Research Article
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Year 2025, Volume: 12 Issue: 3, 155 - 161, 30.09.2025
https://doi.org/10.17350/HJSE19030000362

Abstract

References

  • 1. Buza V, Niculae M, Hanganu D, Pall E, Burtescu RF, Olah NK. et al. Biological activities and chemical profile of Gentiana asclepiadea and Inula helenium ethanolic extracts. Molecules. 2022;27(11):3560. doi:10.3390/molecules27113560
  • 2. Akcın TA, Akcın A. Anatomy and micromorphology of Inula helenium subsp. orgyalis and I. ensifolia (Asteraceae) from Turkey. Not Sci Biol. 2017;9(1):104–109. doi:10.15835/nsb919950
  • 3. Wang J, Zhao YM, Guo CY, Zhang SM, Liu CL, ZhangDS, et al. Ultrasound-assisted extraction of total flavonoids from Inula helenium. Pharmacogn Mag. 2012;8(30):166–170. doi:10.4103/0973-1296.96581
  • 4. Aybastıer Ö. Efficacy of methanol-water extract of Inula helenium root against oxidative DNA damage. J Tradit Chin Med. 2021;41(2). doi:10.19852/j.cnki.jtcm.20210209.008
  • 5. Zlatić N, Jakovljević D, Stanković M. Temporal, plant part, and interpopulation variability of secondary metabolites and antioxidant activity of Inula helenium L. Plants. 2019;8(6):179. doi:10.3390/plants8060179
  • 6. Özcan FŞ, Dikmen H, Özcan N, Çetin Ö, Çelik M, Trendafilova A. Microwave-assisted extraction optimization of sesquiterpene lactones from Inula helenium roots: A sustainable approach to reduce energy consumption and carbon footprint. Food Sci Nutr. 2024;12(1):255–267. doi:10.1002/fsn3.3775
  • 7. Guo CY, Wang J, Hou Y, Zhao YM, Shen LX, Zhang DS. Orthogonal test design for optimizing the extraction of total flavonoids from Inula helenium. Pharmacogn Mag. 2013;9(35):192–195. doi:10.4103/0973-1296.113260
  • 8. Çoklar H, Akbulut M. Alıç (Crataegus orientalis) meyvesinin antioksidan aktivitesi ve fenolik bileşiklerinin ekstraksiyonu üzerine farklı çözgenlerin etkisi. Derim. 2016;33(2):237–248. doi:10.16882/derim.2016.267908
  • 9. Garcia-Salas P, Morales-Soto A, Segura-Carretero A, Fernández-Gutiérrez A. Phenolic-compound-extraction systems for fruit and vegetable samples. Molecules. 2010;15(12):8813–8826. doi:10.3390/molecules15128813
  • 10. Türkyılmaz M, Tağı Ş, Özkan M. Narın farklı bölümlerinin polifenol içeriği, antioksidan ve antibakteriyel aktivitesi üzerine ekstraksiyon çözgenlerinin etkisi. Akademik Gıda. 2017;15(2):109–118. doi:10.24323/akademik-gida.333632
  • 11. Galvan D, Effting L, Cremasco H, Conte-Junior CA. Recent applications of mixture designs in beverages, foods, and pharmaceutical health: A systematic review and meta-analysis. Foods. 2021;10(8):1941. doi:10.3390/foods10081941
  • 12. Sanjaya IPW, Chan MT, Sukma D, Buchori A, Putra RP, Nurcholis W. D-optimal design optimization of solvent mixture for flavonoid extraction from Phalaenopsis leaves with antioxidant activity. J Pharm Bioallied Sci. 2024;16(1):1–7. doi:10.4103/jpbs.jpbs_372_23
  • 13. Vural N, Cavuldak ÖA, Akay MA. D-optimal design and multi-objective optimization for green extraction conditions developed with ultrasonic probe for oleuropein. J Appl Res Med Aromat Plants. 2021;20:100279. doi:10.1016/j.jarmap.2020.100279
  • 14. Frumuzachi O, Nicolescu A, Babotă M, Mocan A, Sisea CR, Hera O, Rocchetti G. D-optimal design-based ultrasound-assisted extraction optimization and extensive bio-structural analysis of phenolic compounds from Romanian cornelian cherry (Cornus mas L.) genotypes. Food Bioprocess Technol. 2025;1–18. doi:10.1007/s11947-025-03914-6
  • 15. Yan H, Haiming S, Cheng G, Xiaobo L. Chemical constituents of the roots of Inula helenium. Chem Nat Compd. 2012;48(3):522–524. doi:10.1007/s10600-012-0298-x
  • 16. Spiridon I, Nechita CB, Niculaua M, Silion M, Armatu A, Teacă CA, Bodîrlău R. Antioxidant and chemical properties of Inula helenium root extracts. Cent Eur J Chem. 2013;11(10):1699–1709. doi:10.2478/s11532-013-0295-3
  • 17. Özcan FŞ, Özcan N, Dikmen Meral H, Çetin Ö, Çelik M, Trendafilova A. Extraction of sesquiterpene lactones from Inula helenium roots by high-pressure homogenization and effects on antimicrobial, antioxidant, and antiglycation activities. Food Bioprocess Technol. 2024;17(11):4071–4082. doi:10.1007/s11947-024-03361-9
  • 18. Gökbulut A, Özhana O, Satılmiş B, Batçioğlu K, Günal S, Şarer E. Antioxidant and antimicrobial activities, and phenolic compounds of selected Inula species from Turkey. Nat Prod Commun. 2013;8(4):475–478. doi:10.1177/1934578X1300800
  • 19. Bayram M, Topuz S. Madımaktan (Polygonum cognatum Meissn.) Yanıt yüzey yöntemi kullanılarak fenolik bileşik ekstraksiyonunun optimizasyonu. Gıda. 2023;48(1):118–129. doi:10.15237/gida.GD22104
  • 20. Topuz S, Bayram M. Oleuropein extraction from leaves of three olive varieties (Olea europaea L.): Antioxidant and antimicrobial properties of purified oleuropein and oleuropein extracts. J Food Process Preserv. 2022;46(6):e15697. doi:10.1111/jfpp.15697
  • 21. Re R, Pellegrini N, Proteggente A, Pannala A, Yang M, Rice-Evans, C. Antioxidant activity applying an improved ABTS radical cation decolorization assay. Free Radic Biol Med. 1999;26(9–10):1231–1237. doi:10.1016/S0891-5849(98)00315-3
  • 22. Blasi F, Urbani E, Simonetti MS, Chiesi C, Cossignani L. Seasonal variations in antioxidant compounds of Olea europaea leaves collected from different Italian cultivars. J Appl Bot Food Qual. 2016;89. doi:10.5073/JABFQ.2016.089.025
  • 23. Benzie IF, Strain JJ. The ferric reducing ability of plasma (FRAP) as a measure of ‘antioxidant power’: the FRAP assay. Anal Biochem. 1996;239(1):70–76.
  • 24. Kavak DD, Akdeniz B. Sorbus umbellata (Desf.) Fritsch var. umbellata leaves: Optimization of extraction conditions and investigation antimicrobial, cytotoxic, and β-glucuronidase inhibitory potential. Plant Foods Hum Nutr. 2019;74:364–369. doi:10.1007/s11130-019-00743-9
  • 25. Natolino A, Passaghe P, Brugnera G, Comuzzo P. Intensification of grape marc (Vitis vinifera) exploitation by subcritical water-ethanol extraction: Effect on polyphenol bioactivities and kinetic modelling. J Food Eng. 2024;381:112185. doi:10.1016/j.jfoodeng.2024.112185
  • 26. Waszkowiak K, Gliszczyńska-Świgło A. Binary ethanol–water solvents affect phenolic profile and antioxidant capacity of flaxseed extracts. Eur Food Res Technol. 2016;242(5):777–786. doi:10.1007/s00217-015-2585-9
  • 27. Akthar J. Antioxidant and antimicrobial activities of Inula helenium. Technology. 2016;2(3):142–145.
  • 28. Albayrak S, Korkmaz Cinar AE, Paksoy MY, Aksoy A. An investigation on antioxidant and antimicrobial activities of four Inula helenium L. taxa. Iran J Sci Technol. 2015;39(4):473–483. doi:10.22099/ijsts.2015.3398
  • 29. Moradi N, Naghdi Badi H, Kalateh Jari S, Mehrafarin A, Danaee E. Diversity in photosynthetic pigments and phytochemical compounds among Iranian populations of Inula helenium L. Genet Resour Crop Evol. 2025;72(1):751–765. doi:10.1007/s10722-024-01955-y
  • 30. Orhan N, Gökbulut A, Orhan DD. Antioxidant potential and carbohydrate digestive enzyme inhibitory effects of five Inula species and their major compounds. S Afr J Bot. 2017;111:86–92. doi:10.1016/j.sajb.2017.03.040
  • 31. Sevindik E, Aydin S, Paksoy MY, Sokmen BB. Anti-urease, total phenolic content and antioxidant activities of some Inula L. (Asteraceae) taxa in Turkey. Genetika. 2020;52(3):825–834. doi:10.2298/GENSR2003825S

Optimization of Solvent Concentration in Phenolic Compound Extraction from Inula helenium L. Leaves Using D-Optimal Mixture Design

Year 2025, Volume: 12 Issue: 3, 155 - 161, 30.09.2025
https://doi.org/10.17350/HJSE19030000362

Abstract

nula helenium L. (Elecampane) leaves are an underutilized source of natural antioxidants due to their rich phenolic content. Although most studies have investigated roots or other aerial parts, limited information is available on phenolic extraction from I. helenium leaves. This study aimed to optimize the solvent concentrations for phenolic compound extraction from I. helenium leaves using D-Optimal Mixture Design and to evaluate the total phenolic content (TPC), total flavonoid content (TFC), and antioxidant activities of the extracts. Various solvent mixtures (ethanol, methanol, and water) were tested, and the optimal composition was determined as 42.40% ethanol, 0.00% methanol, and 57.60% water. Under these conditions, TPC and TFC were found to be 28.12 mg gallic acid equivalent (GAE)/g dry sample and 27.74 mg quercetin equivalent (QE)/g dry sample, respectively. Antioxidant activities measured by ABTS, DPPH, and FRAP assays were 19.73, 1.42, and 6.10 mg Trolox equivalent (TE)/g dry sample, respectively. These results indicate that I. helenium leaf extracts, with high phenolic content and potent antioxidant activity, represent a promising natural antioxidant source, particularly for applications in the food industry.

References

  • 1. Buza V, Niculae M, Hanganu D, Pall E, Burtescu RF, Olah NK. et al. Biological activities and chemical profile of Gentiana asclepiadea and Inula helenium ethanolic extracts. Molecules. 2022;27(11):3560. doi:10.3390/molecules27113560
  • 2. Akcın TA, Akcın A. Anatomy and micromorphology of Inula helenium subsp. orgyalis and I. ensifolia (Asteraceae) from Turkey. Not Sci Biol. 2017;9(1):104–109. doi:10.15835/nsb919950
  • 3. Wang J, Zhao YM, Guo CY, Zhang SM, Liu CL, ZhangDS, et al. Ultrasound-assisted extraction of total flavonoids from Inula helenium. Pharmacogn Mag. 2012;8(30):166–170. doi:10.4103/0973-1296.96581
  • 4. Aybastıer Ö. Efficacy of methanol-water extract of Inula helenium root against oxidative DNA damage. J Tradit Chin Med. 2021;41(2). doi:10.19852/j.cnki.jtcm.20210209.008
  • 5. Zlatić N, Jakovljević D, Stanković M. Temporal, plant part, and interpopulation variability of secondary metabolites and antioxidant activity of Inula helenium L. Plants. 2019;8(6):179. doi:10.3390/plants8060179
  • 6. Özcan FŞ, Dikmen H, Özcan N, Çetin Ö, Çelik M, Trendafilova A. Microwave-assisted extraction optimization of sesquiterpene lactones from Inula helenium roots: A sustainable approach to reduce energy consumption and carbon footprint. Food Sci Nutr. 2024;12(1):255–267. doi:10.1002/fsn3.3775
  • 7. Guo CY, Wang J, Hou Y, Zhao YM, Shen LX, Zhang DS. Orthogonal test design for optimizing the extraction of total flavonoids from Inula helenium. Pharmacogn Mag. 2013;9(35):192–195. doi:10.4103/0973-1296.113260
  • 8. Çoklar H, Akbulut M. Alıç (Crataegus orientalis) meyvesinin antioksidan aktivitesi ve fenolik bileşiklerinin ekstraksiyonu üzerine farklı çözgenlerin etkisi. Derim. 2016;33(2):237–248. doi:10.16882/derim.2016.267908
  • 9. Garcia-Salas P, Morales-Soto A, Segura-Carretero A, Fernández-Gutiérrez A. Phenolic-compound-extraction systems for fruit and vegetable samples. Molecules. 2010;15(12):8813–8826. doi:10.3390/molecules15128813
  • 10. Türkyılmaz M, Tağı Ş, Özkan M. Narın farklı bölümlerinin polifenol içeriği, antioksidan ve antibakteriyel aktivitesi üzerine ekstraksiyon çözgenlerinin etkisi. Akademik Gıda. 2017;15(2):109–118. doi:10.24323/akademik-gida.333632
  • 11. Galvan D, Effting L, Cremasco H, Conte-Junior CA. Recent applications of mixture designs in beverages, foods, and pharmaceutical health: A systematic review and meta-analysis. Foods. 2021;10(8):1941. doi:10.3390/foods10081941
  • 12. Sanjaya IPW, Chan MT, Sukma D, Buchori A, Putra RP, Nurcholis W. D-optimal design optimization of solvent mixture for flavonoid extraction from Phalaenopsis leaves with antioxidant activity. J Pharm Bioallied Sci. 2024;16(1):1–7. doi:10.4103/jpbs.jpbs_372_23
  • 13. Vural N, Cavuldak ÖA, Akay MA. D-optimal design and multi-objective optimization for green extraction conditions developed with ultrasonic probe for oleuropein. J Appl Res Med Aromat Plants. 2021;20:100279. doi:10.1016/j.jarmap.2020.100279
  • 14. Frumuzachi O, Nicolescu A, Babotă M, Mocan A, Sisea CR, Hera O, Rocchetti G. D-optimal design-based ultrasound-assisted extraction optimization and extensive bio-structural analysis of phenolic compounds from Romanian cornelian cherry (Cornus mas L.) genotypes. Food Bioprocess Technol. 2025;1–18. doi:10.1007/s11947-025-03914-6
  • 15. Yan H, Haiming S, Cheng G, Xiaobo L. Chemical constituents of the roots of Inula helenium. Chem Nat Compd. 2012;48(3):522–524. doi:10.1007/s10600-012-0298-x
  • 16. Spiridon I, Nechita CB, Niculaua M, Silion M, Armatu A, Teacă CA, Bodîrlău R. Antioxidant and chemical properties of Inula helenium root extracts. Cent Eur J Chem. 2013;11(10):1699–1709. doi:10.2478/s11532-013-0295-3
  • 17. Özcan FŞ, Özcan N, Dikmen Meral H, Çetin Ö, Çelik M, Trendafilova A. Extraction of sesquiterpene lactones from Inula helenium roots by high-pressure homogenization and effects on antimicrobial, antioxidant, and antiglycation activities. Food Bioprocess Technol. 2024;17(11):4071–4082. doi:10.1007/s11947-024-03361-9
  • 18. Gökbulut A, Özhana O, Satılmiş B, Batçioğlu K, Günal S, Şarer E. Antioxidant and antimicrobial activities, and phenolic compounds of selected Inula species from Turkey. Nat Prod Commun. 2013;8(4):475–478. doi:10.1177/1934578X1300800
  • 19. Bayram M, Topuz S. Madımaktan (Polygonum cognatum Meissn.) Yanıt yüzey yöntemi kullanılarak fenolik bileşik ekstraksiyonunun optimizasyonu. Gıda. 2023;48(1):118–129. doi:10.15237/gida.GD22104
  • 20. Topuz S, Bayram M. Oleuropein extraction from leaves of three olive varieties (Olea europaea L.): Antioxidant and antimicrobial properties of purified oleuropein and oleuropein extracts. J Food Process Preserv. 2022;46(6):e15697. doi:10.1111/jfpp.15697
  • 21. Re R, Pellegrini N, Proteggente A, Pannala A, Yang M, Rice-Evans, C. Antioxidant activity applying an improved ABTS radical cation decolorization assay. Free Radic Biol Med. 1999;26(9–10):1231–1237. doi:10.1016/S0891-5849(98)00315-3
  • 22. Blasi F, Urbani E, Simonetti MS, Chiesi C, Cossignani L. Seasonal variations in antioxidant compounds of Olea europaea leaves collected from different Italian cultivars. J Appl Bot Food Qual. 2016;89. doi:10.5073/JABFQ.2016.089.025
  • 23. Benzie IF, Strain JJ. The ferric reducing ability of plasma (FRAP) as a measure of ‘antioxidant power’: the FRAP assay. Anal Biochem. 1996;239(1):70–76.
  • 24. Kavak DD, Akdeniz B. Sorbus umbellata (Desf.) Fritsch var. umbellata leaves: Optimization of extraction conditions and investigation antimicrobial, cytotoxic, and β-glucuronidase inhibitory potential. Plant Foods Hum Nutr. 2019;74:364–369. doi:10.1007/s11130-019-00743-9
  • 25. Natolino A, Passaghe P, Brugnera G, Comuzzo P. Intensification of grape marc (Vitis vinifera) exploitation by subcritical water-ethanol extraction: Effect on polyphenol bioactivities and kinetic modelling. J Food Eng. 2024;381:112185. doi:10.1016/j.jfoodeng.2024.112185
  • 26. Waszkowiak K, Gliszczyńska-Świgło A. Binary ethanol–water solvents affect phenolic profile and antioxidant capacity of flaxseed extracts. Eur Food Res Technol. 2016;242(5):777–786. doi:10.1007/s00217-015-2585-9
  • 27. Akthar J. Antioxidant and antimicrobial activities of Inula helenium. Technology. 2016;2(3):142–145.
  • 28. Albayrak S, Korkmaz Cinar AE, Paksoy MY, Aksoy A. An investigation on antioxidant and antimicrobial activities of four Inula helenium L. taxa. Iran J Sci Technol. 2015;39(4):473–483. doi:10.22099/ijsts.2015.3398
  • 29. Moradi N, Naghdi Badi H, Kalateh Jari S, Mehrafarin A, Danaee E. Diversity in photosynthetic pigments and phytochemical compounds among Iranian populations of Inula helenium L. Genet Resour Crop Evol. 2025;72(1):751–765. doi:10.1007/s10722-024-01955-y
  • 30. Orhan N, Gökbulut A, Orhan DD. Antioxidant potential and carbohydrate digestive enzyme inhibitory effects of five Inula species and their major compounds. S Afr J Bot. 2017;111:86–92. doi:10.1016/j.sajb.2017.03.040
  • 31. Sevindik E, Aydin S, Paksoy MY, Sokmen BB. Anti-urease, total phenolic content and antioxidant activities of some Inula L. (Asteraceae) taxa in Turkey. Genetika. 2020;52(3):825–834. doi:10.2298/GENSR2003825S
There are 31 citations in total.

Details

Primary Language English
Subjects Food Engineering
Journal Section Research Articles
Authors

Esra Esin 0000-0003-0470-0015

Semra Topuz Türker 0000-0002-9122-0839

Publication Date September 30, 2025
Submission Date June 12, 2025
Acceptance Date September 11, 2025
Published in Issue Year 2025 Volume: 12 Issue: 3

Cite

Vancouver Esin E, Topuz Türker S. Optimization of Solvent Concentration in Phenolic Compound Extraction from Inula helenium L. Leaves Using D-Optimal Mixture Design. Hittite J Sci Eng. 2025;12(3):155-61.

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