Synthesis and characterization of composite polymer, polyethylene glycol grafted flower-like cupric nano oxide for solid phase microextraction of ultra-trace levels of benzene, toluene, ethyl benzene and o-xylene in human hair and water samples

J Chromatogr A. 2015 Oct 30:1418:21-28. doi: 10.1016/j.chroma.2015.09.044. Epub 2015 Sep 21.

Abstract

In this research, poly (ethylene glycol)-poly (ethylene glycol) grafted flower-like cupric oxidenano particles (PEG-PEG-g-CuO NPs) as a novel fiber coating of solid-phase microextraction (SPME) were synthesized by using sol-gel technology. This fiber was successfully applied to extract and determine the ultra-trace levels of benzene, toluene, ethyl benzene and o-xylene in human hair using head space-solid-phase microextraction (HS-SPME) coupled to gas chromatography-flame ionization detector. Characterization and chemical composition of the nano particle was performed by Fourier transform infrared spectroscopy (FT-IR), energy dispersion spectroscopy (EDS) and back scatter analysis (BSA). These methods confirmed the successful fabrication of PEG-g-CuO NPs. The surface morphology of the fibers were inspected by scanning electron microscopy. The scanning electron microscopy (SEM) revealed many "crack-like" features and highly porous structure on the surface of fiber. The synthesized nanocomposites were used for preconcentration and extraction of benzene, toluene, ethyl benzene and o-xylene (BTEX). The effects of operating parameters such as: desorption temperature and time, extraction temperature, extraction time, stirring speed and salt effect were investigated and optimized. Under the optimal conditions, the method detection limits and the limits of quantification were between 0.00025-50.00000pgmL(-1) and 0.00200-200.00000pgmL(-1), respectively. Linearity was observed over a range 0.00200-200000.00000pgmL(-1). The relative standard deviations for one fiber (repeatability; n=5) were obtained from 3.30 up to 5.01% and between fibers or batch to batch (n=3; reproducibility) in the range of 3.63-6.21%. The developed method was successfully applied to simultaneous determination of BTEX in human hairs, tap water and distillate water.

Keywords: BTEX; Flower-like cupric oxide nano particles; Human hairs; Solid-phase microextraction; Sol–gel technology; Water samples.

Publication types

  • Research Support, Non-U.S. Gov't
  • Retracted Publication

MeSH terms

  • Benzene / analysis
  • Benzene Derivatives / analysis*
  • Chromatography, Gas / methods
  • Copper / chemistry*
  • Flame Ionization
  • Fresh Water / chemistry
  • Hair / chemistry*
  • Humans
  • Nanoparticles
  • Polyethylene Glycols / chemical synthesis
  • Polyethylene Glycols / chemistry*
  • Reproducibility of Results
  • Solid Phase Microextraction / methods*
  • Spectroscopy, Fourier Transform Infrared
  • Toluene / analysis
  • Water Pollutants, Chemical / analysis*
  • Xylenes / analysis

Substances

  • Benzene Derivatives
  • Water Pollutants, Chemical
  • Xylenes
  • Toluene
  • Polyethylene Glycols
  • Copper
  • Benzene
  • ethylbenzene
  • cupric oxide
  • 2-xylene