微波衍生-离子对高效液相色谱-磺化四苯基卟啉光度法同时测定痕量镍、铜、锰和锌

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用磺化四苯基卟啉 (TPPS4 )作柱前衍生试剂 ,在微波作用下进行衍生反应 ,研究了衍生和分离Ni2 + ,Mn2 + ,Zn2 + 和Cu2 + 的最佳条件。在 75 0W的微波作用下衍生反应 3min ,在C18柱上采用乙腈 水 (体积比为 2 2 5∶77 5 )体系作流动相 ,四乙基溴化铵 (TEABr)作离子对试剂 ,在 415nm处检测 ,建立了微波衍生 离子对高效液相色谱快速分离、光度检测Ni2 + ,Mn2 + ,Zn2 + 和Cu2 + 的新方法。络合物和反应试剂在 15min内出峰完毕。Zn2 + ,Cu2 + ,Ni2 + 和Mn2 + 的检测限分别为 0 0 5 μg/L ,0 0 1μg/L ,0 10 μg/L和 0 40 μg/L。所建立的方法用于茶叶样品的分析测定 ,结果令人满意。 The optimum conditions for the derivatization and separation of Ni2 +, Mn2 +, Zn2 + and Cu2 + were studied by derivatization reaction with sulfonated tetraphenylporphyrin (TPPS4) as pre-column derivatization reagent under microwave irradiation. The reaction was carried out under microwave irradiation of 75 0 W for 3 min. The mobile phase was acetonitrile on a C18 column with a volume ratio of 2: 5: 77 5. Tetraethylammonium bromide (TEABr) was used as the ion pair reagent at 415 nm , A new method for rapid determination of Ni2 +, Mn2 +, Zn2 + and Cu2 + by high performance liquid chromatography with microwave derivatization ion pair was established. Complex and reaction reagents peak out in 15min. The detection limits of Zn2 +, Cu2 +, Ni2 + and Mn2 + were 0 0 5 μg / L, 0 0 1 μg / L, 0 10 μg / L and 0 40 μg / L, respectively. The established method was applied to the analysis of tea samples and the results were satisfactory.
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