European Food Research and Technology

, Volume 244, Issue 5, pp 949–957 | Cite as

Development and validation of a novel method for aroma dilution analysis by means of stir bar sorptive extraction

  • Tobias Trapp
  • Deborah A. Jäger
  • Marco A. Fraatz
  • Holger Zorn
Short Communication


Stir bar sorptive extraction (SBSE) coupled with gas chromatography–mass spectrometry–olfactometry (GC–MS–O) allows for isolation and identification of aroma compounds in minimal sample preparation time. By means of this extraction technique in direct sample immersion, an independent approach of aroma dilution analysis (ADA) for the rapid determination of flavor dilution (FD) factors was developed based on dilution of the carrier gas flow. The used gas chromatography system equipped with a thermal desorption unit (TDU) and a cooled injection system (CIS) allowed to independently split the gas flow during thermodesorption and sample injection, respectively. The resulting overall split ratio ratios corresponded to the dilution factors. The developed method based on combining both splitting options allowed to determine FD factors in the range from 4 to 8192 in a reliable and reproducible manner. Validation of the method was performed with an aqueous solution containing 12 authentic standards, and a high linearity was confirmed for the binary logarithmic relationship between the peak area and the overall split ratio.


Stir bar sorptive extraction Olfactometry Aroma dilution analysis Thermodesorption Cryo-focusing Gas chromatography 



Aroma dilution analysis


Aroma extract dilution analysis


Cooled injection system


Direct immersion


Flavor dilution


Gas chromatography




Mass spectrometry




Olfactory detection port


Relative standard deviation


Solvent-assisted flavor evaporation


Stir bar sorptive extraction


Simultaneous distillation–extraction


Selected ion monitoring


Solid-phase microextraction


Split ratio


Thermal desorption unit



This study was financially supported by the excellence initiative of the Hessian Ministry of Science and Art which encompasses generous grants for the LOEWE centre “Insect Biotechnology and Bioresources” and “HessenModellProjekte” (Project No. 478/15-20).

Compliance with ethical standards

Conflict of interest

The authors declare that they have no conflict of interest.

Compliance with ethics requirements

This article does not contain any studies with human or animal subject.

Supplementary material

217_2017_3003_MOESM1_ESM.pdf (198 kb)
Supplementary material 1 (PDF 197 kb)


  1. 1.
    Schieberle P, Grosch W (1987) Evaluation of the flavour of wheat and rye bread crusts by aroma extract dilution analysis. Z Lebensm Unters Forsch 185(2):111–113. CrossRefGoogle Scholar
  2. 2.
    Schieberle P (1995) New developments in methods for analysis of volatile flavor compounds and their precursors. In: Gaonkar AG (ed) Characterization of food: emerging methods. Elsevier, Amsterdam, pp 403–431CrossRefGoogle Scholar
  3. 3.
    Engel W, Bahr W, Schieberle P (1999) Solvent assisted flavour evaporation - a new and versatile technique for the careful and direct isolation of aroma compounds from complex food matrices. Eur Food Res Technol 209(3–4):237–241. CrossRefGoogle Scholar
  4. 4.
    Pico J, Tapia J, Bernal J et al (2017) Comparison of different extraction methodologies for the analysis of volatile compounds in gluten-free flours and corn starch by GC/QTOF. Food Chem. Google Scholar
  5. 5.
    Barba C, Thomas-Danguin T, Guichard E Comparison of stir bar sorptive extraction in the liquid and vapour phases, solvent-assisted flavour evaporation and headspace solid-phase microextraction for the (non)-targeted analysis of volatiles in fruit juice. LWT Food Sci Technol
  6. 6.
    Majcher M, Jeleń HH (2009) Comparison of suitability of SPME, SAFE and SDE methods for isolation of flavor compounds from extruded potato snacks. Int Year Potato 22(6):606–612. Google Scholar
  7. 7.
    Guth H, Grosch W (1993) Identification of potent odourants in static headspace samples of green and black tea powders on the basis of aroma extract dilution analysis (AEDA). Flavour Fragr J 8(4):173–178. CrossRefGoogle Scholar
  8. 8.
    Hinterholzer A, Schieberle P (1998) Identification of the most odour-active volatiles in fresh, hand-extracted juice of Valencia late oranges by odour dilution techniques. Flavour Fragr J 13(1):49–55.<49:AID-FFJ691>3.0.CO;2-S CrossRefGoogle Scholar
  9. 9.
    Fritsch HT, Schieberle P (2005) Identification based on quantitative measurements and aroma recombination of the character impact odorants in a Bavarian Pilsner-type beer. J Agric Food Chem 53(19):7544–7551. CrossRefGoogle Scholar
  10. 10.
    Jelen HH, Majcher M, Dziadas M (2012) Microextraction techniques in the analysis of food flavor compounds: a review. Anal Chim Acta 738:13–26. CrossRefGoogle Scholar
  11. 11.
    Wardencki W, Michulec M, Curylo J (2004) A review of theoretical and practical aspects of solid-phase microextraction in food analysis. Int J Food Sci Tech 39(7):703–717. CrossRefGoogle Scholar
  12. 12.
    David F, Sandra P (2007) Stir bar sorptive extraction for trace analysis. J Chromatogr A 1152(1–2):54–69. CrossRefGoogle Scholar
  13. 13.
    Bicchi C, Iori C, Rubiolo P et al (2002) Headspace Sorptive Extraction (HSSE), Stir Bar Sorptive Extraction (SBSE), and Solid Phase Microextraction (SPME) applied to the analysis of roasted arabica coffee and coffee brew. J Agric Food Chem 50(3):449–459. CrossRefGoogle Scholar
  14. 14.
    Maggi L, Zalacain A, Mazzoleni V et al (2008) Comparison of stir bar sorptive extraction and solid-phase microextraction to determine halophenols and haloanisoles by gas chromatography-ion trap tandem mass spectrometry. Talanta 75(3):753–759. CrossRefGoogle Scholar
  15. 15.
    Contini M, Esti M (2006) Effect of the matrix volatile composition in the headspace solid-phase microextraction analysis of extra virgin olive oil. Food Chem 94:143–150CrossRefGoogle Scholar
  16. 16.
    Ouyang G, Pawliszyn J (2008) A critical review in calibration methods for solid-phase microextraction. Anal Chim Acta 627(2):184–197. CrossRefGoogle Scholar
  17. 17.
    Caven-Quantrill DJ, Buglass AJ (2006) Comparison of micro-scale simultaneous distillation-extraction and stir bar sorptive extraction for the determination of volatile organic constituents of grape juice. J Chromatogr A 1117(2):121–131. CrossRefGoogle Scholar
  18. 18.
    Feng Y, Cai Y, Sun-Waterhouse D et al (2015) Approaches of aroma extraction dilution analysis (AEDA) for headspace solid phase microextraction and gas chromatography–olfactometry (HS-SPME–GC–O): altering sample amount, diluting the sample or adjusting split ratio? Food Chem 187:44–52. CrossRefGoogle Scholar
  19. 19.
    Hwan Kim T (2003) Aroma dilution method using GC injector split ratio for volatile compounds extracted by headspace solid phase microextraction. Food Chem 83(1):151–158. CrossRefGoogle Scholar
  20. 20.
    Zhang Y, Fraatz MA, Horlamus F et al (2014) Identification of potent odorants in a novel nonalcoholic beverage produced by fermentation of wort with shiitake (Lentinula edodes). J Agric Food Chem 62(18):4195–4203. CrossRefGoogle Scholar
  21. 21.
    Trapp T, Zajul M, Ahlborn J et al (2017) Submerged cultivation of Pleurotus sapidus with molasses: aroma dilution analyses by means of solid phase microextraction and stir bar sorptive extraction. J Agric Food Chem. Google Scholar
  22. 22.
    Sasaki T, Koshi E, Take H et al (2017) Characterisation of odorants in roasted stem tea using gas chromatography–mass spectrometry and gas chromatography-olfactometry analysis. Food Chem 220:177–183. CrossRefGoogle Scholar
  23. 23.
    Ibáñez E, López-Sebastián S, Ramos E et al (1998) Analysis of volatile fruit components by headspace solid-phase microextraction. Food Chem 63(2):281–286. CrossRefGoogle Scholar
  24. 24.
    Havemose MS, Justesen P, Bredie W et al (2007) Measurement of volatile oxidation products from milk using solvent-assisted flavour evaporation and solid phase microextraction. Int Dairy J 17:746–752CrossRefGoogle Scholar
  25. 25.
    Lestremau F, Desauziers V, Fanlo JL (2001) Formation of artefacts during air analysis of volatile amines by solid-phase micro extraction. Analyst 126(11):1969–1973. CrossRefGoogle Scholar
  26. 26.
    Adams A, van Lancker F, de Meulenaer B et al (2012) On-fiber furan formation from volatile precursors: a critical example of artefact formation during solid-phase microextraction. J Chromatogr B Anal Technol Biomed Life Sci 897:37–41. CrossRefGoogle Scholar
  27. 27.
    Ochiai N, Sasamoto K, Ieda T et al (2013) Multi-stir bar sorptive extraction for analysis of odor compounds in aqueous samples. J Chromatogr A 1315:70–79. CrossRefGoogle Scholar
  28. 28.
    Ochiai N, Sasamoto K, Kanda H et al (2008) Sequential stir bar sorptive extraction for uniform enrichment of trace amounts of organic pollutants in water samples. J Chromatogr A 1200(1):72–79. CrossRefGoogle Scholar
  29. 29.
    Sgorbini B, Cagliero C, Cordero C et al (2012) New medium-to-high polarity twister coatings for liquid and vapour phase sorptive extraction of matrices of vegetable origin. J Chromatogr A 1265:39–45. CrossRefGoogle Scholar
  30. 30.
    Serrano La, de Hoz K, Salinas MR, Ferrandino A (2016) Different coatings for the HS-SBSE grape volatile analysis in model solution: preliminary results. Food Chem 212:814–820. CrossRefGoogle Scholar

Copyright information

© Springer-Verlag GmbH Germany 2017

Authors and Affiliations

  1. 1.Institute of Food Chemistry and Food BiotechnologyJustus Liebig University GiessenGiessenGermany

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