Dairy Science & Technology

, Volume 92, Issue 4, pp 321–333 | Cite as

Application of HS-SPME–GC-MS-derived variables for monitoring ripening-induced changes in cheese volatile compounds

  • Nebojša P. Milosavljević
  • Polina D. Blagojević
  • Dragiša S. Savić
  • Niko S. RadulovićEmail author
Original Paper


Headspace solid-phase microextraction–gas chromatography-mass spectrometry (HS-SPME–GC-MS) and multivariate statistical analysis (MVA) are widely employed in the analyses/comparison of cheese volatiles. One shortcoming of this approach is that the SPME fiber-coat polarity has a significant effect on the adsorption of volatiles and thus, on the results of MVA. The aim of this study was to test the applicability of different sets of MVA variables, obtained from HS-SPME–GC-MS experiments using the non-polar polydimethylsiloxane (PDMS) and the polar polyacrylate (PA) fibers, in the profiling of cheese volatile compounds and tracking ripening-induced changes. The volatile profiles and ripening-induced changes of two different types of Pasta-Filata “Pirotski kačkavalj” cheese (prepared from raw ewe’s or cow’s milk) were assessed at four different stages of ripening (1, 5, 20, and 30 days). The HS-SPME–GC-MS–MVA results showed that the distribution of volatile compounds into classes gives valuable information concerning cheese type and ripening phase. The extraction with a PA fiber gives a more realistic cheese volatile profile when the relative ratio of the constituent classes is in question, whereas the PDMS fiber is better in recognizing the contribution/concentration of single dominant volatile compounds. For a better and more complete description/profiling of cheese volatiles, we propose the use of combined (transformed) variables that include the information obtained from both PA and PDMS extraction experiments.


Volatile profiles Principal component analysis Agglomerative hierarchical cluster analysis Cheese ripening Pasta-Filata “Pirotski kačkavalj” cheese 



顶空固相微萃取-气质联用(HS-SPME-GC-MS)和多元统计分析(MVA)广泛应用于分析和比较干酪的挥发性化合物。该方法的一个缺点是SPME 纤维外套的极性对挥发性化合物的吸附影响较大,因此也影响了MVA分析的结果。本论文目的是应用不同组合的MVA变量,这些变量是通过HS-SPME-GC-MS实验并采用非极性聚二甲硅氧烷(PDMS)和极性聚丙烯酸酯(PA)纤维萃取跟踪干酪成熟过程中引发的挥发性化合物变化。分析了两种不同类型的Pasta-Filata 和“Pirotski kačkavalj干酪(来自羊奶和牛奶)在四个不同成熟阶段(1,5,20和30 d)所产生挥发性化合物的变化。HS-SPME-GC-MS-MVA实验结果对干酪的类型和成熟阶段挥发性化合物的分布给出了非常重要的信息。利用PA纤维萃取对需要讨论干酪中各种挥发性化合物组分的相对比例给出了更理想的结果。然而PDMS纤维萃取对了解单个主要的挥发性化合物的分布和浓度方面更有优势。为了更好更全面的描述干酪的挥发性化合物,建议将PA和PDMS两种萃取实验的信息结合起来分析干酪成熟过程中挥发性化合物的变化。


挥发性成分 主成分分析 凝聚层次聚类分析 干酪的成熟 帕斯塔费拉塔乳酪 



The research has been supported by the Ministry of Education and Science of Serbia (Project 172061).

Supplementary material

13594_2012_70_MOESM1_ESM.doc (466 kb)
ESM 1 (DOC 466 kb)


  1. Arora G, Cormier F, Lee B (1995) Analysis of odor-active volatiles in cheddar cheese headspace by multidimensional GC/MS/sniffing. J Agric Food Chem 43:748–752CrossRefGoogle Scholar
  2. Barbieri G, Bolzoni L, Careri M, Mangia A, Parolari G, Spagnoli S, Virgili R (1994) Study of the volatile fraction of parmesan cheese. J Agric Food Chem 42:1170–1176CrossRefGoogle Scholar
  3. Delgado FJ, González-Crespo J, Cava R, García-Parra J, Ramírez R (2010) Characterisation by SPME–GC–MS of the volatile profile of a Spanish soft cheese P.D.O. Torta del Casar during ripening. Food Chem 118:182–189CrossRefGoogle Scholar
  4. Fox PF, Wallace JM (1997) Formation of flavour compounds in cheese. Adv Appl Microbiol 45:17–85CrossRefGoogle Scholar
  5. Januszkiewicz J, Sabik H, Azarnia S, Lee B (2008) Optimization of headspace solid-phase microextraction for the analysis of specific flavors in enzyme modified and natural cheddar cheese using factorial design and response surface methodology. J Chromatogr A 1195:16–24CrossRefGoogle Scholar
  6. Johnson AE, Nursten HE, Self R (1969) Aromatic hydrocarbons in foodstuffs and related materials. Chem Ind-London 1:10–12Google Scholar
  7. Knudsten JT, Tollsten L, Bergstrom LG (1994) Floral scents—a checklist of volatile compounds isolated by head-space techniques. Phytochemistry 33:253–280CrossRefGoogle Scholar
  8. Milosavljević N, Joković N, Radulović N, Blagojević P, Savić D (2010) Major volatiles in “Pirotski kačkavalj” cheese made from sheep milk. Preh. ind.– Mleko i ml. proiz. 1–2:122–126Google Scholar
  9. Mondello L, Costa R, Tranchid PQ, Chiofalo B, Zumbo A, Dugo P, Dugo G (2005) Determination of flavor components in Sicilian goat cheese by automated HS-SPME-GC. Flavour Frag J 20:659–665CrossRefGoogle Scholar
  10. Peres C, Viallon C, Berdague J-L (2001) Solid-phase microextraction-mass spectrometry: a new approach to the rapid characterization of cheeses. Anal Chem 73:1030–1036CrossRefGoogle Scholar
  11. Pinho O, Ferreira IM, Ferreira MA (2002) Solid-phase microextraction in combination with GC/MS for quantification of the major volatile free fatty acids in ewe cheese. Anal Chem 74:5199–5204CrossRefGoogle Scholar
  12. Pinho O, Pérès C, Ferreira IM (2003) Solid-phase microextraction of volatile compounds in “Terrincho” ewe cheese. Comparison of different fibers. J Chromatogr A 1011:1–9CrossRefGoogle Scholar
  13. Radulović NS, Blagojević PD (2010) Plant volatiles providing additional evidences to the occurrence of a wild-growing population of Calamintha vardarensis (Greuter et Burdet) Silic outside of its natural habitat. Chem Biodivers 7:2856–2868CrossRefGoogle Scholar
  14. Viallon C, Verdier-Metz I, Denoyer C, Pradel P, Coulon JB, Berdague JL (1999) Desorbed terpenes and sesquiterpenes from forages and cheeses. J Dairy Res 66:319–326CrossRefGoogle Scholar
  15. Ziino M, Condurso C, Romeo V, Giuffrida D, Verzera A (2005) Characterization of “Provola dei Nebrodi”, a typical Sicilian cheese, by volatiles analysis using SPME-GC/MS. Int Dairy J 15:585–593CrossRefGoogle Scholar

Copyright information

© INRA and Springer-Verlag, France 2012

Authors and Affiliations

  • Nebojša P. Milosavljević
    • 1
  • Polina D. Blagojević
    • 2
  • Dragiša S. Savić
    • 3
  • Niko S. Radulović
    • 2
    Email author
  1. 1.College of Agriculture and Food TechnologyProkupljeSerbia
  2. 2.Department of Chemistry, Faculty of Science and MathematicsUniversity of NišNišSerbia
  3. 3.Faculty of TechnologyUniversity of NišLeskovacSerbia

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