Optimization of diclofenac quantification from wastewater treatment plant sludge by ultrasonication assisted extraction

J Chromatogr B Analyt Technol Biomed Life Sci. 2014 May 1;958:48-54. doi: 10.1016/j.jchromb.2014.02.047. Epub 2014 Apr 1.


A rapid quantification method of diclofenac from sludge samples through ultrasonication assisted extraction and solid phase extraction (SPE) was developed and used for the quantification of diclofenac concentrations in sludge samples with liquid chromatography/tandem mass spectrometry (LC-MS/MS). Although the concentration of diclofenac in sludge samples taken from different units of wastewater treatment plants in Istanbul was below the limit of quantification (LOQ; 5ng/g), an optimized method for sludge samples along with the total mass balances in a wastewater treatment plant can be used to determine the phase with which diclofenac is mostly associated. Hence, the results will provide information on fate and transport of diclofenac, as well as on the necessity of alternative removal processes. In addition, since the optimization procedure is provided in detail, it is possible for other researchers to use this procedure as a starting point for the determination of other emerging pollutants in wastewater sludge samples.

Keywords: LC–MS/MS; Method; Micropollutants; Pharmaceutical; Solid phase extraction; Ultrasonication.

Publication types

  • Evaluation Study
  • Research Support, Non-U.S. Gov't

MeSH terms

  • Chromatography, Liquid / methods
  • Diclofenac / isolation & purification*
  • Limit of Detection
  • Sewage / analysis*
  • Solid Phase Extraction / methods*
  • Sonication / methods*
  • Tandem Mass Spectrometry / methods
  • Wastewater / analysis
  • Water Pollutants, Chemical / isolation & purification*


  • Sewage
  • Waste Water
  • Water Pollutants, Chemical
  • Diclofenac