Protocol | Published:

Protocol for the development of automated high-throughput SPME–GC methods for the analysis of volatile and semivolatile constituents in wine samples

Nature Protocols volume 5, pages 162176 (2010) | Download Citation

Abstract

Ever since the invention of gas chromatography (GC), numerous efforts within the chromatographic community have been directed toward the development of fast GC methods. However, the developments in high-speed GC technologies have simultaneously created demand for the availability of compatible detection and sample preparation methods, so that the speed of the overall analytical process is increased. Solid phase micro extraction (SPME) is a sample preparation technique developed to address the need for rapid sample preparation. Therefore, the objective of this protocol is to outline recent developments in SPME technology that can be applied toward high-throughput automated qualitative and quantitative analyses of volatile and semivolatile compounds in wine samples. The use of this protocol facilitates routine high-throughput determinations of 200–500 analytes of different physicochemical properties with SPME step requiring only 10–15 min per sample.

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Acknowledgements

We thank the Natural Sciences and Engineering Research Council of Canada (NSERC) for their financial support. We also thank Stefano Pelagatti (Thermo Fisher Scientific, Milan, Italy) for collaboration and helpful suggestions on the use of TriPlus autosampler. The authors also greatly appreciate the support of LECO for providing us with SPME–GC–TOFMS system.

Author information

Affiliations

  1. Department of Chemistry, University of Waterloo, Waterloo, Ontario, Canada.

    • Sanja Risticevic
    • , Lucie Kudlejova
    • , Rosa Vatinno
    •  & Janusz Pawliszyn
  2. Supelco, Bellefonte, Pennsylvania, USA.

    • Yong Chen
  3. CTC Analytics AG, Zwingen, Switzerland.

    • Bruno Baltensperger
  4. Gerstel Inc., Linthicum, Maryland, USA.

    • John R Stuff
  5. PAS Technology, Magdala, Germany.

    • Dietmar Hein

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Contributions

S.R., Y.C., L.K. and R.V. extensively contributed to the development and evaluation of high-throughput and automated SPME approaches; S.R. combined the data and wrote the protocol; S.R. and L.K. contributed to the development of high-throughput SPME–GC–TOFMS methods for the non-targeted analysis of ice wine samples; Y.C. contributed to development of in-fiber internal standardization and its application toward determination of BTEX in wine samples; B.B. J.R.S. and D.H. contributed to the commercialization of SPME–GC autosamplers and all additional accessories required for automated SPME processes; and J.P. developed the SPME concept and the ideas on improving the throughput of SPME determinations and supervised the projects.

Corresponding author

Correspondence to Janusz Pawliszyn.

Supplementary information

Image files

  1. 1.

    Supplementary Figure 1 | Screen shot of the options/features available in a typical SPME-dedicated software using Gerstel Maestro software as an example.

    The users have options for specifying the conditions for incubation, extraction, agitation, desorption, derivatization/internal standard loading and fibre cleaning parameters.

PDF files

  1. 1.

    Supplementary Table 1

    Functions of most critical SPME specific atoms in macro atom sequence that are used during automated SPME method development with CombiPAL autosampler.

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DOI

https://doi.org/10.1038/nprot.2009.181

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