Simple and solvent-free methodology for simultaneous quantification of methanol and acetic acid content of plant polysaccharides based on headspace solid phase microextraction-gas chromatography (HS-SPME-GC-FID)

A simple and solvent-free methodology is proposed for the simultaneous determination of methanol and acetic acid content of any type of plant cell wall polysaccharides. The methanol and acetic acid, released by saponification, are extracted from the headspace of the aqueous solution by solid phase microextraction (HS-SPME) using a DVB/Carboxen/PDMS fibre. The analytes are separated by gas chromatography and detected using a flame ionization detector (GC-FID). The quantification of methanol and acetic acid is done using external calibration curves. A linear relationship between the concentration of methanol (40–100 mg L−1) and acetic acid (25–105 mg L−1) and their GC peak area was observed (r2=0.987 and 0.988, respectively) with a reproducibility of 10%. HS-SPME-GC-FID revealed to be a clean, simple, fast and reliable methodology for the determination of the methanol and acetic acid content of cell wall polysaccharide extracts.