On-line methodology for the trace level determination of the chlorinated phenol family in water samples


  • Ana María Núñez-Gaytán Universidad Nacional Autónoma de México ; Universidad Michoacana de San Nicolás Hidalgo
  • Luz Elena Vera-Ávila Universidad Nacional Autónoma de México
  • María del Rosario Covarrubias-Herrera Universidad Nacional Autónoma de México




chlorophenols, water analysis, on-line methodology, solid-phase extraction, liquid chromatography


On-line solid-phase extraction – liquid chromatography (SPE-HPLC) methodology was developed for the trace level determination of phenol and 19 chlorophenols in water samples. A small precolumn packed with polymeric adsorbent was placed in a switching valve and used for sample extraction and preconcentration; the trapped compounds were further on-line eluted and analyzed by reversed phase HPLC with UV and coulometric detection. Because of wide differences in hydrophobic character, SPE of the least (phenol and monochlophenols), the medium (di- and trichlorophenols) and the most chlorinated phenols (tetra- and pentachlorophenol) was performed using different sample volume (15-25 mL) and sample composition (0-10% methanol addition). Under these conditions, solute recoveries were ≥ 82% (except phenol, 72%) for concentrations in the range ~3-75 ng/mL. Applying recovery factors, excellent accuracy (100%) and precision (RSD < 6.5%) were achieved for the 20 compounds of interest in replicate analysis (n = 7) of spiked reagent water samples. Method detection limits were 0.5-1 ng/mL with the UV detector and 0.1-0.3 ng/mL with the coulometric detector.


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Author Biographies

Ana María Núñez-Gaytán, Universidad Nacional Autónoma de México ; Universidad Michoacana de San Nicolás Hidalgo

Facultad de Química, Departamento de Química Analítica ; Facultad de Ingeniería Química, Departamento de Química

Luz Elena Vera-Ávila, Universidad Nacional Autónoma de México

Facultad de Química, Departamento de Química Analítica

María del Rosario Covarrubias-Herrera, Universidad Nacional Autónoma de México

Facultad de Química, Departamento de Química Analítica


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