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      Determination of Pentachlorophenol and Hexachlorobenzene in Natural Waters Affected by Industrial Chemical Residues

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          Abstract

          This paper presents the development of a methodology for the simultaneous analysis of pentachlorophenol and hexachlorobenzene in natural waters affected by industrial residues, as its principal goal. Samples were collected in Quarentenário, São Vicente city, where most of the population utilize wells for their supply. The liquid-liquid extraction employed to remove PCP and HCB from the matrix for further identification and quantification, showed very good recovery and repeatability. The recovery range was between 81.5% and 103.0%, with a relative standard deviation of 2.4% and 4.1% for a fortification level of 10 ng L-1. In addition, organochlorine compounds were determined by GC-ECD and/or GC-MS. The limit of quantification was 5 ng L-1 for PCP and 2 ng L-1 for HCB, which are below the maximum level allowed by the EC directives for pesticide residues in drinking water.

          Translated abstract

          Este trabalho teve como principal objetivo o desenvolvimento de uma metodologia para a análise simultânea de pentaclorofenol (PCP) e hexaclorobenzeno (HCB) em água natural de subsuperfície proveniente de uma região afetada por resíduos industriais (São Vicente-SP), onde a maior parte da população se utiliza de poços pouco profundos para o abastecimento. A extração líquido-líquido apresentou bons resultados quanto à recuperação e repetibilidade do método. Para o nível de fortificação de 10 ng L-1 de PCP e HCB a recuperação situou-se entre 81.5% e 103.0%, com um desvio padrão relativo de 2.4% a 4.1%. A determinação dos analitos foi efetuada por GC-ECD e/ou GC-MS. Adicionalmente, o limite de quantificação do método foi de 5 ng L-1 para PCP e 2 ng L-1 para HCB, valores que estão abaixo do nível máximo permitido pelas diretrizes da Comunidade Européia para resíduos de pesticidas em água potável.

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          Most cited references28

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          Guidelines for Drinking Water Quality

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            Fully automated on-line two-dimensional liquid chromatography in combination with ESI MS/MS detection for quantification of sugar phosphates in yeast cell extracts.

            A mass spectrometric quantitative assay was developed for the analysis of 10 sugar phosphates in the yeast Pichia pastoris. As a novelty, two-dimensional chromatography based on a fully automated heart-cutting LC-LC technique was introduced. Using a ten-port valve, ten fractions of the first chromatographic dimension, i.e. anion exchange chromatography (AEC), were transferred and separated by the orthogonal second dimension, i.e. separation on porous graphitized carbon. The chromatographic separation on the second dimension was optimized for each transferred fraction minimizing the separation time and ensuring complete removal of the salt constituents of the AEC eluents. The latter being crucial for electrospray mass spectrometric detection was confirmed by combining the LC-LC separation with on-line ICP-MS detection. These measurements showed that sodium elution was completed after 0.8 min. Consequently, an analysis time of 1 min per transferred peak was established. In this way, the excellent peak capacity given by ion exchange could be conserved in the second dimension at the same time enabling mass spectrometric detection. Sub-μM limits of detection could be obtained by the new LC-LC-MS/MS methods ranging between 0.03 and 0.19 μM for the investigated compounds (only 3GAP showed a LOD of 1 μM). The method was applied to the quantification of ten sugar phosphates in yeast extracts utilizing internal standardization with a fully labeled (13)C yeast extract. Typically, the standard uncertainties for N = 3 replicates assessed by the LC-LC-MS/MS set-up were <5%.
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              Purification of laboratory chemicals

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                Author and article information

                Contributors
                Role: ND
                Role: ND
                Role: ND
                Role: ND
                Role: ND
                Journal
                jbchs
                Journal of the Brazilian Chemical Society
                J. Braz. Chem. Soc.
                Sociedade Brasileira de Química (São Paulo )
                1678-4790
                January 1999
                : 10
                : 1
                : 25-30
                Affiliations
                [1 ] Universidade de São Paulo Brazil
                Article
                S0103-50531999000100005
                10.1590/S0103-50531999000100005
                6bde7707-72de-4717-abbd-dd67e0a5fb5f

                http://creativecommons.org/licenses/by/4.0/

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                Product

                SciELO Brazil

                Self URI (journal page): http://www.scielo.br/scielo.php?script=sci_serial&pid=0103-5053&lng=en
                Categories
                CHEMISTRY, MULTIDISCIPLINARY

                General chemistry
                pentachlorophenol,hexachlorobenzene,organochlorine compounds
                General chemistry
                pentachlorophenol, hexachlorobenzene, organochlorine compounds

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