Enhanced structural properties of calcium cross-linked pectin gel beads incorporated with starch derivatives: Preparation, characterization, and in vitro prebiotic activity - 2025
Enhanced structural properties of calcium cross-linked pectin gel beads incorporated with starch derivatives: Preparation, characterization, and in vitro prebiotic activity
starch derivatives; gel beads; structural analysis; physicochemical properties; in vitro prebiotic activity
Abstract :
[en] In this study, gel beads composed of pectin and four different starch-based derivatives were prepared through calcium ion crosslinking, and their physicochemical characteristics and functional properties were systematically evaluated. The results indicated that the incorporation of starch derivatives increased the internal crosslinking degree and strengthened intermolecular interactions, leading to a more compact and densely arranged porous structure within the composite gel beads. Compared to pure pectin gel beads, the water holding capacity of the composite gel beads improved by 6.06%–15.44% while the swelling rate decreased by 26.16%–37.02%, and the hardness, springiness, chewiness, and gumminess increased by 4.16%–12.75%, 3.40%–4.96%, 1.71%–8.63%, and 8.09%–16.51%, respectively. Additionally, the incorporation of starch derivatives reduced the crystallinity of the composite gel beads and enhanced their thermal stability. Moreover, all five gel beads exhibited notable prebiotic activity, significantly promoting the growth of Lactiplantibacillus plantarum Lp3a. Notably, the gel beads incorporating starch-curcumin complexes (TS-CUR@GB) achieved the highest colony count of 2.15×109 CFU/mL, which was 2.92-fold higher than the blank group. These results demonstrate the potential of starch-based derivatives to improve the structural integrity and functional performance of pectin-based gel systems, offering promising applications in food science and bioactive delivery systems.
Disciplines :
Agriculture & agronomy Chemistry
Author, co-author :
Zhu, Wenqing ; Université de Liège - ULiège > TERRA Research Centre ; College of Food Science and Engineering, Key Laboratory of Food Nutrition and Health in Universities of Shandong, Shandong Agricultural University, Tai'an, Shandong, China
Bai, Ruoxi; College of Food Science and Engineering, Key Laboratory of Food Nutrition and Health in Universities of Shandong, Shandong Agricultural University, Tai'an, Shandong, China
Liang, Shulei; College of Food Science and Engineering, Key Laboratory of Food Nutrition and Health in Universities of Shandong, Shandong Agricultural University, Tai'an, Shandong, China
Yuan, Yuqin; College of Food Science and Engineering, Key Laboratory of Food Nutrition and Health in Universities of Shandong, Shandong Agricultural University, Tai'an, Shandong, China
Zhang, Bin; College of Food Science and Engineering, Key Laboratory of Food Nutrition and Health in Universities of Shandong, Shandong Agricultural University, Tai'an, Shandong, China
Fauconnier, Marie-Laure ; Université de Liège - ULiège > Département GxABT > Chemistry for Sustainable Food and Environmental Systems (CSFES)
Richel, Aurore ; Université de Liège - ULiège > TERRA Research Centre > Chemistry for Sustainable Food and Environmental Systems (CSFES)
Zheng, Zhenjia ; College of Food Science and Engineering, Key Laboratory of Food Nutrition and Health in Universities of Shandong, Shandong Agricultural University, Tai'an, Shandong, China
Language :
English
Title :
Enhanced structural properties of calcium cross-linked pectin gel beads incorporated with starch derivatives: Preparation, characterization, and in vitro prebiotic activity
Almeida, S.F., Silva, G.K.C., Toledo, M.N.A., Sato, A.C.K., Modulating porosity and mechanical properties of pectin hydrogels by starch addition. Journal of Food Science and Technology 58 (2021), 302–310, 10.1007/s13197-020-04543-x.
Bhola, J., Bhadekar, R., Prebiotic effect of daily dietary polyphenols and oligosaccharides on lactobacillus species. Bioactive Carbohydrates Dietary Fibre, 31, 2024, 100407, 10.1016/j.bcdf.2024.100407.
Bu, Q.Y., Chen, Y., Ding, Y., Zhang, K.X., Li, Y.C., You, X.Y., Zhao, G.P., Preparation and characterization of tea polyphenol composite microspheres encapsulated using sodium alginate and crosslinked starch. LWT--Food Science and Technology, 184, 2023, 114888, 10.1016/j.lwt.2023.114888.
Bu, K.X., Huang, D.J., Li, D.P., Zhu, C.H., Encapsulation and sustained release of curcumin by hawthorn pectin and Tenebrio Molitor protein composite hydrogel. International Journal of Biological Macromolecules 222 (2022), 251–261, 10.1016/j.ijbiomac.2022.09.145.
Bušić, A., Belščak-Cvitanović, A., Cebin, A.V., Karlović, S., Kovač, V., Igor, Š., Mršić, G., Komes, D., Structuring new alginate network aimed for delivery of dandelion (Taraxacum officinale L.) polyphenols using ionic gelation and new filler materials. Food Research International 111 (2018), 244–255, 10.1016/j.foodres.2018.05.034.
Cai, R., Pan, S.Y., Li, R.X., Xu, X.Y., Pan, S.Y., Liu, F.X., Curcumin loading and colon release of pectin gel beads: Effect of different de-esterification method. Food Chemistry, 389, 2022, 133130, 10.1016/j.foodchem.2022.133130.
Chan, E.S., Wong, S.L., Lee, P.P., Lee, J.S., Ti, T.B., Zhang, Z.B., Poncelet, D., Ravindra, P., Phan, S.H., Yim, Z.H., Effects of starch filler on the physical properties of lyophilized calcium-alginate beads and the viability of encapsulated cells. Carbohydrate Polymers 83 (2011), 225–232, 10.1016/j.carbpol.2010.07.044.
Chen, L., Tong, Q.Y., Ren, F., Zhu, G.L., Pasting and rheological properties of rice starch as affected by pullulan. International Journal of Biological Macromolecules 66 (2014), 325–331, 10.1016/j.ijbiomac.2014.02.052.
Cortés-Camargo, S., Román-Guerrero, A., Alvarez-Ramirez, J., Alpizar-Reyes, E., Velázquez-Gutiérrez, S.K., Pérez-Alonso, C., Microstructural influence on physical properties and release profiles of sesame oil encapsulated into sodium alginate-tamarind mucilage hydrogel beads. Carbohydrate Polymer Technologies and Applications, 5, 2023, 100302, 10.1016/j.carpta.2023.100302.
Dahal, P., Janaswamy, S., Hydrocolloid-based nutraceutical delivery systems: Potential of κ-carrageenan hydrogel beads for sustained release of curcumin. Food Research International, 183, 2024, 114223, 10.1016/j.foodres.2024.114223.
Dumitriu, R.P., Mitchell, G.R., Vasile, C., Rheological and thermal behaviour of poly (N-isopropylacrylamide)/alginate smart polymeric networks. Polymer International 60 (2011), 1398–1407, 10.1002/pi.3093.
Feltrea, G., Almeidaa, F.S., Satoa, A.C.K., Dacanalb, G.C., Hubinger, M.D., Alginate and corn starch mixed gels: Effect of gelatinization and amylose content on the properties and in vitro digestibility. Food Research International, 132, 2020, 109069, 10.1016/j.foodres.2020.109069.
Günter, E.A., Martynov, V.V., Ananchenko, B.A., Martinson, E.A., Litvinets, S.G., The gel strength and swelling in the gastrointestinal environment of pectin/κ-carrageenan gel particles based on pectins with different degrees of methylesterification. Materials Today Communications, 33, 2022, 104986, 10.1016/j.mtcomm.2022.104986.
Han, X.Y., Ma, P., Shen, M.Y., Wen, H.L., Xie, J.H., Modified porous starches loading curcumin and improving the free radical scavenging ability and release properties of curcumin. Food Research International, 168, 2023, 112770, 10.1016/j.foodres.2023.112770.
Hu, M., Du, X.Q., Liu, G.N., Huang, Y.Y., Qi, B.K., Li, Y., Sodium alginate/soybean protein-epigallocatechin-3-gallate conjugate hydrogel beads: Evaluation of structural, physical, and functional properties. Food & Function 12:24 (2021), 12347–12361, 10.1039/d1fo03099j.
Jiang, X., Gu, Y., Zhang, L., Sun, J., Yan, J., Wang, C., Physicochemical properties of granular and gelatinized lotus rhizome starch with varied proximate compositions and structural characteristics. Foods, 12(23), 2023, 4330, 10.3390/foods12234330.
Jiang, B., Li, W., Hu, X., Wu, J., Shen, Q., Rheology of mung bean starch treated by high hydrostatic pressure. International Journal of Food Properties 18 (2015), 81–92, 10.1080/10942912.2013.819363.
Jiang, X.Y., Li, L., Yan, J.N., Zhang, L.C., Wang, C., Lai, B., Wu, H.T., Characterization of hydrogel beads constructed from gelatinized lotus rhizome starch and sodium alginate by calcium cross-linking. Food Hydrocolloids, 154, 2024, 110102, 10.1016/j.foodhyd.2024.110102.
Lee, T., Chang, Y.H., Structural, physicochemical, and in-vitro release properties of hydrogel beads produced by oligochitosan and de-esterified pectin from yuzu (Citrus junos) peel as a quercetin delivery system for colon target. Food Hydrocolloids, 108, 2020, 106086, 10.1016/j.foodhyd.2020.106086.
Lee, Y.E., Kang, Y.R., Chang, Y.H., Effect of pectic oligosaccharide on probiotic survival and physicochemical properties of hydrogel beads for synbiotic encapsulation of Lactobacillus bulgaricus. Food Bioscience, 51, 2023, 102260, 10.1016/j.fbio.2022.102260.
Lenie, M.D.R., Ahmadzadeh, S., Bockstaele, F.V., Ubeyitogullari, A., Development of a pH-responsive system based on starch and alginate-pectin hydrogels using coaxial 3D food printing. Food Hydrocolloids, 153, 2024, 109989, 10.1016/j.foodhyd.2024.109989.
Li, Q., Duan, M.R., Hou, D., Chen, X.Q., Shi, J.L., Zhou, W., Fabrication and characterization of Ca (II)-alginate-based beads combined with different polysaccharides as vehicles for delivery, release and storage of tea polyphenols. Food Hydrocolloids, 112, 2021, 106274, 10.1016/j.foodhyd.2020.106274.
Li, H., Gao, Z.X., Xu, J.J., Sun, W., Wu, J.R., Zhu, L., Gao, M.J., Zhan, X.B., Encapsulation of polyphenols in pH-responsive micelles self-assembled from octenyl-succinylated curdlan oligosaccharide and its effect on the gut microbiota. Colloids and Surfaces B: Biointerfaces, 219, 2022, 112857, 10.1016/j.colsurfb.2022.112857.
Li, Z.X., Geng, Y.X., Bu, K.X., Chen, Z.T., Xu, K., Zhu, C.H., Construction of a pectin/sodium alginate composite hydrogel delivery system for improving the bioaccessibility of phycocyanin. International Journal of Biological Macromolecules, 269, 2024, 131969, 10.1016/j.ijbiomac.2024.131969.
Li, Y.H., Zhang, C., Li, S.Y., Zhu, Z.Z., Wang, X.H., Cravotto, G., Improving complexation of puerarin with kudzu starch by various ultrasonic pretreatment: Interaction mechanism analysis. Ultrasonics Sonochemistry, 111, 2024, 107095, 10.1016/j.ultsonch.2024.107095.
Lin, S.Y., Liu, X.E., Cao, Y., Liu, S.C., Deng, D.W., Zhang, J.S., Huang, G.H., Effects of xanthan and konjac gums on pasting, rheology, microstructure, crystallinity and in vitro digestibility of mung bean resistant starch. Food Chemistry, 339, 2021, 128001, 10.1016/j.foodchem.2020.128001.
Liu, R., Ci, X.M., Liu, L.L., Wang, X.T., Rifky, M., Liu, R., Sui, W.J., Wu, T., Zhang, M., Chitosan entrapping of sodium alginate/Lycium barbarum polysaccharide gels for the encapsulation, protection and delivery of Lactiplantibacillus plantarum with enhanced viability. International Journal of Biological Macromolecules, 260, 2024, 129615, 10.1016/j.ijbiomac.2024.129615.
Lopes, M.M., Oliveira-Paiva, C.A., Farinas, C.S., Modification of pectin/starch-based beads with additives to improve Bacillus subtilis encapsulation for agricultural applications. International Journal of Biological Macromolecules, 246, 2023, 125646, 10.1016/j.ijbiomac.2023.125646.
Lozano-Vazquez, G., Lobato-Calleros, C., Escalona-Buendia, H., Chavez, G., Alvarez-Ramirez, J., Vernon-Carter, E.J., Effect of the weight ratio of alginate-modified tapioca starch on the physicochemical properties and release kinetics of chlorogenic acid containing beads. Food Hydrocolloids 48 (2015), 301–311, 10.1016/j.foodhyd.2015.02.032.
Paswan, M., Chandel, A.K.S., Malek, N.I., Dholakiya, B.Z., Preparation of sodium alginate/Cur-PLA hydrogel beads for curcumin encapsulation. International Journal of Biological Macromolecules, 254, 2024, 128005, 10.1016/j.ijbiomac.2023.128005.
Qi, X.X., Simsek, S., Chen, B.C., Alginate-based double-network hydrogel improves the viability of encapsulated probiotics during simulated sequential gastrointestinal digestion: Effect of biopolymer type and concentrations. International Journal of Biological Macromolecules 165 (2020), 1675–1685, 10.1016/j.ijbiomac.2020.10.028.
Qiu, Z.C., Li, L.Y., Zhu, W.Q., Qiao, X.G., Zheng, Z.J., Sun-Waterhouse, D.X., Pectins rich in RG-I and galactose extracted from garlic pomace: Physicochemical, structural, emulsifying and antioxidant properties. Food Hydrocolloids, 149, 2024, 109559, 10.1016/j.foodhyd.2023.109559.
Raza, H., Zhou, Q., Cheng, K.W., He, J.Y., Wang, M.F., Synergistic impact of ultrasound-high pressure homogenization on the formation, structural properties, and slow digestion of the starch-phenolic acid complex. Food Chemistry, 445, 2024, 138785, 10.1016/j.foodchem.2024.138785.
Razavi, S., Janfaza, S., Tasnim, N., Gibson, D.L., Hoorfar, M., Microencapsulating polymers for probiotics delivery systems: Preparation, characterization, and applications. Food Hydrocolloids, 120, 2021, 106882, 10.1016/j.foodhyd.2021.106882.
Reichembach, L.H., Petkowicz, C.L.O., Guerrero, P., Caba, K., Pectin and pectin/chitosan hydrogel beads as coffee essential oils carrier systems. Food Hydrocolloids, 151, 2024, 109814, 10.1016/j.foodhyd.2024.109814.
Ren, Y.M., Jiang, L., Wang, W.J., Xiao, Y.H., Liu, S.C., Luo, Y., Shen, M.Y., Xie, J.H., Effects of Mesona chinensis Benth polysaccharide on physicochemical and rheological properties of sweet potato starch and its interactions. Food Hydrocolloids, 99, 2020, 105371, 10.1016/j.foodhyd.2019.105371.
Rohman, S., Kaewtatip, K., Kantachote, D., Tantirungkij, M., Encapsulation of Rhodopseudomonas palustris KTSSR54 using beads from alginate/starch blends. Journal of Applied Polymer Science, 138, 2021, 50084, 10.1002/app.50084.
Sarkar, S., Manna, S., Das, E., Jana, P., Mukherjee, S., Sahu, R., Dua, T.K., Paul, P., Kaity, S., Nandi, G., Fabrication and optimization of extended-release beads of diclofenac sodium based on Ca2+ cross-linked Taro (Colocasia esculenta) stolon polysaccharide and pectin by quality-by-design approach. International Journal of Biological Macromolecules, 271, 2024, 132606, 10.1016/j.ijbiomac.2024.132606.
Silveira, M.P., Almeida, F.L.C., Andreola, K., Alvim, I.D., Prata, A.S., Influence of composition on the internal diffusion mechanism of pectin-starch gel beads. Journal of Applied Polymer Science, 140(9), 2023, E53570, 10.1002/app.53570.
Singh, P., Medronho, B., Alves, L., Silva, G.J., Miguel, M.G., Lindman, B., Development of carboxymethyl cellulose-chitosan hybrid micro- and macroparticles for encapsulation of probiotic bacteria. Carbohydrate Polymers 175 (2017), 87–95, 10.1016/j.carbpol.2017.06.119.
Su, C.Y., Xia, T., Li, D., Wang, L.J., Wang, Y., Hybrid biodegradable materials from starch and hydrocolloid: Fabrication, properties and applications of starch-hydrocolloid film, gel and bead. Critical Reviews in Food Science and Nutrition 64:33 (2023), 12841–12859, 10.1080/10408398.2023.2257786.
Sun, W.X., Bu, K.X., Meng, H.M., Zhu, C.H., Hawthorn pectin/soybean isolate protein hydrogel bead as a promising ferrous ion-embedded delivery system. Colloids and Surfaces B: Biointerfaces, 237, 2024, 113867, 10.1016/j.colsurfb.2024.113867.
Ubeyitogullari, A., Ciftci, O.N., Formation of nanoporous aerogels from wheat starch. Carbohydrate Polymers 147 (2016), 125–132, 10.1016/j.carbpol.2016.03.086.
Ubeyitogullari, A., Ciftci, O.N., A novel and green nanoparticle formation approach to forming low-crystallinity curcumin nanoparticles to improve curcumin's bioaccessibility. Scientific Reports, 9, 2019, 19112, 10.1038/s41598-019-55619-4.
Vaziri, A.S., Alemzadeh, I., Vossoughi, M., Khorasani, A.C., Co-microencapsulation of Lactobacillus plantarum and DHA fatty acid in alginate-pectin-gelatin biocomposites. Carbohydrate Polymers 199 (2018), 266–275, 10.1016/j.carbpol.2018.07.002.
Wan, L., Yang, Z.X., Cai, R., Pan, S.Y., Liu, F.X., Pan, S.Y., Calcium-induced-gel properties for low methoxyl pectin in the presence of different sugar alcohols. Food Hydrocolloids, 112, 2021, 106252, 10.1016/j.foodhyd.2020.106252.
Wang, X.W., Feng, Y.W., Feng, T.T., Modulation effect of glycerol on plasticization and water distribution of vacuum-dried calcium alginate gel beads encapsulating peppermint oil/β-cyclodextrin complex. Food Bioscience, 41, 2021, 100968, 10.1016/j.fbio.2021.100968.
Wang, W.J., Shen, M.Y., Liu, S.C., Jiang, L., Song, Q.Q., Xie, J.H., Gel properties and interactions of Mesona blumes polysaccharide-soy protein isolates mixed gel: The effect of salt addition. Carbohydrate Polymers 192 (2018), 193–201, 10.1016/j.carbpol.2018.03.064.
Wang, S.J., Wu, Z.N., Jia, L.Y., Wang, X.H., He, T., Wang, L., Yao, G.J., Xie, F.Y., Soybean protein isolate-sodium alginate double network emulsion gels: Mechanism of formation and improved freeze-thaw stability. International Journal of Biological Macromolecules, 274, 2024, 133296, 10.1016/j.ijbiomac.2024.133296.
Xiao, W.H., Shen, M.Y., Li, J.W., Li, Y.L., Qi, X., Rong, L.Y., Liu, W.M., Xie, J.H., Preparation and characterization of curcumin-loaded debranched starch/Mesona chinensis polysaccharide microcapsules: Loading levels and in vitro release. Food Hydrocolloids, 141, 2023, 108697, 10.1016/j.foodhyd.2023.108697.
Xiao, W.H., Shen, M.Y., Ren, Y.M., Wen, H.L., Li, J.W., Rong, L.Y., Liu, W.M., Xie, J.H., Controlling the pasting, rheological, gel, and structural properties of corn starch by incorporation of debranched waxy corn starch. Food Hydrocolloids, 123, 2022, 107136, 10.1016/j.foodhyd.2021.107136.
Yang, J.Y., Song, J.L., Miao, S., Gao, Y.X., Mao, L.K., Alginate-based gel beads with bigel structures: Preparation, characterization and bioactive encapsulation. Food Hydrocolloids, 146, 2024, 109294, 10.1016/j.foodhyd.2023.109294.
Ye, J.P., Yang, R., Liu, C.M., Luo, S.J., Chen, J., Hu, X.T., Wu, J.Y., Improvement in freeze-thaw stability of rice starch gel by inulin and its mechanism. Food Chemistry 268 (2018), 324–333, 10.1016/j.foodchem.2018.06.086.
Zhang, Y., Zhao, X.T., Bao, X.Y., Xiao, J., Liu, H.S., Effects of pectin and heat-moisture treatment on structural characteristics and physicochemical properties of corn starch. Food Hydrocolloids, 117, 2021, 106664, 10.1016/j.foodhyd.2021.106664.
Zhang, Y., Zhao, T., Ma, X.R., Innovative modified pectins enriched with galactose: Preparation, characterization, and gel-based properties of curcumin-delivered hydrogel beads. Food Hydrocolloids, 160, 2025, 110757, 10.1016/j.foodhyd.2024.110757 2025.
Zhang, F., Zheng, X.J., Ma, Y., Nan, W.Q., Wu, W.J., Chu, Z.R., Sun, X., Huang, J.H., Muratkhan, M., Yue, F.F., Wang, X., Lv, X., Sodium alginate/low methoxyl pectin composite hydrogel beads prepared via gas-shearing technology for enhancing the colon-targeted delivery of probiotics and modulating gut microbiota. International Journal of Biological Macromolecules, 300, 2025, 140375, 10.1016/j.ijbiomac.2025.140375.
Zhu, W.Q., Bai, X.Y., Du, W.B., Li, L.Y., Fauconnier, M.L., Richel, A., Dong, H.J., Zheng, Z.J., Comparison of the properties of turmeric starch-dioscin-curcumin nanocarriers prepared by antisolvent co-precipitation and antisolvent precipitation. Carbohydrate Polymers, 353, 2025, 123263, 10.1016/j.carbpol.2025.123263.
