓冲溶液(含 10%四氢呋喃(THF))作为流动相输送到富集柱时,螯合物被保留在富集柱的顶部。富集完成后,通过切换六通切换阀的阀,保留的金属-T(4)BPP 螯合物将被反向流动相洗脱,并向分析柱移动。采用 THF(含 0.05 mol l(-1),pH 10.0 吡咯烷-磷酸缓冲盐)和 0.05 mol l(-1),pH 10.0 吡咯烷-磷酸缓冲溶液(含 10%THF)梯度洗脱作为流动相,在分析柱上对螯合物进行了满意的分离。每个金属离子的线性范围为 0.01-120 mug l(-1)。铅、镉和汞的检测限(S/N=3)分别为 1.0、0.5 和 1.0 ng l(-1)。该方法可应用于饮用水中铅、镉和汞的测定(mug l(-1))水平,结果令人满意。

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