HS-SPME-GC/MS-Based Volatile Profiling and Chemometric Discrimination of Selected Herbal Teas

Öz

Herbal teas prepared from aromatic plants possess complex volatile profiles associated with their characteristic sensory properties. In this study, the headspace volatile profiles of aqueous infusions prepared from Teucrium polium, Mentha pulegium, Rosmarinus officinalis, Lavandula stoechas, and Ocimum basilicum were investigated using headspace solid-phase microextraction coupled with gas chromatography–mass spectrometry (HS-SPME-GC/MS). Three independent infusions were prepared for each species, resulting in 15 individual volatile profiles, which were evaluated by principal component analysis (PCA) and hierarchical cluster analysis (HCA). A total of 115 volatile compounds were tentatively identified across the five species. Monoterpenoids were the predominant chemical group in M. pulegium (70.17 ± 0.20%), R. officinalis (81.80 ± 0.04%), L. stoechas (96.95 ± 0.08%), and O. basilicum (77.60 ± 0.35%), whereas T. polium showed a more heterogeneous profile comprising substantial proportions of monoterpenoids (49.95 ± 0.16%) and sesquiterpene hydrocarbons (31.32 ± 0.24%). The principal volatile constituents were carvacrol and germacrene D in T. polium; pulegone, piperitone oxide, limonene, and 1,8-cineole in M. pulegium; 1,8-cineole, borneol, and camphor in R. officinalis; fenchone and camphor in L. stoechas; and linalool, eugenol, and methyl chavicol in O. basilicum. The first two principal components accounted for 66.44% of the total variance. The three independently prepared infusions of each species formed compact groups in the PCA score plot, with T. polium showing the most distinct separation. PCA associated M. pulegium particularly with pulegone-, piperitone oxide-, and piperitenone oxide-related variation, whereas HCA grouped the three preparations of each species together and indicated the closest species-level similarity between R. officinalis and L. stoechas. Overall, HS-SPME-GC/MS combined with PCA and HCA provided a useful exploratory approach for the comparative characterization and species-related differentiation of herbal tea headspace volatile profiles under standardized infusion conditions.

Anahtar Kelimeler

• Herbal tea
• Volatile compounds
• HS-SPME-GC/MS
• Chemometric analysis
• Lamiaceae

Etik Beyan

Ethics committee approval was not required for this study because of there was no study on animals or humans.

Kaynakça

1. Adams, R. P. (2017). Identification of essential oil components by gas chromatography/mass spectrometry, ed. 4.1. Allured Publishing.
2. Bahramikia, S., Gavyar, P. H. H., & Yazdanparast, R. (2022). Teucrium polium L: An updated review of phytochemicals and biological activities. Avicenna Journal of Phytomedicine, 12(3), 224. https://doi.org/10.22038/AJP.2021.19155
3. Bakkali, F., Averbeck, S., Averbeck, D., & Idaomar, M. (2008). Biological effects of essential oils – A review. Food and Chemical Toxicology, 46(2), 446–475. https://doi.org/10.1016/J.FCT.2007.09.106
4. Benabdelkader, T., Zitouni, A., Guitton, Y., Jullien, F., Maitre, D., Casabianca, H., Legendre, L., & Kameli, A. (2011). Essential oils from wild populations of algerian lavandula stoechas L.: Composition, chemical variability, and in vitro biological properties. Chemistry and Biodiversity, 8(5), 937–953. https://doi.org/10.1002/CBDV.201000301.
5. Bozin, B., Mimica-Dukic, N., Samojlik, I., & Jovin, E. (2007). Antimicrobial and Antioxidant Properties of Rosemary and Sage (Rosmarinus officinalis L. and Salvia officinalis L., Lamiaceae) Essential Oils. Journal of Agricultural and Food Chemistry, 55(19), 7879–7885. https://doi.org/10.1021/JF0715323
6. Brindisi, L. J., O’Brien, R., Hayes, B. K., Kotwal, S., Wu, Q., Simon, J. E., & Tepper, B. J. (2025). Relationship between sensory perceptions and volatile and phenolic compounds of fresh basil (Ocimum basilicum L.) evaluated by multivariate statistics. Journal of Food Science, 90(4), e70194. https://doi.org/10.1111/1750-3841.70194.
7. Candela, R. G., Rosselli, S., Bruno, M., & Fontana, G. (2021). A Review of the Phytochemistry, Traditional Uses and Biological Activities of the Essential Oils of Genus Teucrium. Planta Medica, 87(6), 432–479. https://doi.org/10.1055/A-1293-5768
8. Chabane, S., Boudjelal, A., Napoli, E., Benkhaled, A., & Ruberto, G. (2021). Phytochemical composition, antioxidant and wound healing activities of Teucrium polium subsp. capitatum (L.) Briq. essential oil. Journal of Essential Oil Research, 33(2), 143–151. https://doi.org/10.1080/10412905.2020.1842260

9. Chen, L. X., Lai, Y. F., Zhang, W. X., Cai, J., Hu, H., Wang, Y., Zhao, J., & Li, S. P. (2020). Comparison of volatile compounds in different parts of fresh Amomum villosum Lour. From different geographical areas using cryogenic grinding combined HS-SPME-GC-MS. Chinese Medicine (United Kingdom), 15(1), 97. https://doi.org/10.1186/S13020-020-00377-Z.
10. Dharsono, H. D. A., Putri, S. A., Kurnia, D., Dudi, D., & Satari, M. H. (2022). Ocimum Species: A Review on Chemical Constituents and Antibacterial Activity. Molecules, 27(19), 6350. https://doi.org/10.3390/MOLECULES27196350.
11. Djebili, S., Taş, M., Bouguerra, A., Kucukaydin, S., Ceylan, O., Duru, M. E., & Barkat, M. (2022). Volatile compound profile and essential oil composition of three wild Algerian aromatic plants with their antioxidant and antibiofilm activities. Journal of Food Measurement and Characterization, 16(2), 987–999. https://doi.org/10.1007/S11694-021-01220-1.
12. Duru, M. E., Taş, M., Çayan, F., Küçükaydın, S., & Tel-Çayan, G. (2021). Characterization of volatile compounds of Turkish pine honeys from different regions and classification with chemometric studies. European Food Research and Technology, 247(10), 2533–2544. https://doi.org/10.1007/S00217-021-03817-8
13. El Omari, N., Aguerd, O., Balahbib, A., El Menyiy, N., Amanullah, M., Chew, J., Ming, L. C., & Bouyahya, A. (2025). Expediting multiple biological properties of main bioactive compounds of Mentha pulegium L. AMB Express 15(1), 105. https://doi.org/10.1186/S13568-025-01911-8
14. Figueiredo, A. C., Barroso, J. G., Pedro, L. G., & Scheffer, J. J. C. (2008). Factors affecting secondary metabolite production in plants: Volatile components and essential oils. Flavour and Fragrance Journal, 23(4), 213–226. https://doi.org/10.1002/FFJ.1875.
15. Göksu Sürücü, C., Tolun, A., Halisçelik, O., & Artık, N. (2024). Brewing method-dependent changes of volatile aroma constituents of green tea (Camellia sinensis L.). Food Science and Nutrition, 12(10), 7186–7201. https://doi.org/10.1002/FSN3.4307.
16. Başer, K. H. C., & Kırımer, N. (2018). Essential oils of Anatolian Lamiaceae-An update. Natural Volatiles & Essential Oils, 5(4), 1–28.
17. Juergens, U. R., Dethlefsen, U., Steinkamp, G., Gillissen, A., Repges, R., & Vetter, H. (2003). Anti-inflammatory activity of 1.8-cineol (eucalyptol) in bronchial asthma: a double-blind placebo-controlled trial. Respiratory Medicine, 97(3), 250–256. https://doi.org/10.1053/RMED.2003.1432
18. Kataoka, H., Lord, H. L., & Pawliszyn, J. (2000). Applications of solid-phase microextraction in food analysis. Journal of Chromatography A, 880(1–2), 35–62. https://doi.org/10.1016/S0021-9673(00)00309-5
19. Lin, J., Zhang, P., Pan, Z., Xu, H., Luo, Y., & Wang, X. (2013). Discrimination of oolong tea (Camellia sinensis) varieties based on feature extraction and selection from aromatic profiles analysed by HS-SPME/GC–MS. Food Chemistry, 141(1), 259–265. https://doi.org/10.1016/J.FOODCHEM.2013.02.128
20. Maggio, A., Roscigno, G., Bruno, M., De Falco, E., & Senatore, F. (2016). Essential-Oil Variability in a Collection of Ocimum basilicum L. (Basil) Cultivars. Chemistry & Biodiversity, 13(10), 1357–1368. https://doi.org/10.1002/CBDV.201600069
21. Mahboubi, M., & Haghi, G. (2008). Antimicrobial activity and chemical composition of Mentha pulegium L. essential oil. Journal of Ethnopharmacology, 119(2), 325–327. https://doi.org/10.1016/J.JEP.2008.07.023
22. McKay, D. L., & Blumberg, J. B. (2006). A review of the bioactivity and potential health benefits of peppermint tea (Mentha piperita L.). Phytotherapy Research, 20(8), 619–633. https://doi.org/10.1002/PTR.1936.
23. Patel, M., Lee, R., Merchant, E. V., Juliani, H. R., Simon, J. E., & Tepper, B. J. (2021). Descriptive aroma profiles of fresh sweet basil cultivars (Ocimum spp.): Relationship to volatile chemical composition. Journal of Food Science, 86(7), 3228–3239. https://doi.org/10.1111/1750-3841.15797.
24. Poswal, F. S., Russell, G., Mackonochie, M., MacLennan, E., Adukwu, E. C., & Rolfe, V. (2019). Herbal Teas and their Health Benefits: A Scoping Review. Plant Foods for Human Nutrition, 74(3), 266–276. https://doi.org/10.1007/S11130-019-00750-W
25. Rafya, M., Zehhar, N., Hafidi, A., & Benkhalti, F. (2024). Review of Rosmarinus officinalis L. essential oil, hydrosol, and residues analysis: Composition, bioactivities, and valorization. Industrial Crops and Products, 221, 119392. https://doi.org/10.1016/J.INDCROP.2024.119392
26. Sánchez-López, J. A., Yener, S., Smrke, S., Märk, T. D., Bonn, G., Zimmermann, R., Biasioli, F., & Yeretzian, C. (2020). Extraction kinetics of tea aroma compounds as a function brewing temperature, leaf size and water hardness. Flavour and Fragrance Journal, 35(4), 365–375. https://doi.org/10.1002/FFJ.3571
27. Sevindik, M., Kilibarda, S., Uysal, I., Šavikin, K., Banjac, N., & Popović-Đorđević, J. (2025). Overview of phytochemical composition and bioactivity of Lavandula species. Phytochemistry Reviews 2025, 1–26. https://doi.org/10.1007/S11101-025-10180-Z
28. Telci, I., Bayram, E., Yilmaz, G., & Avci, B. (2006). Variability in essential oil composition of Turkish basils (Ocimum basilicum L.). Biochemical Systematics and Ecology, 34(6), 489–497. https://doi.org/10.1016/J.BSE.2006.01.009
29. Tschiggerl, C., & Bucar, F. (2010). Investigation of the Volatile Fraction of Rosemary Infusion Extracts. Scientia Pharmaceutica, 78(3), 483. https://doi.org/10.3797/SCIPHARM.1004-23
30. Ultee, A., Kets, E. P. W., & Smid, E. J. (1999). Mechanisms of action of carvacrol on the food-borne pathogen Bacillus cereus. Applied and Environmental Microbiology, 65(10), 4606–4610. https://doi.org/10.1128/AEM.65.10.4606-4610.1999
31. Uritu, C. M., Mihai, C. T., Stanciu, G. D., Dodi, G., Alexa-Stratulat, T., Luca, A., Leon-Constantin, M. M., Stefanescu, R., Bild, V., Melnic, S., & Tamba, B. I. (2018). Medicinal plants of the family Lamiaceae in pain therapy: A review. Pain Research and Management, 2018. https://doi.org/10.1155/2018/7801543
32. Wirtu, S. F., Mishra, A. K., Jule, L. T., & Ramaswamy, K. (2024). Ocimum basilicum and Ocimum americanum: A Systematic Literature Review on Chemical Compositions and Antimicrobial Properties. Natural Product Communications, 19(4). https://doi.org/10.1177/1934578X241247640
33. Wright, J., Wulfert, F., Hort, J., & Taylor, A. J. (2007). Effect of Preparation Conditions on Release of Selected Volatiles in Tea Headspace. Journal of Agricultural and Food Chemistry, 55(4), 1445–1453. https://doi.org/10.1021/JF062657V
34. Yang, Z., Baldermann, S., & Watanabe, N. (2013). Recent studies of the volatile compounds in tea. Food Research International, 53(2), 585–599. https://doi.org/10.1016/J.FOODRES.2013.02.011
35. Zárybnický, T., Matoušková, P., Lancošová, B., Šubrt, Z., Skálová, L., & Boušová, I. (2018). Inter-Individual Variability in Acute Toxicity of R-Pulegone and R-Menthofuran in Human Liver Slices and Their Influence on miRNA Expression Changes in Comparison to Acetaminophen. International Journal of Molecular Sciences, 19(6). https://doi.org/10.3390/IJMS19061805
36. Zeng, Q., Wang, H., Tuo, J., Ding, Y., Cao, H., & Yue, C. (2025). Volatile Organic Compounds in Teas: Identification, Extraction, Analysis, and Application of Tea Aroma. Foods, 14(15), 2574. https://doi.org/10.3390/FOODS14152574.
37. Zhu, Y., Lv, H. P., Shao, C. Y., Kang, S., Zhang, Y., Guo, L., Dai, W. D., Tan, J. F., Peng, Q. H., & Lin, Z. (2018). Identification of key odorants responsible for chestnut-like aroma quality of green teas. Food Research International, 108, 74–82. https://doi.org/10.1016/J.FOODRES.2018.03.026