Grape seeds (Vitis vinifera) are rich in phytochemicals that have antioxidant properties. The influence of independent variables such as microwave power (100, 150, and 200 W), extraction time (2, 4, and 6 min), and solvent concentration (30%, 45%, and 60% ethanol) and their interactions on total phenols and the antioxidant activity (1,1-diphenyl-2-picrylhydrazyl (DPPH) and ferric ion reducing antioxidant power (FRAP)) were determined; and the microwave-assisted extraction (MAE) process was optimized using a central composite design. The total phenols that were expressed as gallic acid equivalents (GAE), catechin equivalents (CAT), and tannic acid equivalents (TAE) were significantly influenced by the solvent concentration and the time of extraction. A numerical optimization was carried out to obtain the overall conditions for MAE of phenolic antioxidants from grape seed. The response variables were maximized for 6 min of MAE of grape seed (GS) with 32.6% ethanol at 121 W with a desirability function of 0.947. The predicted extraction yields were 13 ± 0.89, 21.6 ± 1.59, and 15.9 ± 1.32 mg GAE, CAT, and TAE, respectively per gram of GS. The predicted antioxidant activity per gram of dry weight GS was 80.9% for the inhibition of DPPH and 135 μM ascorbic acid equivalents for FRAP test. The predicted response values were significantly correlated with the observed ones as follows: GAE r = 0.995, CAT r = 0.990, TAE r = 0.996, DPPH r = 0.996, and FRAP r = 0.996.
This is a preview of subscription content, access via your institution.
Buy single article
Instant access to the full article PDF.
Price excludes VAT (USA)
Tax calculation will be finalised during checkout.
Abdeshahian, P., Samat, N., & Yusoff, W. M. W. (2010). Utilization of palm kernel cake for production of beta-glucosidase by Aspergillus niger FTCC 5003 in solid substrate fermentation using an aerated column bioreactor. Biotechnology, 9(1), 17–24.
Al-Awwadi, N. A., Araiz, C., Bornet, A., Delbosc, S., Cristol, J. P., Linck, N., et al. (2005). Extracts enriched in different polyphenolic families normalize increased cardiac NADPH oxidase expression while having differential effects on insulin resistance, hypertension, and cardiac hypertrophy in high-fructose-fed rats. Journal of Agricultural and Food Chemistry, 53(1), 151–157.
Bail, S., Stuebiger, G., Krist, S., Unterweger, H., & Buchbauer, G. (2008). Characterisation of various grape seed oils by volatile compounds, triacylglycerol composition, total phenols and antioxidant capacity. Food Chemistry, 108(3), 1122–1132.
Ballard, T. S., Mallikarjunan, P., Zhou, K., & O’Keefe, S. F. (2009). Optimizing the extraction of phenolic antioxidants from peanut skins using response surface methodology. Journal of Agricultural and Food Chemistry, 57(8), 3064–3072.
Baoshan Sun, M., & Spranger, I. (2005). Review: quantitative extraction and analysis of grape and wine proanthocyanidins and stilbenes. Ciência Téc Vitiv, 20(2), 59–89.
Benzie, I. F. F., & Strain, J. (1996). The ferric reducing ability of plasma (FRAP) as a measure of “antioxidant power”: the FRAP assay. Analytical Biochemistry, 239(1), 70–76.
Bezerra, M. A., Santelli, R. E., Oliveira, E. P., Villar, L. S., & Escaleira, L. A. (2008). Response surface methodology (RSM) as a tool for optimization in analytical chemistry. Talanta, 76(5), 965–977.
Buci Koji, A., Planini, M., Tomas, S., Jakobek, L., & Šeruga, M. (2009). Influence of solvent and temperature on extraction of phenolic compounds from grape seed, antioxidant activity and colour of extract. International Journal of Food Science and Technology, 44(12), 2394–2401.
Cacace, J., & Mazza, G. (2003). Mass transfer process during extraction of phenolic compounds from milled berries. Journal of Food Engineering, 59(4), 379–389.
Canals, R., Llaudy, M., Valls, J., Canals, J., & Zamora, F. (2005). Influence of ethanol concentration on the extraction of color and phenolic compounds from the skin and seeds of Tempranillo grapes at different stages of ripening. Journal of Agricultural and Food Chemistry, 53(10), 4019–4025.
Castillo, J., Benavente-Garcia, O., Lorente, J., Alcaraz, M., Redondo, A., Ortuno, A., et al. (2000). Antioxidant activity and radioprotective effects against chromosomal damage induced in vivo by X-rays of flavan-3-ols (Procyanidins) from grape seeds (Vitis vinifera): Comparative study versus other phenolic and organic compounds. Journal of Agricultural and Food Chemistry, 48(5), 1738–1745.
Chen, S., & Spiro, M. (1994). Study of microwave extraction of essential oil constituents from plant materials. The Journal of Microwave Power and Electromagnetic Energy, 29(4), 231–241.
Cheynier, V., & Rigaud, J. (1986). HPLC separation and characterization of flavonols in the skins of Vitis vinifera var. Cinsault. American Journal of Enology and Viticulture, 37(4), 248.
Craveiro, A., Matos, F., Alencar, J., & Plumel, M. (1989). Microwave oven extraction of an essential oil. Flavour and Fragrance Journal, 4(1), 43–44.
Dandekar, D. V., & Gaikar, V. (2002). Microwave assisted extraction of curcuminoids from Curcuma longa. Separation Science and Technology, 37(11), 2669–2690.
Deighton, N., Brennan, R., Finn, C., & Davies, H. V. (2000). Antioxidant properties of domesticated and wild Rubus species. Journal of the Science of Food and Agriculture, 80(9), 1307–1313.
Del Bas, J. M., Fernández-Larrea, J., Blay, M., Ardèvol, A., Salvadó, M. J., Arola, L., et al. (2005). Grape seed procyanidins improve atherosclerotic risk index and induce liver CYP7A1 and SHP expression in healthy rats. The FASEB Journal, 19(3), 479.
FAOSTAT. (2011). World production quantity of grapes: 2009. Food and Agricultural Organization of the United Nations. FAO Statistics Division 2011. Available at: http://faostat.fao.org/. Accessed 04 October 2011.
Freitas, V. A. P., Glories, Y., Bourgeois, G., & Vitry, C. (1998). Characterisation of oligomeric and polymeric procyanidins from grape seeds by liquid secondary ion mass spectrometry. Phytochemistry, 49(5), 1435–1441.
Ganzler, K., Szinai, I., & Salgo, A. (1990). Effective sample preparation method for extracting biologically active compounds from different matrices by a microwave technique. Journal of Chromatography. A, 520, 257–262.
Garcia-Marino, M., Rivas-Gonzalo, J. C., Ibanez, E., & Garcia-Moreno, C. (2006). Recovery of catechins and proanthocyanidins from winery by-products using subcritical water extraction. Analytica Chimica Acta, 563(1–2), 44–50.
Ghafoor, K., Choi, Y. H., Jeon, J. Y., & Jo, I. H. (2009). Optimization of ultrasound-assisted extraction of phenolic compounds, antioxidants, and anthocyanins from grape (Vitis vinifera) seeds. Journal of Agricultural and Food Chemistry, 57(11), 4988–4994.
Gokturk Baydar, N., Ozkan, G., & Yasar, S. (2007). Evaluation of the antiradical and antioxidant potential of grape extracts. Food Control, 18(9), 1131–1136.
Gómez-Alonso, S., García-Romero, E., & Hermosín-Gutiérrez, I. (2007). HPLC analysis of diverse grape and wine phenolics using direct injection and multidetection by DAD and fluorescence. Journal of Food Composition and Analysis, 20(7), 618–626.
Guo, L., Wang, L. H., Sun, B., Yang, J. Y., Zhao, Y. Q., Dong, Y. X., et al. (2007). Direct in vivo evidence of protective effects of grape seed procyanidin fractions and other antioxidants against ethanol-induced oxidative DNA damage in mouse brain cells. Journal of Agricultural and Food Chemistry, 55(14), 5881–5891.
Haaland, P. D. (1989). Experimental design in biotechnology. Boca Raton: CRC.
Harman, D. (1995). Role of antioxidant nutrients in aging: overview. Age, 18(2), 51–62.
Hong, N., Yaylayan, V. A., Raghavan, G. S., Paré, J. R., & Bélanger, J. M. (2001). Microwave-assisted extraction of phenolic compounds from grape seed. Natural Product Letters, 15(3), 197.
Jayaprakasha, G. K., & Jaganmohan Rao, L. (2000). Phenolic constituents from lichen Parmotrema stuppeum (Nyl.) Hale and their antioxidant activity. Zeitschrift fu¨r Naturforschung, 55, 1018–1022.
Jayaprakasha, G., Singh, R., & Sakariah, K. (2001). Antioxidant activity of grape seed (Vitis vinifera) extracts on peroxidation models in vitro. Food Chemistry, 73(3), 285–290.
Jayaprakasha, G., Selvi, T., & Sakariah, K. (2003). Antibacterial and antioxidant activities of grape (Vitis vinifera) seed extracts. Food Research International, 36(2), 117–122.
Katalinic, V., Milos, M., Modun, D., Musi, I., & Boban, M. (2004). Antioxidant effectiveness of selected wines in comparison with (+)-catechin. Food Chemistry, 86(4), 593–600.
Kim, S. Y., Jeong, S. M., Park, W. P., Nam, K., Ahn, D., & Lee, S. C. (2006). Effect of heating conditions of grape seeds on the antioxidant activity of grape seed extracts. Food Chemistry, 97(3), 472–479.
Koundouras, S., Marinos, V., Gkoulioti, A., Kotseridis, Y., & van Leeuwen, C. (2006). Influence of vineyard location and vine water status on fruit maturation of nonirrigated cv. Agiorgitiko (Vitis vinifera L.). Effects on wine phenolic and aroma components. Journal of Agricultural and Food Chemistry, 54(14), 5077–5086.
Lee, J., Koo, N., & Min, D. (2004). Reactive oxygen species, aging, and antioxidative nutraceuticals. Comprehensive Reviews in Food Science and Food Safety, 3(1), 21–33.
Li, H., Wang, X., Li, P., Li, Y., & Wang, H. (2008). Comparative study of antioxidant activity of grape (Vitis vinifera) seed powder assessed by different methods. Journal of Food and Drug Analysis, 16, 67–73.
Lundstedt, T., Seifert, E., Abramo, L., Thelin, B., Nystrom, A., Pettersen, J., et al. (1998). Experimental design and optimization. Chemometrics and Intelligent Laboratory Systems, 42(1–2), 3–40.
Maier, T., Schieber, A., Kammerer, D. R., & Carle, R. (2009). Residues of grape (Vitis vinifera L.) seed oil production as a valuable source of phenolic antioxidants. Food Chemistry, 112(3), 551–559.
Mandic, A. I., Ilas, S. M., Etkovi, G. S., Anadanovi-Brunet, J. M., & Tumbas, V. T. (2008). Polyphenolic composition and antioxidant activities of grape seed extract. International Journal of Food Properties, 11(4), 713–726.
Mayer, R., Stecher, G., Wuerzner, R., Silva, R. C., Sultana, T., Trojer, L., et al. (2008). Proanthocyanidins: target compounds as antibacterial agents. Journal of Agricultural and Food Chemistry, 56(16), 6959–6966.
Mazza, G., & Francis, F. (1995). Anthocyanins in grapes and grape products. Critical Reviews in Food Science and Nutrition, 35(4), 341–371.
Meyer, A. S., Yi, O. S., Pearson, D. A., Waterhouse, A. L., & Frankel, E. N. (1997). Inhibition of human low-density lipoprotein oxidation in relation to composition of phenolic antioxidants in grapes (Vitis vinifera). Journal of Agricultural and Food Chemistry, 45(5), 1638–1643.
Nair, V. D. P., Dairam, A., Agbonon, A., Arnason, J., Foster, B., & Kanfer, I. (2007). Investigation of the antioxidant activity of African potato (Hypoxis hemerocallidea). Journal of Agricultural and Food Chemistry, 55(5), 1707–1711.
Nemes, S. M., & Orsat, V. (2009). Microwave-assisted extraction of secoisolariciresinol diglucoside—Method development. Food and Bioprocess Technology 1-9.
Nemes, S. M., & Orsat, V. (2010). Screening the experimental domain for the microwave-assisted extraction of secoisolariciresinol diglucoside from flaxseed prior to optimization procedures. Food and Bioprocess Technology, 3(2), 300–307.
Pallaroni, L., Von Holst, C., Eskilsson, C., & Björklund, E. (2002). Microwave-assisted extraction of zearalenone from wheat and corn. Analytical and Bioanalytical Chemistry, 374(1), 161–166.
Pan, X., Liu, H., Jia, G., & Shu, Y. Y. (2000). Microwave-assisted extraction of glycyrrhizic acid from licorice root. Biochemical Engineering Journal, 5(3), 173–177.
Pan, X., Niu, G., & Liu, H. (2003). Microwave-assisted extraction of tea polyphenols and tea caffeine from green tea leaves. Chemical Engineering and Processing, 42(2), 129–133.
Pan, Y., Wang, K., Huang, S., Wang, H., Mu, X., He, C., et al. (2008). Antioxidant activity of microwave-assisted extract of longan (Dimocarpus Longan Lour.) peel. Food Chemistry, 106(3), 1264–1270.
Pinent, M., Blay, M., Blade, M., Salvado, M., Arola, L., & Ardevol, A. (2004). Grape seed-derived procyanidins have an antihyperglycemic effect in streptozotocin-induced diabetic rats and insulinomimetic activity in insulin-sensitive cell lines. Endocrinology, 145(11), 4985.
Pokorn, J. (1991). Natural antioxidants for food use. Trends in Food Science & Technology, 2, 223–227.
Puiggròs, F., Llópiz, N., Ardévol, A., Bladé, C., Arola, L., & Salvadó, M. J. (2005). Grape seed procyanidins prevent oxidative injury by modulating the expression of antioxidant enzyme systems. Journal of Agricultural and Food Chemistry, 53(15), 6080–6086.
Ramchandani, A. G., Chettiyar, R. S., & Pakhale, S. S. (2010). Evaluation of antioxidant and anti-initiating activities of crude polyphenolic extracts from seedless and seeded Indian grapes. Food Chemistry, 119(1), 298–305.
Singh, A., Sabally, K., Kubow, S., Donnelly, D. J., Gariepy, Y., Orsat, V., et al. (2011). Microwave-assisted extraction of phenolic antioxidants from potato peels. Molecules, 16(3), 2218–2232.
Spranger, I., Sun, B., Mateus, A. M., Freitas, V., & Ricardo-da-Silva, J. M. (2008). Chemical characterization and antioxidant activities of oligomeric and polymeric procyanidin fractions from grape seeds. Food Chemistry, 108(2), 519–532.
Stintzing, F. C., Stintzing, A. S., Carle, R., Frei, B., & Wrolstad, R. E. (2002). Color and antioxidant properties of cyanidin-based anthocyanin pigments. Journal of Agricultural and Food Chemistry, 50(21), 6172–6181.
Sun, Y., Liao, X., Wang, Z., Hu, X., & Chen, F. (2007). Optimization of microwave-assisted extraction of anthocyanins in red raspberries and identification of anthocyanin of extracts using high-performance liquid chromatography–mass spectrometry. European Food Research and Technology, 225(3), 511–523.
Terra, X., Valls, J., Vitrac, X., Mérrillon, J. M., Arola, L., Ardèvol, A., et al. (2007). Grape-seed procyanidins act as antiinflammatory agents in endotoxin-stimulated RAW 264.7 macrophages by inhibiting NFkB signaling pathway. Journal of Agricultural and Food Chemistry, 55(11), 4357–4365.
Thostenson, E., & Chou, T. W. (1999). Microwave processing: fundamentals and applications. Composites Part A: Applied Science and Manufacturing, 30(9), 1055–1071.
Wang, S., Chen, F., Wu, J., Wang, Z., Liao, X., & Hu, X. (2007). Optimization of pectin extraction assisted by microwave from apple pomace using response surface methodology. Journal of Food Engineering, 78(2), 693–700.
Wang, Y., Xi, G. S., Zheng, Y. C., & Miao, F. S. (2010). Microwave-assisted extraction of flavonoids from Chinese herb Radix puerariae (Ge Gen). Journal of Medicinal Plant Research, 4(4), 304–308.
Wrolstad, R. E., Durst, R. W., & Lee, J. (2005). Tracking color and pigment changes in anthocyanin products. Trends in Food Science & Technology, 16(9), 423–428.
Yamakoshi, J., Saito, M., Kataoka, S., & Tokutake, S. (2002). Procyanidin-rich extract from grape seeds prevents cataract formation in hereditary cataractous (ICR/f) rats. Journal of Agricultural and Food Chemistry, 50(17), 4983–4988.
Zumbo, B., & Harwell, M. (1999). The methodology of methodological research: Analyzing the results of simulation experiments (Paper No. ESQBS-99-2). Prince George, BC: University of Northern British Columbia Edgeworth Laboratory for Quantitative Behavioral Science.
We thank the Dept. of Foreign Affairs and International Trade, Canada for providing the Canadian Commonwealth Scholarship, 2010. Thanks to Simona Nemes and Ashutosh Singh, Dept. of Bioresource Engineering, McGill University for their technical expertise and support.
Rights and permissions
About this article
Cite this article
Krishnaswamy, K., Orsat, V., Gariépy, Y. et al. Optimization of Microwave-Assisted Extraction of Phenolic Antioxidants from Grape Seeds (Vitis vinifera). Food Bioprocess Technol 6, 441–455 (2013). https://doi.org/10.1007/s11947-012-0800-2
- Gallic acid
- Tannic acid
- Response surface methodology
- Antioxidant activity