Modeling and optimizing microwave-assisted extraction of antioxidants from Thymbra Spicata L. and characterization of their phenolic constituents

  • Mustafa BenerEmail author


Response surface methodology was used for modeling and optimizing microwave-assisted extraction of antioxidants from Thymbra spicata L. as a factor of temperature, extraction time, solvent concentration, and solvent-to-solid ratio. The prepared extracts showed maximum antioxidant properties, including total phenolic content (TPC), total antioxidant capacity (TAC), and radical scavenging activity (RSA) at the optimum operating conditions. All models calculated for the three responses that are TPC, TAC, and RSA were noteworthy (p < 0.0001) and showed a significant relationship between the response and independent parameters. There was a close relationship between the experimental and the predicted values obtained using the proposed method. The phenolic antioxidant profile of Thymbra spicata L. extract was characterized with the UPLC-PDA-ESI–MS/MS system and rosmarinic acid was found as a major component (1089.2 ± 10.9 mg/100 g-DS). In the future, this optimized and modeled MAE method can be applied in food and pharmaceutical industries to effectively extract antioxidants from edible Thymbra spicata L. plant.


Thymbra spicata L. Antioxidant Microwave-assisted extraction Response surface methodology UPLC-PDA-ESI–MS/MS 



I thank Istanbul University-Cerrahpasa Application and Research Center for the Measurement of Food Antioxidants for sharing its research infrastructures.

Compliance with ethical standards

Conflict of interest

The author states that there is no conflict of interest.

Supplementary material

10068_2019_687_MOESM1_ESM.docx (109 kb)
Supplementary material 1 (DOCX 109 kb)


  1. Ak T, Gülçin, İ. Antioxidant and radical scavenging properties of curcumin. Chem. Biol. Interact. 174: 27-37 (2008)CrossRefGoogle Scholar
  2. Akkol EK, Avcı G, Küçükkurt I, Keleş H, Tamer U, Ince S, Yesilada E. Cholesterol-reducer, antioxidant and liver-protective effects of Thymbra spicata L. var. spicata. J. Ethnopharmacol. 126: 314-319 (2009)CrossRefGoogle Scholar
  3. Apak R, Güçlü K, Özyürek M, Karademir SE. Novel total antioxidant capacity index for dietary polyphenols and vitamins C and E, using their cupric ion reducing capability in the presence of neocuproine: CUPRAC method. J. Agric. Food Chem. 52: 7970-7981 (2004)CrossRefGoogle Scholar
  4. Askun T, Tumen G, Satil F, Ates M. Characterization of the phenolic composition and antimicrobial activities of Turkish medicinal plants. Pharm. Biol. 47: 563-571 (2009)CrossRefGoogle Scholar
  5. Barani H, Maleki H. Plasma and ultrasonic process in the dyeing of wool fibres with madder in presence of Lecithin. J. Disper. Sci. Technol. 32: 1191-1199 (2011)CrossRefGoogle Scholar
  6. Bener M, Özyürek M, Güçlü K, Apak R. Optimization of microwave-assisted extraction of curcumin from Curcuma longa L. (Turmeric) and evaluation of antioxidant activity in multi-test systems. Rec. Nat. Prod. 10: 542-554 (2016)Google Scholar
  7. Bener M, Shen Y, Apak R, Finley JW, Xu Z. Release and degradation of anthocyanins and phenolics from blueberry pomace during thermal acid hydrolysis and dry heating. J. Agric. Food Chem. 61: 6643-6649 (2013)CrossRefGoogle Scholar
  8. Bozkurt H. Utilization of natural antioxidants: Green tea extract and Thymbra spicata oil in Turkish dry-fermented sausage. Meat Sci. 73: 442-450 (2006)CrossRefGoogle Scholar
  9. Cacace JE, Mazza G. Mass transfer process during extraction of phenolic compounds from milled berries. J. Food Eng. 59: 379-389 (2003)CrossRefGoogle Scholar
  10. Camel V. Microwave-assisted solvent extraction of environmental samples. TrAC-Trends Anal. Chem. 19: 229-248 (2000)CrossRefGoogle Scholar
  11. Chen Y, Xie MY, Gong XF. Microwave-assisted extraction used for the isolation of total triterpenoid saponins from Ganoderma atrum. J. Food Eng. 81: 162-170 (2007)CrossRefGoogle Scholar
  12. Croft KD. The chemistry and biological effects of flavonoids and phenolic acids. Ann. NY Acad. Sci. 854: 435-442 (1998)CrossRefGoogle Scholar
  13. Çelik SE, Tufan AN, Bekdeşer B, Özyürek M, Güçlü K, Apak R. Identification and determination of phenolics in Lamiaceae species by UPLC-DAD-ESI-MS/MS. J. Chromatogr. Sci. 55: 291-300 (2017)CrossRefGoogle Scholar
  14. Do QD, Angkawijaya AE, Tran-Nguyen PL, Huynh LH, Soetaredjo FE, Ismadji S, Ju YH. Effect of extraction solvent on total phenol content, total flavonoid content, and antioxidant activity of Limnophila aromatica. J. Food Drug Anal. 22: 296-302 (2014)CrossRefGoogle Scholar
  15. Dorman HD, Bachmayer O, Kosar M, Hiltunen R. Antioxidant properties of aqueous extracts from selected Lamiaceae species grown in Turkey. J. Agric. Food Chem. 52: 762-770 (2004)CrossRefGoogle Scholar
  16. Fan G, Han Y, Gu Z, Chen D. Optimizing conditions for anthocyanins extraction from purple sweet potato using response surface methodology (RSM). LWT-Food Sci. Technol. 41: 155-160 (2008)CrossRefGoogle Scholar
  17. Fleisher Z, Fleisher A. Extract analyses of Satureja thymbra L. and Thymbra spicata L. aromatic plants of the holy land and the Sinai Part XVII. J. Essent. Oil Res. 17: 32-35 (2005)CrossRefGoogle Scholar
  18. Gan C-Y, Latiff AA. Optimisation of the solvent extraction of bioactive compounds from Parkia speciosa pod using response surface methodology. Food Chem. 124: 1277-1283 (2011)CrossRefGoogle Scholar
  19. Gumus T, Albayrak S, Sagdic O, Arici M. Effect of gamma irradiation on total phenolic contents and antioxidant activities of Satureja hortensis, Thymus vulgaris, and Thymbra spicata from Turkey. Int. J. Food Prop. 14: 830-839 (2011)CrossRefGoogle Scholar
  20. Hancı S, Sahin S, Yılmaz L. Isolation of volatile oil from thyme (Thymbra spicata) by steam distillation. Nahrung 47: 252-255 (2003)CrossRefGoogle Scholar
  21. Hemwimon S, Pavasant P, Shotipruk A Microwave-assisted extraction of antioxidative anthraquinones from roots of Morinda citrifolia. Sep. Purif. Technol. 54: 44-50 (2007)CrossRefGoogle Scholar
  22. İlbay Z, Şahin S, Kırbaşlar Şİ. Optimisation of ultrasound-assisted extraction of rosehip (Rosa canina L.) with response surface methodology. J. Sci. Food Agric. 93: 2804-2809 (2013)CrossRefGoogle Scholar
  23. Kan Y, Chen T, Wu Y, Wu J. Antioxidant activity of polysaccharide extracted from Ganoderma lucidum using response surface methodology. Int. J. Biol. Macromol. 72: 151-157 (2015)CrossRefGoogle Scholar
  24. Lee W, Yusof S, Hamid N, Baharin B. Optimizing conditions for hot water extraction of banana juice using response surface methodology (RSM). J. Food Eng. 75: 473-479 (2006)CrossRefGoogle Scholar
  25. Naczk M, Shahidi F. Phenolics in cereals, fruits and vegetables: Occurrence, extraction and analysis. J. Pharmaceut. Biomed. 41: 1523-1542 (2006)CrossRefGoogle Scholar
  26. Ozel MZ, Gogus F, Lewis AC. Subcritical water extraction of essential oils from Thymbra spicata. Food Chem. 82: 381-386 (2003)CrossRefGoogle Scholar
  27. Özyürek M, Bener M, Güçlü K, Apak R. Antioxidant/antiradical properties of microwave-assisted extracts of three wild edible mushrooms. Food Chem. 157: 323-331 (2014)CrossRefGoogle Scholar
  28. Pinelo M, Rubilar M, Jerez M, Sineiro J, Núñez MJ. Effect of solvent, temperature, and solvent-to-solid ratio on the total phenolic content and antiradical activity of extracts from different components of grape pomace. J. Agric. Food Chem. 53: 2111-2117 (2005)CrossRefGoogle Scholar
  29. Rafiee Z, Jafari SM, Alami M, Khomeiri M. Microwave-assisted extraction of phenolic compounds from olive leaves; a comparison with maceration. J. Anim. Plant Sci. 21: 738-745 (2011)Google Scholar
  30. Raman G, Gaikar VG. Microwave-assisted extraction of piperine from Piper nigrum. Ind. Eng. Chem. Res. 41: 2521-2528 (2002)CrossRefGoogle Scholar
  31. Sánchez-Moreno C, Larrauri JA, Saura-Calixto F. A procedure to measure the antiradical efficiency of polyphenols. J. Sci. Food Agric. 76: 270-276 (1998)CrossRefGoogle Scholar
  32. Shan B, Cai YZ, Sun M, Corke H. Antioxidant capacity of 26 spice extracts and characterization of their phenolic constituents. J. Agric. Food Chem. 53: 7749-7759 (2005)CrossRefGoogle Scholar
  33. Simić VM, Rajković KM, Stojičević SS, Veličković DT, Nikolić NČ, Lazić ML, Karabegović IT. Optimization of microwave-assisted extraction of total polyphenolic compounds from chokeberries by response surface methodology and artificial neural network. Sep. Purific. Technol. 160: 89-97 (2016)CrossRefGoogle Scholar
  34. Singleton VL, Orthofer R, Lamuela-Raventós RM. Analysis of total phenols and other oxidation substrates and antioxidants by means of Folin-ciocalteu reagent. Methods Enzymol. 299: 152-178 (1999)CrossRefGoogle Scholar
  35. Sonsuzer S, Sahin S, Yilmaz L. Optimization of supercritical CO2 extraction of Thymbra spicata oil. J. Supercrit. Fluid. 30: 189-199 (2004)CrossRefGoogle Scholar
  36. Spigno G, Tramelli L, De Faveri DM. Effects of extraction time, temperature and solvent on concentration and antioxidant activity of grape marc phenolics. J. Food Eng. 81: 200-208 (2007)CrossRefGoogle Scholar
  37. Stocker P, Yousfi M, Djerridane O, Perrier J, Amziani R, El Boustani S, Moulin A. Effect of flavonoids from various Mediterranean plants on the enzymatic activity of intestinal carboxylesterase. Biochimie 86: 919-925 (2004)CrossRefGoogle Scholar
  38. Thompson LU. Antioxidants and hormone-mediated health benefits of whole grains. Crit. Rev. Food Sci. 34: 473-497 (1994)CrossRefGoogle Scholar
  39. Ünlü M, Vardar-Ünlü G, Vural N, Dönmez E, Özbaş ZY. Chemical composition, antibacterial and antifungal activity of the essential oil of Thymbra spicata L. from Turkey. Nat. Prod. Res. 23: 572-579 (2009)CrossRefGoogle Scholar
  40. Wang L, Weller CL. Recent advances in extraction of nutraceuticals from plants. Trends Food Sci. Technol. 17: 300-312 (2006)CrossRefGoogle Scholar
  41. Wettasinghe M, Shahidi F. Evening primrose meal: a source of natural antioxidants and scavenger of hydrogen peroxide and oxygen-derived free radicals. J. Agric. Food Chem. 47: 1801-1812 (1999)CrossRefGoogle Scholar
  42. Yilmaz Y, Toledo RT. Oxygen radical absorbance capacities of grape/wine industry byproducts and the effect of solvent type on the extraction of grape seed polyphenols. J. Food Compos. Anal. 19: 41-48 (2006)CrossRefGoogle Scholar
  43. Yuan JF, Zhang ZQ, Fan ZC, Yang JX. Antioxidant effects and cytotoxicity of three purified polysaccharides from Ligusticum chuanxiong Hort, Carbohyd. Polym. 74: 822-827 (2008)CrossRefGoogle Scholar
  44. Zigoneanu I, Williams L, Xu Z, Sabliov C. Determination of antioxidant components in rice bran oil extracted by microwave-assisted method. Bioresour. Technol. 99: 4910-4918 (2008)CrossRefGoogle Scholar
  45. Zuo Y, Zeng A, Yuan X, Yu K. Extraction of soybean isoflavones from soybean meal with aqueous methanol modified supercritical carbon dioxide. J. Food Eng. 89: 384-389 (2008)CrossRefGoogle Scholar

Copyright information

© The Korean Society of Food Science and Technology 2019

Authors and Affiliations

  1. 1.Division of Analytical Chemistry, Department of Chemistry, Faculty of EngineeringIstanbul University-CerrahpasaIstanbulTurkey

Personalised recommendations