Comparison of different aroma-active compounds of Sichuan Dark brick tea (Camellia sinensis) and Sichuan Fuzhuan brick tea using gas chromatography–mass spectrometry (GC–MS) and aroma descriptive profile tests

  • Cong-ning Nie
  • Xiao-xue Zhong
  • Li He
  • Yuan Gao
  • Xiang Zhang
  • Cong-ming Wang
  • Xiao DuEmail author
Original Paper


Sichuan dark brick tea (Camellia sinensis) and Sichuan Fuzhuan brick tea have significantly different aroma characteristics although both of them have almost the same processing methods. Thus, these two types of tea were used as the research materials to determine the differences in their aroma compounds. The volatile compounds in the two types of tea were identified and quantified by headspace solid-phase microextraction coupled with gas chromatography–mass spectrometry (HS-SPME–GC–MS), results showed that they both had 37 common volatile compounds. Then the aroma-active components were identified by odour activity value (OAV). It was found that SFBT had 20 aroma-active components, of which β-ionone had the largest OAV (199547.72). SDBT has 21 aroma-active ingredients (including all 20 aroma-active components of SFBT), of which β-ionone again has the largest OAV (114800.66). Finally, the aroma profile differences between the two tea samples were studied by aroma profile tests, and the results showed that the main aroma differences of SDBT and SFBT were caused by β-ionone, epoxydihydrolinalool II, methyl salicylate, geranylacetone, nerolidol, benzaldehyde, benzyl acetate, nonanal, trans,trans-2,4-heptadienal and 1-octen-3-ol, in addition, defined SFBT’s ‘fungi flower aroma’ and SDBT’s ‘aged fragrance’ from the level of aroma monomer.


Dark tea Aroma-active compounds Odour activity value Gas chromatography–mass spectrometry 



Odour activity value


Gas chromatography–mass spectrometry


Sichuan Dark brick tea


Sichuan Fuzhuan brick tea


Headspace solid-phase microextraction


Odour threshold


Principal component analysis



First, I would like to thank my wife Li Hui for her encouragement and assistance during my writing. Second, I would like to thank Professor Xu Jing-yi and Lecturer Zhou Yao for their valuable opinions which were put forward in the manuscript, in addition, I would like to thank Master Zhou Li-he and Master Luo Wei-chen for their selfless help in language.

Author contributions

CN was responsible for the sorting of the experimental data and proofreading and wrote the manuscript. XZ was responsible for the design, implementation of the tests and collection of raw data. LH revised the manuscript critically for important intellectual content. YG, XZ, CW were responsible for some experiments. XD provided design ideas, ensured the smooth progress of the tests and revised the outline and the manuscript.

Compliance with ethical standards

Conflict of interest

There is no conflict of interest in this manuscript, which has been approved by all authors for publication. On behalf of my co-authors, I declare that this study is an unpublished original study and that it is not considered to be published in whole or in part elsewhere. All the authors listed approved the declaration.

Compliance with ethics requirements

The study was approved by the local ethics committee in China.


  1. 1.
    Adams TB, Cohen SM, Doull J, Feron VJ, Goodman JI, Marnett LJ et al (2004) The FEMA GRAS assessment of cinnamyl derivatives used as flavor ingredients. Food Chem Toxicol 42(2):157–185Google Scholar
  2. 2.
    Afsharypuor S, Suleimany M (2002) Volatile oil constituents of Brassica oleracea var. gongylodes seeds. J Essent Oil Res 14(1):18–19Google Scholar
  3. 3.
    And CS, Schieberle P (2006) Characterization of the key aroma compounds in the beverage prepared from darjeeling black tea: quantitative differences between tea leaves and infusion. J Agric Food Chem 54(3):916–924Google Scholar
  4. 4.
    Angioni A, Barra A, Coroneo V, Dessi S, Cabras P (2006) Chemical composition, seasonal variability, and antifungal activity of Lavandula stoechas L. ssp. stoechas essential oils from stem/leaves and flowers. J Agric Food Chem 54(12):4364–4370Google Scholar
  5. 5.
    Ansorena D, Gimeno O, Astiasarán I, Bello J (2001) Analysis of volatile compounds by GC–MS of a dry fermented sausage: chorizo de Pamplona. Food Res Int 34(1):67–75Google Scholar
  6. 6.
    Asuming WA, Beauchamp PS, Descalzo JT, Dev BC, Dev V, Frost S, Ma CW (2005) Essential oil composition of four Lomatium Raf. species and their chemotaxonomy. Biochem Syst Ecol 33(1):17–26Google Scholar
  7. 7.
    Baranauskiene R, Venskutonis PR, Viskelis P, Dambrauskiene E (2003) Influence of nitrogen fertilizers on the yield and composition of thyme (Thymus vulgaris). J Agric Food Chem 51(26):7751–7758Google Scholar
  8. 8.
    Boulanger R, Crouzet J (2000) Free and bound flavour components of Amazonian fruits: 2. cupuacu volatile compounds. Flavour Fragr J 15(4):251–257Google Scholar
  9. 9.
    Cajka T, Hajslova J, Cochran J, Holadova K, Klimankova E (2007) Solid phase microextraction—comprehensive two dimensional gas chromatography—time-of-flight mass spectrometry for the analysis of honey volatiles. J Sep Sci 30(4):534–546Google Scholar
  10. 10.
    Chaturvedula PSV, Prakash I (2011) The aroma, taste, color and bioactive constituents of tea. J Med Plants Res 5(11):2110–2124Google Scholar
  11. 11.
    Chen G, Song H, Ma C (2010) Aroma-active compounds of Beijing roast duck. Flavour Fragr J 24(4):186–191Google Scholar
  12. 12.
    Chen B, Liu XY, Pu HJ, Chen YH, Jiang DH, Gao XL et al (2015) Study on variation of main chemical components during pu’er tea fermentation process of different raw materials. J Food Saf Qual 6(4):1279–1286Google Scholar
  13. 13.
    Cho IH, Namgung H-J, Choi H-K, Kim Y-S (2008) Volatiles and key odorants in the pileus and stipe of pine-mushroom (Tricholoma matsutake Sing.). Food Chem 106(1):71–76Google Scholar
  14. 14.
    Chun WX (2005) Tea biochemistry, 3rd edn. China Agricultural Press, BeiJingGoogle Scholar
  15. 15.
    Cui J, Yang X, Dong A-J, Cheng D-Y, Wang J, Zhao H-T, Xu R-B, Wang P, Li W-J (2011) Chemical composition and antioxidant activity of Euphorbia fischeriana essential oil from China. J Med Plants Res 5(19):4798–4894Google Scholar
  16. 16.
    Fanaro GB, Duarte RC, Santillo AG, Pinto-e-Silva MEM, Purgatto E, Villavicento ALCH (2012) Evaluation of γ-radiation on oolong tea odor volatiles. Radiat Phys Chem 81(8):1152–1156Google Scholar
  17. 17.
    Forero DP, Orrego CE, Peterson DG, Osorio C (2015) Chemical and sensory comparison of fresh and dried lulo (Solanum quitoense Lam.) fruit aroma. Food Chem 169:85–91Google Scholar
  18. 18.
    Gassenmeier K, Schieberle P (1994) Comparison of important odorants in puff-pastries prepared with butter or margarine. LWT Food Sci Technol 27(3):282–288Google Scholar
  19. 19.
    Grosch W (2010) Determination of potent odourants in foods by aroma extract dilution analysis (AEDA) and calculation of odour activity values (OAVs). Flavour Fragr J 9(4):147–158Google Scholar
  20. 20.
    Han W-W, LI Z-S, Zheng Q-C, Sun C-C (2006) Toward a blueprint for β-primeverosidase from tea leaves structure/function properties: Homology modeling study. J Theor Comput Chem 05 (spec01):433–446Google Scholar
  21. 21.
    Hazzit M, Baaliouamer A, Faleiro ML, Miguel MG (2006) Composition of the essential oils of Thymus and Origanum species from Algeria and their antioxidant and antimicrobial activities. J Agric Food Chem 54(17):6314–6321Google Scholar
  22. 22.
    Huang H, Liu ZH, Huang JA, Li S, Li J, Wu Y et al (2010) Isolation and identification of “Jinhua” fungi from the loose tea with “fungus growing”. J Tea Sci 30(5):350–354Google Scholar
  23. 23.
    Ibdah M, Azulay Y, Portnoy V, Wasserman B, Bar E, Meir A et al (2006) Functional characterization of cmccd1, a carotenoid cleavage dioxygenase from melon. Phytochemistry 67(15):1579–1589Google Scholar
  24. 24.
    Isleten MH (2017) Aroma characterization of five microalgae species using solid-phase microextraction and gas chromatography-mass spectrometry/olfactometry. Food Chem 240:1210–1218Google Scholar
  25. 25.
    Jalali-Heravi M, Zekavat B, Sereshti H (2006) Characterization of essential oil components of Iranian geranium oil using gas chromatography-mass spectrometry combined with chemometric resolution techniques. J Chromatogr A 1114(1):154–163Google Scholar
  26. 26.
    Joshi R, Gulati A (2015) Fractionation and identification of minor and aroma-active constituents in kangra orthodox black tea. Food Chem 167:290–298Google Scholar
  27. 27.
    Karagül-Yüceer Y, Vlahovich KN, Drake MA, Cadwallader KR (2003) Characteristic aroma components of rennet casein. J Agric Food Chem 51(23):6797–6801Google Scholar
  28. 28.
    Kartal N, Sokmen M, Tepe B, Daferera D, Polissiou M, Sokmen A (2007) Investigation of the antioxidant properties of Ferula orientalis L. using a suitable extraction procedure. Food Chem 100(2):584–589Google Scholar
  29. 29.
    Kukic J, Petrovic S, Pavlovic M, Couladis M, Tzakou O, Niketic M (2006) Composition of essential oil of Stachys alpina L. ssp dinarica Murb. Flavour Fragr J 21(3):539–542Google Scholar
  30. 30.
    Kundakovic T, Fokialakis N, Kovacevic N, Chinou I (2007) Essential oil composition of Achillea lingulata and A. umbellata. Flavour Fragr J 22(3):184–187Google Scholar
  31. 31.
    Liu D (2017) Effect of Fuzhuan brick-tea addition on the quality and antioxidant activity of skimmed set-type yoghurt. Int J Dairy Technol 71:22–23Google Scholar
  32. 32.
    Liu Y, He C, Song H (2018) Comparison of fresh watermelon juice aroma characteristics of five varieties based on gas chromatography-olfactometry-mass spectrometry. Food Res Int 107:119–129Google Scholar
  33. 33.
    Liu F, Wang Y, Zhang T, Tang X, Wang X, Chunhua LI (2018) Review on aroma change during black tea processing. J Tea Sci 38(1):9–19Google Scholar
  34. 34.
    Lozano PR, Drake M, Benitez D, Cadwallader KR (2007) Instrumental and sensory characterization of heat-induced odorants in aseptically packaged soy milk. J Agric Food Chem 55(8):3018–3026Google Scholar
  35. 35.
    Maia JGS, Andrade EHA, Zoghbi MGB (2000) Volatile constituents of the leaves, fruits and flowers of cashew (Anacardium occidentale L.). J Food Comp Anal 13(3):227–232Google Scholar
  36. 36.
    Maia JGS, Taveira FSN, Andrade EHA, da Silva MHL, Zoghbi MGB (2003) Essential oils of Lippia grandis Schau. Flavour Fragr J. 18(5):417–420Google Scholar
  37. 37.
    Maia JGS, Andrade EHA, da Silva ACM, Oliveira J, Carreira LMM, Araújo JS (2005) Leaf volatile oils from four Brazilian Xylopia species. Flavour Fragr. J 20(5):474–477Google Scholar
  38. 38.
    Mallard WG, Andriamaharavo NR, Mirokhin YA, Halket JM, Stein SE (2014) Creation of libraries of recurring mass spectra from large data sets assisted by a dual-column workflow. Anal Chem 86(20):10231–10238Google Scholar
  39. 39.
    Marongiu B, Porcedda S, Piras A, Sanna G, Murreddu M, Loddo R (2006) Extraction of Juniperus communis L. ssp. nana Willd. essential oil by supercritical carbon dioxide. Flavour Fragr J 21(1):148–154Google Scholar
  40. 40.
    Mesa-Arango AC, Betancur-Galvis L, Montiel J, Bueno JG, Baena A, Duran DC, Martinez JR, Stashenko EE (2010) Antifungal activity and chemical composition of the essential oils of Lippia alba (Miller) N.E. Brown grown in different regions of Colombia. J Essent Oil Res. 22(6):568–574Google Scholar
  41. 41.
    Miettinen SM, Hyvönen LA, Tuorila H (2003) Timing of intensity perception of a polar vs nonpolar aroma compound in the presence of added vegetable fat in milk. J Agric Food Chem 51(18):5437–5443Google Scholar
  42. 42.
    Mo H, Zhang H, Li Y, Zhu Y (2008) Antimicrobial activity of the indigenously microbial fermented Fuzhuan brick-tea. J Biotechnol 136(4):S722Google Scholar
  43. 43.
    Morawicki RO, Beelman RB (2008) Study of the biosynthesis of 1-octen-3-ol using a crude homogenate of Agaricus bisporus in a bioreactor. J Food Sci 73(3):C135–C139Google Scholar
  44. 44.
    Morawicki RO, Beelman RB, Petreson D, Demirci A (2005) Biosynthesis of 1-octen-3-ol and 10-oxo-trans-8-decenoic acid using a crude homogenate of Agaricus bisporus: reaction scale up. Process Biochem 40(1):131–137Google Scholar
  45. 45.
    Noudogbessi J-P, Yedomonhan P, Sohounhloue DCK, Chalchat J-C, Figueredo G (2008) Chemical composition of essential oil of Syzygium guineense (Willd.) DC .var. guineense (Myrtaceae) from Benin. Rec Nat Prod, 33–38Google Scholar
  46. 46.
    Ogawa K, Moon JH, Guo W, Yagi A, Watanabe N, Sakata K (1995) A study on tea aroma formation mechanism: alcoholic aroma precursor amounts and glycosidase activity in parts of the tea plant. Z Naturforsch C 50(7–8):493–498Google Scholar
  47. 47.
    Ortega-Heras M, Gonzalez-Sanjose ML, Beltran S (2002) Aroma composition of wine studied by different extraction methods. Anal Chim Acta 458(1):85–93Google Scholar
  48. 48.
    Palmeira SF Jr, Moura FS, Alves VL, de Oliveira FM, Bento ES, Conserva LM, Andrade EHA (2004) Neutral components from hexane extracts of Croton sellowii. Flavour Fragr J 19(1):69–71Google Scholar
  49. 49.
    Pavlovic M, Kovacevic N, Tzakou O, Couladis M (2006) Essential oil composition of Anthemis triumfetti (L.) DC. Flavour Fragr J. 21(2):297–299Google Scholar
  50. 50.
    Pino JA, Mesa J, Muñoz Y, Martí MP, Marbot R (2005) Volatile components from mango (Mangifera indica L.) cultivars. J Agric Food Chem 53(6):2213–2223Google Scholar
  51. 51.
    Radulescu V, Chiliment S, Oprea E (2004) Capillary gas chromatography-mass spectrometry of volatile and semi-volatile compounds of Salvia officinalis. J Chromatogr A 1027(1–2):121–126Google Scholar
  52. 52.
    Roussis V, Tsoukatou M, Petrakis PV, Chinou I, Skoula M, Harborne JB (2000) Volatile constituents of four Helichrysum species growing in Greece. Biochem Syst Ecol 28(2):163–175Google Scholar
  53. 53.
    Saroglou V, Arfan M, Shabir A, Hadjipavlou-Litina D, Skaltsa H (2007) Composition and antioxidant activity of the essential oil of Teucrium royleanum Wall. ex Benth growing in Pakistan. Flavour Fragr J 22(2):154–157Google Scholar
  54. 54.
    Selli S, Rannou C, Prost C, Robin J, Serot T (2006) Characterization of aroma-active compounds in rainbow trout (Oncorhynchus mykiss) eliciting an off-odor. J Agric Food Chem 54(25):9496–9502Google Scholar
  55. 55.
    Seo WH, Baek HH (2005) Identification of characteristic aroma-active compounds from water dropword (Oenanthe javanica DC.). J Agric Food Chem 53(17):6766–6770Google Scholar
  56. 56.
    Siani AC, Ramos MFS, Menezes-de-Lima O Jr., Ribeiro-dos-Santos R, Fernadez-Ferreira E, Soares ROA, Rosas EC, Susunaga GS, Guimarães AC, Zoghbi MGB, Henriques MGMO (1999) Evaluation of anti-inflammatory-related activity of essential oils from the leaves and resin of species of Protium. J. Ethnopharmacol. 66(1):57–69Google Scholar
  57. 57.
    Skaltsa HD, Mavrommati A, Constantinidis T (2001) A chemotaxonomic investigation of volatile constituents in Stachys subsect Swainsonianeae (Labiatae). Phytochemistry 57(2):235–244Google Scholar
  58. 58.
    Song H, Cadwallader KR (2008) Aroma components of American country ham. J Food Sci 73(1):C29–C35Google Scholar
  59. 59.
    Song H, Xia L (2010) Aroma extract dilution analysis of a beef flavouring prepared from flavour precursors and enzymatically hydrolysed beef. Flavour Fragr J 23(3):185–193Google Scholar
  60. 60.
    Song LB, Huang JA, Liu ZH, Huang H, Wang KB (2009) Study on the activity of dark tea extracts to fxr and lxr model. J Tea Sci 29(2):131–135Google Scholar
  61. 61.
    Stojanovic IZ, Radulovic NS, Mitrovic YLJ, Stamenkovic SM, Stojanovic GS (2011) Volatile constituents of selected Parmeliaceae lichens. J Serb Chem Soc 76(7):987–994Google Scholar
  62. 62.
    Su Y, Wang C, Yinlong G (2009) Analysis of volatile compounds from Mentha hapioealyx Briq by GC–MS based on accurate mass measurements and retention indices. Acta Chem Sinica 67(6):546–554Google Scholar
  63. 63.
    Tuberoso CIG, Kowalczyk A, Coroneo V, Russo MT, Dessì S, Cabras P (2005) Chemical composition and antioxidant, antimicrobial, and antifungal activities of the essential oil of Achillea ligustica all. J Agric Food Chem 53(26):10148–10153Google Scholar
  64. 64.
    van Gemert LJ (2011) Compilations of odour threshold values in air, water and other media and compilations of flavour threshold values in water & other media.
  65. 65.
    Varlet V, Knockaert C, Prost C, Serot T (2006) Comparison of odor-active volatile compounds of fresh and smoked salmon. J Agric Food Chem 54(9):3391–3401Google Scholar
  66. 66.
    Waché Y, Bosser-DeRatuld A, Lhuguenot JC, Belin JM (2003) Effect of cis/trans isomerism of β-carotene on the ratios of volatile compounds produced during oxidative degradation. J Agric Food Chem 51(7):1984–1987Google Scholar
  67. 67.
    Wang D, Ando K, Morita K, Kubota K, Kobayashi A (1994) Optical isomers of linalool and linalool oxides in tea aroma. J Agric Chem Soc Jpn 58(11):2050–2053Google Scholar
  68. 68.
    Xiao-Ming JI (2006) The trade and dissemination of China dark tea. J Tea Sci 49(8):159–165Google Scholar
  69. 69.
    Xu A, Wang Y, Wen J, Liu P, Liu Z, Li Z (2011) Fungal community associated with fermentation and storage of Fuzhuan brick-tea. Int J Food Microbiol 146(1):14–22Google Scholar
  70. 70.
    Xue JB (2016) Microbial community in Chinese rice wine inoculated raw wheat Qu and analysis of enzyme and flavour produced by isolated microbes. Doctoral dissertation, Jiangnan UniversityGoogle Scholar
  71. 71.
    Yan M, Wei BY, Teng JW, Li H, Ning X (2017) Analyses of fungal community by illumina miseq platforms and characterization of Eurotium species on Liupao tea, a distinctive post–fermented tea from China. Food Res Int 99(1):641–649Google Scholar
  72. 72.
    Yang Z, Baldermann S, Watanabe N (2013) Recent studies of the volatile compounds in tea. Food Res Int 53(2):585–599Google Scholar
  73. 73.
    Yao Y, Wu M, Huang Y, Li C, Pan X, Zhu W et al (2017) Appropriately raising fermentation temperature beneficial to the increase of antioxidant activity and gallic acid content in Eurotium cristatum fermented loose tea. LWT Food Sci Technol 82:248–254Google Scholar
  74. 74.
    Zeng Y-X, Zhao C-X, Liang Y-Z, Yang H, Fang H-Z, Yi L-Z, Zeng Z-D (2007) Comparative analysis of volatile components from Clematis species growing in China. Anal Chim Acta 595(1–2):328–339Google Scholar
  75. 75.
    Zeng L, Zhou Y, Fu X, Mei X, Cheng S, Gui J et al (2017) Does oolong tea (Camellia sinensis) made from a combination of leaf and stem smell more aromatic than leaf-only tea? contribution of the stem to oolong tea aroma. Food Chem 237:488–498Google Scholar
  76. 76.
    Zhang L, Zhang ZZ, Zhou YB, Ling TJ, Wan XC (2013) Chinese dark teas: postfermentation, chemistry and biological activities. Food Res Int 53(2):600–607Google Scholar
  77. 77.
    Zhao MM, Cao Y, Cai Y, Guo-Wan SU, Feng YZ (2016) Identification of aroma-active compounds from Yang Jiang Douchi by sde and hs-spme combined with GC–MS/O. Mod Food Sci Technol (5):264–275Google Scholar
  78. 78.
    Zheng CH, Kim TH, Kim KH, Leem YH, Lee HJ (2004) Characterization of potent aroma compounds in Chrysanthemum coronarium L. (Garland) using aroma extract dilution analysis. Flavour Fragr J 19(5):401–405Google Scholar
  79. 79.
    Zhu M, Li E, He H (2008) Determination of volatile chemical constitutes in tea by simultaneous distillation extraction, vacuum hydrodistillation and thermal desorption. Chromatographia 68(7/8):603–610Google Scholar
  80. 80.
    Zhu J, Wang L, Xiao Z, Niu Y (2018) Characterization of the key aroma compounds in mulberry fruits by application of gas chromatography-olfactometry (GC-O), odor activity value (OAV), gas chromatography-mass spectrometry (GC–MS) and flame photometric detection (FPD). Food Chem 245:775–785Google Scholar

Copyright information

© Springer-Verlag GmbH Germany, part of Springer Nature 2019

Authors and Affiliations

  • Cong-ning Nie
    • 1
  • Xiao-xue Zhong
    • 2
  • Li He
    • 1
  • Yuan Gao
    • 1
  • Xiang Zhang
    • 1
  • Cong-ming Wang
    • 1
  • Xiao Du
    • 1
    Email author
  1. 1.Sichuan Agricultural UniversityChengduChina
  2. 2.Yibin Vocational and Technical CollegeYibinChina

Personalised recommendations