Gas chromatography-mass spectrometry determination of earthy-musty odorous compounds in waters by two phase hollow-fiber liquid-phase microextraction using polyvinylidene fluoride fibers

J Chromatogr A. 2014 Feb 14:1329:45-51. doi: 10.1016/j.chroma.2014.01.002. Epub 2014 Jan 13.

Abstract

A rapid and sensitive method for the determination of earthy-musty odorous compounds, 2-methylisoborneol, 2-isopropyl-3-methoxy pyrazine, 2,4,6-trichloroanisole, 2,3,6-trichloroanisole, and geosmin, in water samples has been developed. The method was based on coupling a new polyvinylidene fluoride (PVDF) hollow-fiber liquid-phase microextraction system with gas chromatography-mass spectrometry (GC-MS). The PVDF hollow fibers have high porosity and an enhanced solvent compatibility for extraction of the target analytes. Experimental conditions were optimized by investigating the type of extraction solvent, sample pH, sodium chloride concentration, stirring speed, extraction time, and GC-MS conditions. Under optimized conditions, the earthy-musty odorous compounds exhibited good linearity (R>0.995) in the concentration range of 6.2-250ng/L. The repeatability and reproducibility of the method were lower than 6.8% and 9.8%, respectively. The limit of detection and limit of quantification values were lower than 2.0 and 6.2ng/L, respectively. The analysis of different water samples such as tap, pond, rive and waste water indicated minimal matrix effects. Analyte recoveries for real samples spiked at different concentrations were between 84.4% and 117.5%.

Keywords: Gas chromatography–mass spectrometry; Hollow-fiber liquid-phase microextraction; Odorous compounds; Polyvinylidene fluoride; Waters.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Gas Chromatography-Mass Spectrometry / methods*
  • Hydrogen-Ion Concentration
  • Liquid Phase Microextraction / methods*
  • Odorants / analysis*
  • Polyvinyls / chemistry*
  • Reproducibility of Results
  • Sodium Chloride / chemistry
  • Solvents / chemistry
  • Water / chemistry

Substances

  • Polyvinyls
  • Solvents
  • Water
  • polyvinylidene fluoride
  • Sodium Chloride