Journal of Food Science and Technology

, Volume 56, Issue 11, pp 4834–4843 | Cite as

Optimization of Headspace-Solid Phase Microextraction (HS-SPME) technique for the analysis of volatile compounds of margarine

  • Ceyda Dadalı
  • Yeşim ElmacıEmail author
Original Article


The objective of the study was to develop optimum Headspace-Solid Phase Microextraction (HS-SPME) conditions for determining volatile compounds of margarine. The effects of fiber type, extraction temperature, extraction time on extraction rates of 2,3 butandione, dimethyl disulfide, nonanal, butanoic acid, hexanoic acid, octanoic acid, γ-nonalactone, δ-decalactone, total area and number of volatile compounds were investigated. A response surface methodology was applied using three independent variables such as fiber type, extraction temperature and extraction time. The fiber type, extraction temperature and extraction time were arranged with Box–Behnken design. The results shows that extraction temperature and extraction time affect both total area and number of volatile compounds but fiber type effect total area of volatile compounds. The optimum HS-SPME conditions were determined as 47.54 °C extraction temperature and 33.63 min extraction time using DVB/CAR/PDMS fiber type.


SPME Optimization Response surface methodology Margarine Volatile compounds 



This study was supported by Ege University Scientific Research Projects Coordination Unit (Project No: 16/MUH/028). The authors would also like to thank Aromsa, Inc. for supplying the aroma used in this research.


  1. Acree T, Arn H (2016) Flavornet and human odor space. Accessed 15 June 2017
  2. Adahchour M, Vreuls RJJ, van der Heijden A, Brinkman UAT (1999) Trace-level determination of polar flavour compounds in butter by solid-phase extraction and gas chromatography–mass spectrometry. J Chromatogr A 844:295–305. CrossRefPubMedGoogle Scholar
  3. Adahchour M, Wiewel J, Verdel R, Vreuls RJJ, Brinkman UAT (2005) Improved determination of flavour compounds in butter by solid-phase (micro) extraction and comprehensive two-dimensional gas chromatography. J Chromatogr A 1086:99–106. CrossRefPubMedGoogle Scholar
  4. Anonymus (2017) Selection Guide for Supelco SPME Fibers. Accessed 19 June 2017
  5. Arthur L, Killam L, Buchholz K, Pawliszyn J (1992) Automation and optimization of solid-phase microextraction. Anal Chem 64:1960–1966. CrossRefGoogle Scholar
  6. Balasubramanian S, Panigrahi S (2011) Solid-phase microextraction (SPME) techniques for quality characterization of food products: a review. Food Bioprocess Technol 4:1–26. CrossRefGoogle Scholar
  7. Charry-Parra G, DeJesus-Echevarria M, Perez FJ (2011) Beer volatile analysis: optimization of HS/SPME coupled to GC/MS/FID. J Food Sci 76:C205–C211. CrossRefPubMedGoogle Scholar
  8. Chen Y, Shirey RE, Sidisky LM (2010) Determination of diacetyl in butter and air samples by SPME coupled with GC–MS. Chromatographia 72:999–1004. CrossRefGoogle Scholar
  9. Ho CW, Wan Aida WM, Maskat MY, Osman H (2006) Optimization of headspace solid phase microextraction (HS-SPME) for gas chromatography mass spectrometry (GC–MS) analysis of aroma compound in palm sugar (Arenga pinnata). J Food Compost Anal 19:822–830. CrossRefGoogle Scholar
  10. Kataoka H, Lord HL, Pawliszyn J (2000) Applications of solid-phase microextraction in food analysis. J Chromatogr A 880:35–62. CrossRefPubMedGoogle Scholar
  11. Kurtovic I, Marshall SN, Miller MR, Zhao X (2011) Flavour development in dairy cream using fish digestive lipases from Chinook salmon (Oncorhynchus tshawytscha) and New Zealand hoki (Macruronus novaezealandiae). Food Chem 127:1562–1568. CrossRefGoogle Scholar
  12. Laia OM, Ghazalia HM, Cho F, Chong CL (2000) Physical and textural properties of an experimental table margarine prepared from lipase-catalysed transesterified palm stearin: palmkernel olein mixture during storage. Food Chem 71:173–179. CrossRefGoogle Scholar
  13. Lanças F (2003) The role of the separation sciences in the 21th century. J Braz Chem Soc 14:183–197. CrossRefGoogle Scholar
  14. Lecanu L, Ducruet V, Jouquand C, Gratadoux JJ, Feigenbaum A (2002) Optimization of headspace solid-phase microextraction (spme) for the odor analysis of surface-ripened cheese. J Agric Food Chem 50:3810–3817. CrossRefPubMedGoogle Scholar
  15. Liu Y, Meng Z, Zhang F, Shan L, Wang X (2010) Influence of lipid composition, crystallization behavior and microstructure on hardness of palm oil-based margarines. Eur Food Res Technol 230:759–767. CrossRefGoogle Scholar
  16. Lozano PR, Miracle ER, Krause AJ, Drake M, Cadwallader KR (2007) Effect of cold storage and packaging material on the major aroma components of sweet cream butter. J Agric Food Chem 55:7840–7846. CrossRefPubMedGoogle Scholar
  17. Ma QL, Hamid N, Bekhit AED, Robertson J, Law TF (2013) Optimization of headspace solid phase microextraction (HS-SPME) for gas chromatography mass spectrometry (GC–MS) analysis of aroma compounds in cooked beef using response surface methodology. Microchem J 111:16–24. CrossRefGoogle Scholar
  18. Mallia S, Escher F, Schlichtherle-Cerny H (2008) Aroma-active compounds of butter: a review. Eur Food Res Technol 2263:315–325. CrossRefGoogle Scholar
  19. Mondello L, Costa R, Tranchida PQ, Chiofalo B, Zumbo A, Dugo P, Dugo G (2005) Determination of flavor components in Sicilian goat cheese by automated HS-SPME-GC. Flavour Fragr J 20:659–665. CrossRefGoogle Scholar
  20. Pawliszyn JB (1997) Solid-phase microextraction. Theory and practice. Wiley-VCH, New YorkGoogle Scholar
  21. Pawliszyn J (2009) Handbook of solid phase microextraction. Chemical Industry Press of China, OntarioGoogle Scholar
  22. Pellati F, Benvenuti S, Yoshizaki F, Bertelli D, Rossi MC (2005) Headspace solid-phase microextraction-gas chromatography–mass spectrometry analysis of the volatile compounds of Evodia species fruits. J Chromatogr A 1087:265–273. CrossRefPubMedGoogle Scholar
  23. Peña RM, Barciela J, Herrero C, García-Martín S (2008) Headspace Solid-Phase microextraction gas chromatography–mass spectrometry analysis of volatiles in orujo spirits from a defined geographical origin. J Agric Food Chem 56:2788–2794. CrossRefPubMedGoogle Scholar
  24. Peterson DG, Reineccius GA (2003a) Determination of the aroma impact compounds in heated sweet cream butter. Flavour Fragr J 18:320–324. CrossRefGoogle Scholar
  25. Peterson DG, Reineccius GA (2003b) Characterization of the volatile compounds that constitute fresh sweet cream butter aroma. Flavour Fragr J 18:215–220. CrossRefGoogle Scholar
  26. Pinho O, Ferreira I, Santos L (2006) Method optimization by solid-phase micro-extraction in combination with gas chromatography with mass spectrometry for analysis of beer volatile fraction. J Chromatogr A 1121:145–153. CrossRefPubMedGoogle Scholar
  27. Povolo M, Contarini G (2003) Comparison of solid-phase microextraction and purge-and trap methods for the analysis of the volatile fraction of butter. J Chromatogr A 985:117–125. CrossRefPubMedGoogle Scholar
  28. Rega B, Fournier N, Guichard E (2003) Solid Phase Microextraction (SPME) of orange juice flavor: odor representativeness by direct gas chromatography olfactometry (D-GC-O). J Agric Food Chem 51:7092–7099. CrossRefPubMedGoogle Scholar
  29. Roberts DD, Pollien P, Milo C (2000) Solid-phase microextraction method development for headspace analysis of volatile flavor compounds. J Agric Food Chem 48:2430–2437. CrossRefPubMedGoogle Scholar
  30. Rodrigues F, Caldeira M, Camara JS (2008) Development of a dynamic headspace solid-phase microextraction procedure coupled to GC–qMSD for evaluation the chemical profile in alcoholic beverages. Anal Chim Acta 609:82–104. CrossRefPubMedGoogle Scholar
  31. Rodriguez-Bencomo JJ, Muñoz-González C, Martín-Álvarez PJ, Lázaro E, Mancebo R, Castañé X, Pozo-Bayón MA (2012) Optimization of a HS-SPME-GC-MS procedure for beer volatile profiling using response surface methodology: application to follow aroma stability of beers under different storage conditions. Food Anal Methods 5:1386–1397. CrossRefGoogle Scholar
  32. Ruiz J, Cava R, Ventanas J, Jensen MT (1998) Headspace solid phase microextraction for the analysis of volatiles in a meat Product: dry-cured Iberian ham. J Agric Food Chem 46:4688–4694. CrossRefGoogle Scholar
  33. Salum P, Erbay Z, Kelebek H, Selli S (2017) Optimization of Headspace Solid-Phase Microextraction with different fibers for the analysis of volatile compounds of white-brined cheese by using Response Surface Methodology. Food Anal Methods 10:1956–1964. CrossRefGoogle Scholar
  34. Shiota M, Isogai T, Iwasawa A, Kotera M (2011) Model studies on volatile release from different semisolid fat blends correlated with changes in sensory perception. J Agric Food Chem 59:4904–4912. CrossRefPubMedGoogle Scholar
  35. Wagner R, Franco MRB (2012) Effect of the variables time and temperature on volatile compounds extraction of salami by solid phase microextraction. Food Anal Methods 5:1186–1195. CrossRefGoogle Scholar
  36. Zellner BD, Dugo P, Dugo G, Mondello L (2008) Gas chromatography–olfactometry in food flavour analysis. J Chromatogr A 1186:123–143. CrossRefGoogle Scholar
  37. Zhu JY, Chai XS (2005) Some recent developments in headspace gas chromatography. Curr Anal Chem 1:79–83. CrossRefGoogle Scholar

Copyright information

© Association of Food Scientists & Technologists (India) 2019

Authors and Affiliations

  1. 1.Department of Food Engineering, Engineering FacultyEge UniversityIzmirTurkey

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