High performance liquid chromatography hyphenated to inductively coupled plasma mass spectrometry for V and Ni quantification as tetrapyrroles |
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Authors: | Christiane Bé atrice Duyck,Tatiana Dillenburg Saint'PierreNorbert Miekeley,Teresa Cristina Oliveira da FonsecaPeter Szatmari |
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Affiliation: | a Pontifícia Universidade Católica do Rio de Janeiro (PUC-Rio), R. Marquês de São Vicente, 225, Gávea, Rio de Janeiro, RJ, 22451-900, Brazilb Universidade Federal Fluminense (UFF), Campus do Valonguinho, Outeiro de São João Batista, s/n°, 24020-150, Niterói, RJ, Brazilc Centro de Pesquisas Leopoldo A. Miguez de Mello da Petrobras (CENPES), Av. Horácio Macedo, 950, Cidade Universitária, Rio de Janeiro, RJ, 21941-915, Brazil |
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Abstract: | A method was developed for the determination of V and Ni as tetrapyrroles by High Performance Liquid Chromatography hyphenated to Inductively Coupled Plasma Mass Spectrometry (HPLC-ICP-MS) using reversed phase and elution gradient. Chlorinated solvents and tetrahydrofuran were investigated as regard to separation time and ICP-MS detection efficiencies. The final elution gradient program started from pure methanol to a mixture of 20:80 (v/v) chloroform:methanol. External quantification of V and Ni with inorganic standards by flow injection ICP-MS, used online with HPLC, resulted in 95% of recoveries. The Limits of Detection for V during methanol elution and for Ni during the 20% chloroform gradient elution were evaluated by their minimum detectable concentrations, which were, respectively, 5 μg L− 1 and 8 μg L− 1. The methodology was applied to polar and resin fractions separated from a Brazilian crude oil and a sediment extract from an oil-polluted area in the Guanabara Bay, Rio de Janeiro, Brazil. Vanadium as tetrapyrroles represented the totality of V content in the polar fraction, whereas Ni was in different polar forms in the resin and sediment extract. |
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Keywords: | Reversed phase HPLC ICP-MS Flow injection Tetrapyrroles Porphyrins |
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