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

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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Figure 1: An image of the commercially available TriPlus autosampler for the performance of automated solid phase micro extraction (SPME) processes.
Figure 2: The illustration of the symmetric relationship between absorption and desorption in solid phase micro extraction (SPME).
Figure 3: The detailed experimental procedure outlining the steps required to carry out the in-fiber internal standardization SPME calibration approach.
Figure 4: The effect of sample temperature on extraction efficiency for analytes of different physicochemical properties present in ice wine samples.
Figure 5: Suggested data mining approach for non-targeted profiling of complex food samples using high-speed gas chromatography GC–TOFMS system.
Figure 6: Extraction time profiles for selected method optimization compounds present in ice wine samples.
Figure 7: Total ion current (TIC) chromatogram of Canadian white wine (Vidal grape variety, vintage year 2000) obtained with optimized SPME–GC–TOFMS conditions.

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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

Authors and Affiliations

Authors

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

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. (JPG 1492 kb)

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. (PDF 70 kb)

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Risticevic, S., Chen, Y., Kudlejova, L. et al. Protocol for the development of automated high-throughput SPME–GC methods for the analysis of volatile and semivolatile constituents in wine samples. Nat Protoc 5, 162–176 (2010). https://doi.org/10.1038/nprot.2009.181

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