Desorption Temperature, Solid-Phase Microextraction (SPME), and Natural Product Analyses, how Low Can we Go?


Solid phase microextraction (SPME) has become a common technique for volatile sampling due to its ease of use and limited technical requirements. The solvent-free nature of SPME is also exceptionally attractive for gas chromatography mass spectrometry (GC/MS) analysis. To ensure efficient transfer of the sample to the GC, the manufacturer recommend injector desorption temperatures in the range of 200 to 320 °C. A high desorption temperature can, however, have unwanted effects on analyses of plant and insect produced semiochemicals. By investigating the quantitative and qualitative chromatographic responses at varying inlet temperatures for a component blend of seven plant produced volatile compounds, we found the thermally labile plant-nematode signaling compound, pregeijerene to degrade to geijerene at all tested temperatures within the recommended range (200, 240, and 280 °C), but that it did not break down with an inlet temperature below 200 °C (100 °C and 150 °C). Degradation was also detected for the sesquiterpene germacrene D, but only at the highest inlet temperature tested (280 °C). Surprisingly, an inlet temperature of 200 °C gave the highest sample recovery, measured as total peak area while an inlet temperature of 100 °C as well as 280 °C gave the lowest total area values. An increase in desorption time from 3 to 5 min. Resulted in a recovery at 100 °C close to that obtained at 200 °C. Peak broadening was minimal, and only observed at the 100 °C inlet temperature. Based on these results, we highly recommend that SPME users include desorption temperature as one variable when developing sampling procedures for novel biological systems to ensure that potentially present thermally labile compounds are not degraded.

This is a preview of subscription content, access via your institution.

Fig. 1
Fig. 2


  1. Alborn HT (2018) A technique for thermal desorption analyses suitable for thermally-labile, volatile compounds. J Chem Ecol 44:103–110

    CAS  Article  Google Scholar 

  2. Ali JG, Alborn HT, Stelinski LL (2011) Constitutive and induced subterranean plant volatiles attract both entomopathogenic and plant parasitic nematodes. J Ecol 99:26–35

    CAS  Article  Google Scholar 

  3. Ali JG, Alborn HT, Campos-Herrera R, Kaplan F, Duncan LW, Rodriguez-Saona C, Koppenhöfer AM, Stelinski LL (2012) Subterranean, herbivore-induced plant volatile increases biological control activity of multiple beneficial nematode species in distinct habitats. PLoS One 7:e38146

    CAS  Article  Google Scholar 

  4. Bülow N, König WA (2000) The role of germacrene D as a precursor in sesquiterpene biosynthesis: investigations of acid catalyzed, photochemically and thermally induced rearrangements. Phytochem 55:141–168

    Article  Google Scholar 

  5. Gonzalez ML, Carnicero M, De la Torre R, Ortuño J, Segura J (1995) Influence of the injection technique on the thermal degradation of cocaine and its metabolites in gas chromatography. J Chromatogr B Biomed Sci Appl 664:317–327

    CAS  Article  Google Scholar 

  6. Jalili V, Barkhordari A, Ghiasvand A (2020) A comprehensive look at solid-phase microextraction technique: a review of reviews. Microchem J 152:104319

    CAS  Article  Google Scholar 

  7. Kudlejova L, Risticevic S, Vuckovic D (2012) Solid-phase microextraction method development. In: Pawliszyn J (ed) Handbook of solid phase microextraction. Elsevier, Waterloo, pp 201–249

    Google Scholar 

  8. Kuzovkina IN, Szarka S, Héthelyi É, Lemberkovics E, Szöke É (2009) Composition of essential oil in genetically transformed roots of Ruta graveolens. Russ J Plant Physiol 56:846–851

    CAS  Article  Google Scholar 

  9. Langenfeld JJ, Hawthorne SB, Miller DJ (1996) Optimizing split/splitless injection port parameters for solid-phase microextraction. J Chromatogr A 740:139–145

    CAS  Article  Google Scholar 

  10. Sigma Aldrich (2018) SPME for GC analysis, getting started with solid phase microextraction. Accessed 1 April 2020

  11. Uclés S, Hakme E, Ferrer C, Fernández-Alba AR (2018) Analysis of thermally labile pesticides by on-column injection gas chromatography in fruit and vegetables. Anal Bioanal Chem 410:6861–6871

    Article  Google Scholar 

  12. Yaacob KB, Abdullah CM, Joulain D (1989) Essential oil of Ruta graveolens L. J of Essent Oil Res 1:203–207

    CAS  Article  Google Scholar 

Download references

Author information



Corresponding author

Correspondence to Alexander M. Gaffke.

Rights and permissions

Reprints and Permissions

About this article

Verify currency and authenticity via CrossMark

Cite this article

Gaffke, A.M., Alborn, H.T. Desorption Temperature, Solid-Phase Microextraction (SPME), and Natural Product Analyses, how Low Can we Go?. J Chem Ecol 47, 134–138 (2021).

Download citation


  • Plant volatile
  • SPME
  • Thermally labile
  • GC-MS
  • Injector desorption temperature