Optimization And Validation Of
A Chromatographic Methodology
For The Quantification Of PAHs In
Drinking Water Samples
Author(s)
A. S. Cardoso, S. A. Feliciano, M. H. Rebelo, S. S. José & C. Reis
Abstract
Polycyclic aromatic hydrocarbons (PAHs) are one of the most important
persistent organic toxic micropollutants present in water. These compounds are
essentially known for their carcinogenic, mutagenic and genotoxic properties,
especially the PAHs containing four or more aromatic rings.
The determination of these compounds in water is a challenging situation,
making it necessary to develop specific methods with very low detection limits.
This work describes the optimization and validation of a methodology for the
determination of the five PAHs proposed in the Portuguese legislation, using a
solid phase extraction technique followed by a reverse-phase high performance
liquid chromatography with fluorescence detection: benzo[b]fluoranthene,
benzo[k]fluoranthene, benzo[ghi]perylene, indene[1,2,3-cd]pyrene and
benzo[a]pyrene.
The performance of the methodology was tested in terms of linearity, limits of
detection and quantification, trueness, repeatability and intermediate precision,
following the recommendations of the international standard ISO/IEC 17025.
The method showed good linearity for the tested concentration range, with limits
of detection less than 0.29 ng/L for all the PAHs. Analytical recoveries,
repeatability and intermediate precision were calculated in ultra-pure, bottled and
tap water, with recoveries values ranging from 80 to 110%, repeatability and
precision RSD values less than 15%.
The methodology was applied to real water samples, fifty water springs from
Sintra municipality. In the samples analyzed, PAHs were detected under the
limits proposed by the legislation.
Keywords: drinking water, polycyclic aromatic hydrocarbons, SPE-HPLC-FLD,
validation, Natural spring waters.
Keywords
drinking water, polycyclic aromatic hydrocarbons, SPE-HPLC-FLD,
validation, Natural spring waters.
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