Preconcentration of pharmaceuticals residues in sediment samples using microwave assisted micellar extraction coupled with solid phase extraction and their determination by HPLC-UV

J Chromatogr B Analyt Technol Biomed Life Sci. 2008 Feb 15;863(1):150-7. doi: 10.1016/j.jchromb.2008.01.026. Epub 2008 Jan 20.

Abstract

An analytical method combining microwave assisted micellar extraction (MAME) and solid phase extraction (SPE) has been developed to extract and preconcentrate a selected group of eight pharmaceutical compounds in sediment samples prior to their determination using liquid chromatography with an UV-DAD detector. A non-ionic surfactant, Polyoxyethylene 10 lauryl ether (POLE) was used for the MAME extraction and the different parameters for the optimization process were studied. Then, SPE was used to clean-up and preconcentrate the target analytes in the extract, prior to their determination using HPLC-UV. The method was applied to the determination of the selected pharmaceuticals compounds in several kinds of sediment samples with different characteristics. Relative recoveries for spiked sediment samples were over 70% and relative standard deviations (RSDs) were under 11% for all recoveries tested. Detection limits between 4 and 167ngg(-1) were obtained. The method was validated using Soxhlet extraction procedure.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Calibration
  • Chemical Phenomena
  • Chemistry, Physical
  • Chromatography, High Pressure Liquid
  • Drug Residues / analysis*
  • Geologic Sediments / analysis*
  • Indicators and Reagents
  • Micelles
  • Microwaves
  • Polidocanol
  • Polyethylene Glycols
  • Quality Control
  • Soil / analysis
  • Soil Pollutants / analysis*
  • Solid Phase Extraction
  • Spain
  • Spectrophotometry, Ultraviolet

Substances

  • Indicators and Reagents
  • Micelles
  • Soil
  • Soil Pollutants
  • Polidocanol
  • Polyethylene Glycols