Effect of encapsulation of polyphenolic compounds of unripe (sour) grape waste on its quality and stability

Document Type : Original research


Department of Food Industry, Faculty of Agriculture, Ferdowsi University of Mashhad, Mashhad, Iran


In the present study, to prepare the polyphenolic extract of sour grape waste, the simultaneous effect of enzyme (pectinase, Yieldmash) and ultrasound (for 10, 25 and 40 minutes at sound intensity of 30, 60 and 90%) treatments was used and the best sample was encapsulated with maltodextrin and basil seed gum (BSG). To optimize the preparation of microcapsules, Design-Expert 13.0 and response surface methodology (RSM) were used. This design included 3 independent variables of maltodextrin level, BSG level and spray dryer inlet temperature. Finally, the best sample in encapsulation was examined by scanning electron microscope (SEM) and differential scanning calorimetry (DSC). The results showed that by increasing sound intensity, extraction efficiency, total phenol and antioxidant activity increased significantly (p ≤ 0.01). The highest factors were observed in the sample extracted by enzyme and ultrasound at 90% sound intensity for 40 minutes (p ≤ 0.01). In second phase, increasing the inlet temperature of the dryer and the level of maltodextrin as a carrier reduced the encapsulation efficiency and the DPPH radical scavenging activity of the capsules non-linearly. The optimum conditions included 12.129% maltodextrin, 0.5% BSG and the inlet temperature of the dryer of 177.22 °C. The results of DSC showed that the formation of complexes between the compounds led to the formation of heat-stable capsules. The average size of the particles was 1.04 micrometers. According to the results of SEM, the microcapsules had an irregular and quasi-spherical shape. At all the pH and temperatures, the microencapsulated sample had higher stability (p ≤ 0.05). Over time, the bioavailability and release of phenolic compounds increased significantly (p ≤ 0.05).


Main Subjects

Abdel-Aty, A. M., Barakat, A. Z., & Mohamed, S. A. (2023). Garden cress gum and maltodextrin as microencapsulation coats for entrapment of garden cress phenolic-rich extract: Improved thermal stability, storage stability, antioxidant and antibacterial activities. Food Science & Biotechnology, 32, 47-58.
Acosta-Estrada, B. A., Villela-Castrejón, J., Perez-Carrillo, E., Gómez-Sánchez, C. E., & Gutiérrez-Uribe, J. A. (2019). Effects of solid-state fungi fermentation on phenolic content, antioxidant properties and fiber composition of lime cooked maize by-product (nejayote). Journal of Cereal Science90, 102-127.‏
Aguiar, J., Costa, R., Rocha, F., Estevinho, B. N., & Santos, L. (2017). Design of microparticles containing natural antioxidants: Preparation, characterization and controlled release studies. Powder technology, 313, 287-292.
Arabshahi-D, S., Devi, D. V., & Urooj, A. (2007). Evaluation of antioxidant activity of some plant extracts and their heat, pH and storage stability. Food Chemistry100, 1100-1105.
Balasubramaniam, V. G., Ayyappan, P., Sathvika, S., & Antony, U. (2019). Effect of enzyme pretreatment in the ultrasound assisted extraction of finger millet polyphenols. Journal of Food Science and Technology56, 1583-1594.‏
Bayram, Y., Ozkan, K., & Sagdic, O. (2023). Valorization of viticulture waste as verjuice powders: their characterization, storage stability and application in beverage formulation. European Food Research & Technology, 1-14.
Capanoglu, E., De Vos, R. C., Hall, R. D., Boyacioglu, D., & Beekwilder, J. (2013). Changes in polyphenol content during production of grape juice concentrate. Food Chemistry139, 521-526.
Castilla, P., Echarri, R., Dávalos, A., Cerrato, F., Ortega, H., Teruel, J. L & Lasunción, M. A. (2006). Concentrated red grape juice exerts antioxidant, hypolipidemic, and antiinflammatory effects in both hemodialysis patients and healthy subjects. The American Journal of Clinical Nutrition84, 252-262.
Carneiro, H. C., Tonon, R. V., Grosso, C. R., & Hubinger, M. D. (2013). Encapsulation efficiency and oxidative stability of flaxseed oil microencapsulated by spray drying using different combinations of wall materials. Journal of Food Engineering, 115, 443-451. 
Charpashlo, E., Ghorani, B., & Mohebbi, M. (2021). Multilayered electrospinning strategy for increasing the bioaccessibility of lycopene in gelatin-based sub-micron fiber structures. Food Hydrocollid113, 106-121.
Dehghan Thanha, Rahela, Mahdian, Elham, Amini Fard, Mohammad Hossein, Bayat, Hassan, & Garajian, Reza. (2018). Optimizing the extraction conditions of red pepper phenolic compounds using ultrasound waves using the response surface method. Journal of Research & Innovation in Food Science & Technology, 11, 87-97.
Domínguez, R., Pateiro, M., Munekata, P. E., McClements, D. J., & Lorenzo, J. M. (2021). Encapsulation of bioactive phytochemicals in plant-based matrices and application as additives in meat and meat products. Molecules26, 3984.‏ 
Estevinho, B. N., & Rocha, F. (2020, June). Development of Food–Grade Controlled Delivery Systems by Microencapsulation of Polyphenols with Health Benefits. In Central European Congress on Food (pp. 495-510). Cham: Springer International Publishing.
Ersus, S., & Yurdagel, U. (2007). Microencapsulation of anthocyanin pigments of black carrot (Daucus carota L.) by spray drier. Journal of food engineering, 80(3), 805-812.
FAO, (2011). Global food losses and food waste – Extent, causes and prevention. (accessed 6.2.2017).
Fontana, A. R., Antoniolli, A., & Bottini, R. (2013). Grape pomace as a sustainable source of bioactive compounds: Extraction, characterization, and biotechnological applications of phenolics. Journal of agricultural and food chemistry61, 8987-9003.‏
Fernando, C. D., & Soysa, P. (2015). Extraction Kinetics of phytochemicals and antioxidant activity during black tea (Camellia sinensis L.) brewing. Nutrition journal, 14, 1-7.
Guler, A., Tokuşoğlu, Ö., & Artik, N. (2018). Alterations on phenolic compounds and antioxidant activity during sour grape juice concentrate processing. Ciência e Técnica Vitivinícola33, 32-49.
Gómez, B., Barba, F. J., Domínguez, R., Putnik, P., Kovačević, D. B., Pateiro, M., & Lorenzo, J. M. (2018). Microencapsulation of antioxidant compounds through innovative technologies and its specific application in meat processing. Trends in Food Science & Technology82, 135-147.‏
Gençdağ, E., Görgüç, A., Anakiz, S., & Yilmaz, F. M. (2023). Processing of verjuice by ultrasound-assisted microwave heating: An assessment on the enzyme activity retention, technological parameters, and bioactive properties. Food Science & Technology International, 10820132231176580.
Karapinar, M., & Sengun, I. Y. (2007). Antimicrobial effect of koruk (unripe grape - Vitis vinifera) juice against Salmonella typhimurium on salad vegetables. Food Control, 18, 702-706.
López de Dicastillo, C., López‐Carballo, G., Gavara, R., Muriel Galet, V., Guarda, A., & Galotto, M. J. (2019). Improving polyphenolic thermal stability of Aristotelia Chilensis fruit extract by encapsulation within electrospun cyclodextrin capsules. Journal of Food Processing & Preservation43, 14-24.‏
Lv, L., Wei, L., Chen, D., Liu, J., Lin, S., Ye, H., & Yuan, Y. (2015). Optimization of ultrasound-assisted extraction of polyphenols from maize filaments by response surface methodology and its identification. Journal of Applied Botany & Food Quality, 88(1).
Martino, E., Ramaiola, I., & Urbano, M. (2006). Microwave-assisted extraction of coumarin and related compounds from Melilotus officinalis (L.) Pallas alternative to soxhlet and ultrasound-assisted extraction. Journal of Chromatography A, 1125, 147 -151.
Maran, J. P., Manikandan, S., Nivetha, C. V., & Dinesh, R. (2017). Ultrasound assisted extraction of bioactive compounds from Nephelium lappaceum L. fruit peel using central composite face centered response surface design. Arabian Journal of Chemistry,  10, 45-57.
Mirabella, N., Castellani, V., & Sala, S. (2014). Current options for the valorization of food manufacturing waste: a review. Journal of Cleaner Production65, 28-41.
Mattivi, F., Guzzon, R., Vrhovsek, U., Stefanini, M., & Velasco, R. (2006). Metabolite profiling of grape: Flavonols and anthocyanins. Journal of Agricultural & Food Chemistry54, 7692-7702.‏
Nikfardjam, M. S. P. (2008). General and polyphenolic composition of unripe grape juice (verjus/verjuice) from various producers. Mitteilungen Klosterneuburg, 58, 28- 31.
Öncül, N., & Karabiyikli, Ş. (2015). Factors affecting the quality attributes of unripe grape functional food products. Journal of Food Biochemistry, 39(6), 689-695.
Oszmiański, J., Wojdyło, A., & Kolniak, J. (2011). Effect of pectinase treatment on extraction of antioxidant phenols from pomace, for the production of puree-enriched cloudy apple juices. Food Chemistry127, 623-631.
Ordoñez A AL, Gomez J D, Vattuone M A, lsla M I. (2006). Antioxidant activities of sechium edule (Jacq) Swartz extracts. Food Chemistry, 97, 452-458.
Puri, S., Singh, S., & Sohal, S. K. (2022). Oviposition behaviour and biochemical response of an insect pest, Zeugodacus cucurbitae (Coquillett)(Diptera: Tephritidae) to plant phenolic compound phloroglucinol. Comparative Biochemistry and Physiology Part C: Toxicology & Pharmacology, 255, 109291.
‏ Phan, L. H. N., Nguyen, T. N. T., & Le, V. V. M. (2012). Ultrasonic treatment of mulberry (Morus alba) mash in the production of juice with high antioxidant level. Journal of Science & Technology50, 204-209.
Ricci, A., Mejia, J. A. A., Versari, A., Chiarello, E., Bordoni, A., & Parpinello, G. P. (2022). Microencapsulation of polyphenolic compounds recovered from red wine lees: Process optimization and nutraceutical study. Food & Bioproducts Processing132, 1-12.
Rehman, A., Ahmad, T., Aadil, R. M., Spotti, M. J., Bakry, A. M., Khan, I. M., & Tong, Q. (2019). Pectin polymers as wall materials for the nano-encapsulation of bioactive compounds. Trends in Food Science & Technology90, 35-46.
Salvia-Trujillo, L., & McClements, D. J. (2016). Enhancement of lycopene bioaccessibility from tomato juice using excipient emulsions: Influence of lipid droplet size. Food Chemistry210, 295-304.
Shishir, M. R. I., Xie, L., Sun, C., Zheng, X., & Chen, W. (2018). Advances in micro and nano-encapsulation of bioactive compounds using biopolymer and lipid-based transporters. Trends in Food Science & Technology78, 34-60.‏
SEl, G., Ella, F. M. A., Emad, M. H., Shalaby, E., & Doha, H. (2014). Antioxidant activity of phenolic compounds from different grape wastes. International Journal of Food Processing Technology5, 29- 42.‏
Tomé-Carneiro, J., & Visioli, F. (2016). Polyphenol-based nutraceuticals for the prevention and treatment of cardiovascular disease: Review of human evidence. Phytomedicine, 23(11), 1145-1174.
‏Turkmen, F. U., Takci, H. A. M., & Sekeroglu, N. (2017). Total phenolic and flavonoid contents, antioxidant and antimicrobial activities of traditional unripe grape products. Indian Journal of Pharmaceutical Education & Research51, 489-493.‏
Wootton-Beard, P. C., Moran, A., & Ryan, L. (2011). Stability of the total antioxidant capacity and total polyphenol content of 23 commercially available vegetable juices before and after in vitro digestion measured by FRAP, DPPH, ABTS and Folin–Ciocalteu methods. Food Research International44, 217-224.‏
Wijesinghe, W. A. J. P., & Jeon, Y. J. (2012). Enzyme-assistant extraction (EAE) of bioactive components: a useful approach for recovery of industrially important metabolites from seaweeds: a review. Fitoterapia, 83(1), 6-12.
Wei, M., Ma, T., Cao, M., Wei, B., Li, C., Li, C., & Sun, X. (2022). Biomass estimation and characterization of the nutrient components of thinned unripe grapes in China and the global grape industries. Food Chemistry, 15, 100-123.
Xia, E. Q., Deng, G. F., Guo, Y. J., & Li, H. B. (2010). Biological activities of polyphenols from grapes. International Journal of Molecular Sciences11, 622-646.‏
Salvia-Trujillo, L., & McClements, D. J. (2016). Enhancement of lycopene bioaccessibility from tomato juice using excipient emulsions: Influence of lipid droplet size. Food Chemistry, 210, 295-304.
Zhang, R., Zhang, Z., Zou, L., Xiao, H., Zhang, G., Decker, E. A., & McClements, D. J. (2016). Enhancement of carotenoid bioaccessibility from carrots using excipient emulsions: Influence of particle size of digestible lipid droplets. Food & Function, 7(1), 93-103.