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Method development and validation for phenol and nitrophenols in tap water by HPLC using a monolithic column

M.M. Cledera-Castro, A. Santos-Montes, R. Izquierdo-Hornillos

LC-GC Europe Vol. 19, nº. 7, pp. 424 - 431

Summary:

An isocratic HPLC method for the determination of phenol and nitrophenols (4-nitrophenol, 2-nitrophenol, 4,6-dinitro-o-cresol and 2,4-dinitrophenol) has been developed and validated using 2-chlorophenol as internal standard (IS) and a monolithic column in tap water samples. Prior to HPLC, the method requires solid-phase extraction (SPE) using polymeric Lichrolut EN cartridges. The method development involved the study of methanol and acetonitrile as organic modifiers, pH and flow-rate using a Chromolith RP-18e (150 mm × 4.6 mm I.D.) column. After comparing the performance of the separations obtained with both organic modifiers, the optimum separation of these compounds was achieved using 50 mM acetate buffer (pH 5.0)-acetonitrile (80:20, v/v) as mobile phase, 3 mL min-1 flow-rate and UV detection at maximum absorbance wavelength. Under these conditions, all analytes were separated (Rs > 2.0) in an analysis time of less than 3.5 min and the most important validation parameters were evaluated. The recoveries obtained in the accuracy test for all phenols studied were in the 90–112\% range using a preconcentration factor of 40, and the intraday and interday precisions [expressed as coefficient of variation (CV)] were smaller than 15\%. Finally, the proposed method was applied to wastewater samples from several industries.


Published on paper: January 2006.

Published on-line: July 2006.



Citation:
M.M. Cledera-Castro, A. Santos-Montes, R. Izquierdo-Hornillos, Method development and validation for phenol and nitrophenols in tap water by HPLC using a monolithic column. LC-GC Europe. Vol. 19, nº. 7, pp. 424 - 431, January 2006. [Online: July 2006]


    Research topics:
  • Experimental analysis

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