Development of a solid phase microextraction protocol for the GC-MS determination of volatile off-flavour compounds from citral degradation in oil-in-water emulsions.

The conditions for headspace solid phase microextraction (HS-SPME) analysis of volatile off-flavour compounds in citral emulsion were determined. Type of SPME phase (65 μm PDMS/DVB, 100 μm PDMS and 75μm CAR/PDMS), adsorption temperature and salt concentration were significant factors affecting total peak area in the gas chromatogram and optimised in one factor experiments. Then, adsorption temperature (30-50°C), adsorption time (20-40 min), and salt concentration (0-6M) were studied to develop HS-SPME condition for obtaining the highest extraction efficiency. PDMS/DVB in 65 μm was the optimum fiber because of high adsorption efficiency and good reproducibility. The optimal condition was adsorption at 50°C for 40 min and 6M salt added to sample. Good Linearity, high recovery, good reproducibility and low limit of detection (LOD) for all off-odour compounds according to the optimised SPME conditions indicated that the SPME procedure was applicable for the analysis of the degraded citral products in headspace volatile of emulsion.