Simultaneous determination of phenol, methylphenols, chlorophenols and bisphenol-A by headspace solid-phase microextraction-gas chromatography-mass spectrometry in water samples and industrial effluents

Abstract

A headspace solid-phase microextraction (HS-SPME) coupled with gas chromatography-mass spectrometry (GC-MS) automatic method for simultaneous determination of trace amounts of phenol, methylphenols (MPs), chlorophenols (CPs) and bisphenol-A (BPA) in water samples and industrial effluents has been developed. Prior to SPME extraction, a direct derivatisation step using acetic anhydride was performed. Four different SPME fibre coatings (75 µm CAR-PDMS, 65 µm PDMS-DVB, 100 µm PDMS and 85 µm PA) were tested. The parameters affecting the HS-SPME process and derivatisation step studied were: extraction time (5–60 min) and temperature (40–100°C), derivatisation time (5–10 min), sample agitation (0–500 rpm), addition of sodium chloride (0–40%). The GC-MS quantification was performed by internal standard calibration and the limits of detection (LODs) were in the low ng L⁻¹. The proposed analytical procedure provided a good linearity (r ² > 0.9931) for standard solutions and a repeatability ranging from 4.8 to 15.2% (n = 5). The obtained results show that the developed method was rapid, simple and efficient for phenol, MPs, CPs and BPA analysis, and provides a good alternative to SPE and LLE. Finally, the proposed method has been applied successfully to analyse water samples, municipal solid waste landfill and industrial effluents.

Keywords:

• headspace solid-phase microextraction
• gas chromatography-mass spectrometry
• phenol
• chlorophenols
• bisphenol-A
• derivatisation

Acknowledgements

We gratefully acknowledge the contribution of all the HBAN team, Cemagref ANTONY, and the financial support of the Tunisian Ministry of Higher Education, Scientific Research and Technology and the R2DS research programme of the Region Ile de France.