Skip to main content
SpringerLink
Log in

Ultrasound-assisted extraction process of phenolic antioxidants from Olive leaves: a nutraceutical study using RSM and LC–ESI–DAD–MS

  • Original Article
  • Published:
Journal of Food Science and Technology Aims and scope Submit manuscript

Abstract

In recent years, there has been an ever growing interest in finding new natural sources of food antioxidants. As a main fruit crop, olive is also valued due to its phenolic-containing leaves. Mathematically based optimization methods are used as powerful tools to extract different antioxidant compounds. The present study is aimed to provide an efficient extraction method for total phenol content (TPC), total flavonoid content (TFC) and antioxidant ability (DPPH scavenging assay and FRAP). The effects of ultrasonic temperature (35–65 °C), ultrasonic time (5–15 min), and ethanol to water ratio (Et: W) (25–75%) were evaluated. Second-order polynomial models were used through a rotatable Box-Behnken design (BBD) consisting of 15 experimental runs with three replicates at the center point. Interactional effects of the studied factors were significant in most cases for all responses. The highest extraction efficiency was found to be fifty-one percent of ethanol (65 °C, 15 min) to water ratio. Under optimal conditions, values for TPC, TFC, DPPHsc and FRAP assay were 183.4 (mg GAE. g−1 DW), 696.77 (mg Quercetin. g−1 DW), 78.98 (DPPHsc %) and 1942 µmol Fe+2/g DW, respectively. R 2 values (R 2 > 0.92) showed that RSM models could efficiently predict the yield of all responses. In the LC–ESI–MS–DAD profiling of the optimized extract, 27 compounds were identified with oleuropein as the main compound. In the present study, olive leaf is introduced as a promising source of natural antioxidant and can be used in food industries following further studies.

This is a preview of subscription content, log in via an institution to check access.

Access this article

Log in via an institution

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Institutional subscriptions

Fig. 1
Fig. 2
Fig. 3
Fig. 4

Similar content being viewed by others

References

  • Abbas S, Hayat K, Karangwa E, Bashari M, Zhang X (2013) An overview of ultrasound-assisted food-grade nanoemulsions. Food Eng Rev 5:139–157

    Article  CAS  Google Scholar 

  • Benzie IF, Strain J (1996) The ferric reducing ability of plasma (FRAP) as a measure of “antioxidant power”: the FRAP assay. Anal Biochem 239:70–76

    Article  CAS  Google Scholar 

  • Box GE, Wilson K (1951) On the experimental attainment of optimum conditions. J R Stat Soc Ser B (Methodol) 13:1–45

    Google Scholar 

  • Chandrapala J, Leong T (2015) Ultrasonic processing for dairy applications: recent advances. Food Eng Rev 7:143–158

    Article  Google Scholar 

  • Chemat F, Rombaut N, Sicaire A-G, Meullemiestre A, Fabiano-Tixier A-S, Abert-Vian M (2017) Ultrasound-assisted extraction of food and natural products. Mechanisms, techniques, combinations, protocols and applications. A review. Ultrason Sonochem 34:540–560

    Article  CAS  Google Scholar 

  • Chen C, Shao Y, Tao Y, Wen H (2015a) Optimization of dynamic microwave-assisted extraction of Armillaria polysaccharides using RSM, and their biological activity. Food Sci Technol-LEB 64:1263–1269

    Article  CAS  Google Scholar 

  • Chen M, Zhao Y, Yu S (2015b) Optimisation of ultrasonic-assisted extraction of phenolic compounds, antioxidants, and anthocyanins from sugar beet molasses. Food Chem 172:543–550

    Article  CAS  Google Scholar 

  • Chiou A, Karathanos VT, Mylona A, Salta FN, Preventi F, Andrikopoulos NK (2007) Currants (Vitis vinifera L.) content of simple phenolics and antioxidant activity. Food Chem 102:516–522

    Article  CAS  Google Scholar 

  • Erbay Z, Icier F (2010) The importance and potential uses of olive leaves. Food Rev Int 26:319–334

    Article  CAS  Google Scholar 

  • Fattahi M, Rahimi R (2016) Optimization of extraction parameters of phenolic antioxidants from leaves of Capparis spinosa using response surface methodology. Food Anal Method 9:2321–2334

    Article  Google Scholar 

  • García-Villalba R, Larrosa M, Possemiers S, Tomás-Barberán F, Espín J (2014) Bioavailability of phenolics from an oleuropein-rich olive (Olea europaea) leaf extract and its acute effect on plasma antioxidant status: comparison between pre-and postmenopausal women. Eur J Nutr 53:1015–1027

    Article  Google Scholar 

  • Ghanbari R, Anwar F, Alkharfy KM, Gilani A-H, Saari N (2012) Valuable nutrients and functional bioactives in different parts of olive (Olea europaea L.)-a review. Int J Mol Sci 13:3291–3340

    Article  CAS  Google Scholar 

  • Ignat I, Volf I, Popa VI (2011) A critical review of methods for characterisation of polyphenolic compounds in fruits and vegetables. Food Chem 126:1821–1835

    Article  CAS  Google Scholar 

  • Ilaiyaraja N, Likhith K, Babu GS, Khanum F (2015) Optimisation of extraction of bioactive compounds from Feronia limonia (wood apple) fruit using response surface methodology (RSM). Food Chem 173:348–354

    Article  CAS  Google Scholar 

  • Jemai H, Bouaziz M, Fki I, El Feki A, Sayadi S (2008) Hypolipidimic and antioxidant activities of oleuropein and its hydrolysis derivative-rich extracts from Chemlali olive leaves. Chem-Biol Interact 176:88–98

    Article  CAS  Google Scholar 

  • Khiari Z, Makris DP, Kefalas P (2009) An investigation on the recovery of antioxidant phenolics from onion solid wastes employing water/ethanol-based solvent systems. Food Bioprocess Tech 2:337–343

    Article  CAS  Google Scholar 

  • Lee L-S, Lee N, Kim YH, Lee C-H, Hong SP, Jeon Y-W, Kim Y-E (2013) Optimization of ultrasonic extraction of phenolic antioxidants from green tea using response surface methodology. Molecules 18:13530–13545

    Article  CAS  Google Scholar 

  • Liyana-Pathirana C, Shahidi F (2005) Optimization of extraction of phenolic compounds from wheat using response surface methodology. Food Chem 93:47–56

    Article  CAS  Google Scholar 

  • Lobo V, Patil A, Phatak A, Chandra N (2010) Free radicals, antioxidants and functional foods: Impact on human health. Pharmacogn Rev 4:118

    Article  CAS  Google Scholar 

  • Macías-Sánchez M, Mantell C, Rodriguez M, de la Ossa EM, Lubián L, Montero O (2009) Comparison of supercritical fluid and ultrasound-assisted extraction of carotenoids and chlorophyll a from Dunaliella salina. Talanta 77:948–952

    Article  Google Scholar 

  • Meziant L, Benchikh Y, Louaileche H (2014) Deployment of response surface methodology to optimize recovery of dark fresh fig (Ficus carica L., var. Azenjar) total phenolic compounds and antioxidant activity. Food Chem 162:277–282

    Article  Google Scholar 

  • Myers WR, Montgomery DC (2003) Response surface methodology. Encycl Biopharm Stat 1:858–869

    Google Scholar 

  • Nakajima J-i, Tanaka I, Seo S, Yamazaki M, Saito K (2004) LC/PDA/ESI-MS profiling and radical scavenging activity of anthocyanins in various berries. J BioMed Biotech 2004:241–247

    Article  Google Scholar 

  • Niknam V, Ebrahimzadeh H (2002) Phenolics contents in Astragalus species. Pak J Bot 34:283–289

    Google Scholar 

  • Omar SH (2010) Oleuropein in olive and its pharmacological effects. Sci Pharm 78:133–154

    Article  CAS  Google Scholar 

  • Özcan MM, Matthäus B (2017) A review: benefit and bioactive properties of olive (Olea europaea L.) leaves. Eur Food Res Technol 243:89–99

    Article  Google Scholar 

  • Prakash O, Talat M, Hasan S, Pandey RK (2008) Factorial design for the optimization of enzymatic detection of cadmium in aqueous solution using immobilized urease from vegetable waste. Bioresource Technol 99:7565–7572

    Article  CAS  Google Scholar 

  • Prommuak C, De-Eknamkul W, Shotipruk A (2008) Extraction of flavonoids and carotenoids from Thai silk waste and antioxidant activity of extracts. Sep Purif Technol 62:444–448

    Article  CAS  Google Scholar 

  • Puértolas E, Saldana G, Álvarez I, Raso J (2011) Experimental design approach for the evaluation of anthocyanin content of rose wines obtained by pulsed electric fields. Influence of temperature and time of maceration. Food Chem 126:1482–1487

    Article  Google Scholar 

  • Radojkovića M, Zekovića Z, Jokićb S, Vidovića S (2012) Determination of optimal extraction parameters of mulberry leaves using Response Surface Methodology (RSM). Rom Biotech Lett 17:7295–7308

    Google Scholar 

  • Şahin S, Şamlı R (2013) Optimization of olive leaf extract obtained by ultrasound-assisted extraction with response surface methodology. Ultrason sonochem 20:595–602

    Article  Google Scholar 

  • Shi J, Yu J, Pohorly J, Young JC, Bryan M, Wu Y (2003) Optimization of the extraction of polyphenols from grape seed meal by aqueous ethanol solution. J Food Agric Environ 1:42–47

    CAS  Google Scholar 

  • Shin Y, Liu RH, Nock JF, Holliday D, Watkins CB (2007) Temperature and relative humidity effects on quality, total ascorbic acid, phenolics and flavonoid concentrations, and antioxidant activity of strawberry. Postharvest Biol Tec 45:349–357

    Article  CAS  Google Scholar 

  • Silva EM, Rogez H, Larondelle Y (2007) Optimization of extraction of phenolics from Inga edulis leaves using response surface methodology. Sep Purif Technol 55:381–387

    Article  CAS  Google Scholar 

  • Slinkard K, Singleton VL (1977) Total phenol analysis: automation and comparison with manual methods. Am J Enol Viticult 28:49–55

    CAS  Google Scholar 

  • Valko M, Leibfritz D, Moncol J, Cronin MT, Mazur M, Telser J (2007) Free radicals and antioxidants in normal physiological functions and human disease. Int J Biochem Cell Biol 39:44–84

    Article  CAS  Google Scholar 

  • Vinatoru M, Toma M, Radu O, Filip P, Lazurca D, Mason T (1997) The use of ultrasound for the extraction of bioactive principles from plant materials. Ultrason Sonochem 4:135–139

    Article  CAS  Google Scholar 

Download references

Acknowledgements

Work performed in Department of Department of Plant Biology, College of Science, University of Tehran. The authors are very grateful to the members of “Soil and Water Research Department of Zanjan Agricultural and Natural Resources Research and Education Center” and “Department of Horticulture of Urmia University” for their scientific support in some parts of the present study.

Funding

This study was funded by University of Tehran.

Author information

Authors and Affiliations

  1. Department of Plant Biology, and Center of Excellence in Phylogeny of Living Organisms in Iran, School of Biology, College of Science, University of Tehran, Tehran, 14155-6455, Iran

    Habib Shirzad, Vahid Niknam & Hassan Ebrahimzadeh

  2. Soil and Water Research Department, Zanjan Agricultural and Natural Resources Research and Education Center, Agricultural Research, Education and Extension Organization (AREEO), Zanjan, Iran

    Mehdi Taheri

Authors
  1. Habib Shirzad
    View author publications

    You can also search for this author in PubMed Google Scholar

  2. Vahid Niknam
    View author publications

    You can also search for this author in PubMed Google Scholar

  3. Mehdi Taheri
    View author publications

    You can also search for this author in PubMed Google Scholar

  4. Hassan Ebrahimzadeh
    View author publications

    You can also search for this author in PubMed Google Scholar

Corresponding author

Correspondence to Vahid Niknam.

Ethics declarations

Conflict of interest

The authors declare that there is no conflict of interest in this study.

Ethical approval

This article does not contain any studies with human participants performed by any of the authors.

Informed consent

Publication has been approved by all individual participants.

Electronic supplementary material

Below is the link to the electronic supplementary material.

13197_2017_2676_MOESM1_ESM.doc

Analysis of variance (ANOVA) and the estimated regression coefficients for the total phenolic content (TPC), total flavonoid content (TFC), and DPPHsc (%), FRAP. values to determine the suitability of second-order polynomial model fitting in the experimental data (DOC 63 kb)

Rights and permissions

Reprints and permissions

About this article

Check for updates. Verify currency and authenticity via CrossMark

Cite this article

Shirzad, H., Niknam, V., Taheri, M. et al. Ultrasound-assisted extraction process of phenolic antioxidants from Olive leaves: a nutraceutical study using RSM and LC–ESI–DAD–MS. J Food Sci Technol 54, 2361–2371 (2017). https://doi.org/10.1007/s13197-017-2676-7

Download citation

  • Revised:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s13197-017-2676-7

Keywords

Search

Navigation