Headspace (HS) and headspace solid phase microextraction (HS-SPME) analysis by gas chromatography-mass spectrometry (GC/MS) have been found to be suitable methods for the analysis of volatile organic compounds. The objectives of this paper are to study the possibilities of multiple headspace extraction (MHE) for the quantitative determination of volatile compounds in mushroom samples and to compare the results obtained using three different sample treatment techniques. For this purpose, HS with two different injection techniques (pressure-loop system and gas-tight syringe autosampling system) and HS-SPME have been studied. Three processes were optimized for the analysis of 20 volatile compounds by experimental design technique based on Central Composite Design (CCD) and Full Factorial Design depending on the used methodology. Once the designs were finished, a trade off among optimum conditions for each compound analyzed was reached. At optimum conditions, appropriate extraction time and sample amount for the three techniques used were established. Finally, the methods were validated in terms of linearity, detection and quantitation limits and repeatability. The most suitable method was then applied to the quantitative analysis of seven mushroom samples. A detailed comparison of the analytical performance characteristics of HS and HS-SPME as sample treatment techniques for final GC/MS determination is given. In addition, MHE has been proved to be an adequate technique to avoid matrix effects in complex samples quantitation. Its applicability to the determination of volatile mushroom components, along with its limitations, is discussed in this work.
Keywords: GC/MS; HS-SPME; Headspace analysis; Multiple headspace extraction; Mushroom; Volatile compounds.
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