Evaluation of physicochemical and functional properties of corn resistant starch prepared by autoclaving method

Document Type : Research Article


1 PhD Student, Department of Food Science and Technology, Ferdowsi University of Mashhad, Mashhad, Iran.

2 Professor, Department of Food Science and Technology, Ferdowsi University of Mashhad, Mashhad, Iran

3 Assistant Professor, Iranian Academic Center for Education Culture and Research (ACECR), Mashhad, Iran


Resistant starch (RS) is part of starch, which remains unchanged and not digested after 120 minutes of incubation against digestive enzymes such as α-amylase. Among the various types of resistant starch, resistant starch type 3 has been given more attention due to its thermal stability during the heat treatment process of foods. In order to produce resistant starch type 3, the granular structure of starch should be destroyed by heating in the presence of sufficient water, followed by amylose chains re-association upon cooling. Autoclaving of starch-based products leads to retrogradation and, as a result, increases the amount of resistant starch. The purpose of this study was to investigate the effect of various autoclaving temperatures (108, 121 and 134°C) and autoclave-cooling cycles (1 to 3 cycles) on the formation of resistant starch and its physicochemical and functional properties. The results showed that with increasing the autoclaving temperature as well as temperature cycles, the amount of resistant starch formation increased. The solubility of produced resistant starch was significantly higher than natural corn starch, while it did not change in term of apparent amylose. Also, the autoclaving-retrogradation process led to changes in starch crystalline type from A to B and V, and the degree of starch crystallinity also increased. Scanning electron micrographs showed significant changes in starch granules and formation of a sponge like texture which was due to the autoclaving process. Also, all textural properties (hardness, cohesiveness, springiness and gumminess) of resistant starch were reduced compared to natural corn starch.

Graphical Abstract

Evaluation of physicochemical and functional properties of corn resistant starch prepared by autoclaving method


  • The effect of autoclave temperature and heating cycles on the formation of resistant starch from native maize starch was investigated.
  • Increasing the autoclave temperature and heating cycles increased the amount of resistant starch.
  • The autoclave process led to crystalline structure change of corn starch from type A to B and V.
  • Textural properties of the gel obtained from resistant starch were reduced compared to native starch.


Main Subjects

[1] Berry, C. (1986). Resistant starch: formation and measurement of starch that survives exhaustive digestion with amylolytic enzymes during the determination of dietary fibre. J. Cereal Sci., 4, 301-14.
[2] Sajilata, M. G., Singhal, R. S., Kulkarni, P.R. (2006). Resistant Starch–A Review. Compr Rev Food Sci F., 5, 1-17.
[3] Douglas, L.C., Sanders, M.E. (2008). Probiotics and prebiotics in dietetics practice. J Am Diet Assoc., 3, 108-510.
[4] Wepner, B., Berghofer, E., Miesenberger, E., Tiefenbacher, K. (1999). Citrate starch: Application as resistant starch in different food systems. Starch/Stärke., 51, 354-361.
[5] Kim, S.K., Kwak, J.E. (2004). Estimation of resistant starch content of high-amylose corn starch. Food Sci. Biotechnol., 13, 71–74.
[6] Haralampu, S.G. (2000). Resistant starch—a review of the physical properties and biological impact of RS3. Carbohydr. Polym., 41, 285-292.
[7] Eerlingen, R.C., Delcour, J.A. (1995). Formation, analysis, structure and properties of type III enzyme resistant starch. J Cereal Sci., 22, 129–138.
[8] Augustin, M.A., Sanguansri, P., Htoon, A. (2008). Functional performance of a resistant starch ingredient modified using a microfluidiser. Innov Food Sci Emerg Technol., 9, 224-231.
[9] Lertwanawatana, P., Frazier, R.A., Niranjan, K. (2015). High pressure intensification of cassava resistant starch (RS3) yields. Food Chem., 181, 85–93.
[10] Sievert, D., Pomeranz, Y. (1989). Enzyme-resistant starch. I. Characterization and evaluation by enzymatic, thermoanalytical, and microscopic methods. Cereal Chem., 66, 342-347.
[11] Szczodrak, J., Pomeranz, Y. (1991). Starch and enzyme-resistant starch from high-amylose barley. Cereal Chem., 68, 589-596.
[12] Dundar, A.N., Gocmen, D. (2013). Effects of autoclaving temperature and storing time on resistant starch formation and its functional and physicochemical properties. Carbohydr Polym., 97, 764-771.
[13] Ozturk, S., Koksel, H., Perry, N.G. (2011). Production of resistant starch from acid-modified amylotype starches with enhanced functional properties. J. Food Eng., 103, 156-164.
[14] AOAC. (2000). Official Methods of Analysis Association of Official Analytical Chemists, 17th edn. In:Cunnif, P. (Ed.)., Arlington, VA, USA., pp 1-37.
 [15] ISO (Intrenational Organization for Standardization). (2007). ISO 6647: Norme internationale: Riz-détermination de la teneur em amylose. Geneva, Switzerland.
[16] Leach, H.W. (1959). Structure of starch granules. I. Swelling and solubility patterns of various starches. Cereal Chem., 36, 534-544.
 [17] Huang, M., Kennedy, J.F., Li, B., Xu, X., Xie, B.J. (2007). Characters of rice starch gel modified by gellan, carrageenan, and glucomannan: a texture profile analysis study. Carbohydr. Polym., 69, 411–418.
[18] Li, S., Ward, R., Gao, Q. (2011). Effect of heat-moisture treatment on the formation and physicochemical properties of resistant starch from mung bean (Phaseolus radiatus) starch. Food Hydrocoll., 25, 1702-1709.
[19] Milašinović, M.S., Radosavljević, M.M., Dokić, L.P. (2010). Effects of autoclaving and pullulanase debranching on the resistant starch yield of normal maize starch. J Serb Chem Soc., 75, 449-458.
[20] Onyango, C., Bley, T., Jacob, A., Henle, T., Rohm, H. (2006). Influence of incubation temperature and time on resistant starch type III formation from autoclaved and acid-hydrolysed cassava starch. Carbohydr. Polym., 66, 494-499.
[21] Aparicio‐Saguilán, A., Flores‐Huicochea, E., Tovar, J., García‐Suárez, F., Gutiérrez‐Meraz, F., Bello‐Pérez, L.A. (2005). Resistant Starch‐rich Powders Prepared by Autoclaving of Native and Lintnerized Banana Starch: Partial Characterization. StarchStärke, 57, 405-412.
[22] Zhao, X.H., Lin, Y. (2009). The impact of coupled acid or pullulanase debranching on the formation of resistant starch from maize starch with autoclaving–cooling cycles. Eur Food Res Technol., 230, 179-184.
[23] Gao, H., Cai, J., Han, W., Huai, H., Chen, Y., Wei, C. (2014). Comparison of starches isolated from three different Trapa species. Food Hydrocoll., 37, 174-181.
[24] Chinnaswamy, R., Hanna, M.A. (1988). Relationship between amylose content and extrusion-expansion properties of com starches. Cereal Chem., 65, 138-143.
[25] Seetharaman, K., Tziotis, A., Borras, F., White, P.J., Ferrer, M., Robutti, J. (2001). Thermal and functional characterization of starch from Argentinean corn. Cereal Chem., 78, 379-386.
[26] Ratnayake, W.S., Jackson, D.S. (2007). A new insight into the gelatinization process of native starches. Carbohydr. Polym., 67, 511-529.
[27] Wu, H.C.H., Sarko, A. (1978). The double-helical molecular structure of B-amylose. Carbohydr. Res., 61, 7-26
[28] Morris, V.J. (1990). Starch gelation and retrogradation. Trends Food Sci Tech., 1, 2-6.
[29] Adebowale, K.O., Lawal, O.S. (2002). Effect of annealing and heat moisture conditioning on the physicochemical characteristics of Bambarra groundnut (Voandzeia subterranea) starch. Mol Nutr Food Res., 46, 311-316.
[30] Köksel, H., Basman, A., Kahraman, K., Ozturk, S. (2007). Effect of acid modification and heat treatments on resistant starch formation and functional properties of corn starch. Int J Food Prop., 10, 691-702.
[31] Yu, S., Ma, Y., Menager, L., Sun, D.W. (2012). Physicochemical properties of starch and flour from different rice cultivars. Food Bioprocess Tech., 5, 626-637.
[32] Lawal, O.S. (2004). Composition, physicochemical properties and retrogradation characteristics of native, oxidised, acetylated and acid-thinned new cocoyam (Xanthosoma sagittifolium) starch. Food Chem., 87, 205-218.
[33] Zeng, S., Wu, X., Lin, S., Zeng, H., Lu, X., Zhang, Y., Zheng, B. (2015). Structural characteristics and physicochemical properties of lotus seed resistant starch prepared by different methods. Food Chem., 186, 213-222.
[34] Fannon, J.E., Hauber, R.J., BeMiller, J.N. (1992). Surface pores of starch granules. Cereal Chem., 69, 284-288.
[35] Stone, L.A., Lorenz, K. (1984). The Starch of Amaranthus—Physico‐chemical Properties and Functional Characteristics. StarchStärke., 36, 232-237.
[36] Singh, N., Kaur, L., Sandhu, K.S., Kaur, J., Nishinari, K. (2006). Relationships between physicochemical, morphological, thermal, rheological properties of rice starches. Food Hydrocoll., 20, 532-542.
[37] Szczesniak, A.S. (2002). Texture is a sensory property. Food Qual Prefer., 13, 215-225.
[38] Choi, S.G., Kerr, W.L. (2003). Effects of chemical modification of wheat starch on molecular mobility as studied by pulsed 1 H NMR. LWT - Food Sci Technol., 36, 105-112.
[39] Czechowska-Biskup, R., Rokita, B., Lotfy, S., Ulanski, P., Rosiak, J.M. (2005). Degradation of chitosan and starch by 360-kHz ultrasound. Carbohydr. Polym., 60, 175-184.
[40] Sanderson, G.R. (1990). Gellan gum, in: Harris, P. Food gels. Springer Netherlands, pp 201-232.
[41] Marshall, S.G., Vsisey, M. (1972). Sweetness perception in relation to some textural characteristics of hydrocolloid gels. J. Texture Stud., 3, 173-185.
[42] Majzoobi, M., Ghiasi, F., Habibi, M., Hedayati, S., Farahnaky, A. (2014). Influence of soy protein isolate on the quality of batter and sponge cake. J Food Process Pres., 38, 1164-1170.
[43] Yamin, F.F., Lee, M., Pollak, L.M., White, P.J. (1999). Thermal properties of starch in corn variants isolated after chemical mutagenesis of inbred line B73. Cereal Chem., 76, 175-181.
[44] Zhang, Y., Zeng, H., Wang, Y., Zeng, S., Zheng, B. (2014). Structural characteristics and crystalline properties of lotus seed resistant starch and its prebiotic effects. Food Chem., 155, 311-318.
[45] Lin, J.H., Singh, H., Wen, C.Y., Chang, Y.H. (2011). Partial-degradation and heat-moisture dual modification on the enzymatic resistance and boiling-stable resistant starch content of corn starches. J. Cereal Sci., 54, 83-89.
[46] Song, Y., Jane, J. (2000). Characterization of barley starches of waxy, normal, and high amylose varieties. Carbohydr. Polym., 41, 365-377.
[47] Donovan, J.W., Lorenz, K., Kulp, K. (1983). Differential Scanning Calorimetry of Heat-Moisture. Cereal Chem., 60, 381-387.
[48] Adebowale, K.O., Lawal, O.S. (2003). Microstructure, physicochemical properties and retrogradation behaviour of Mucuna bean (Mucuna pruriens) starch on heat moisture treatments. Food Hydrocoll., 17, 265-272.
[49] Lopez-Rubio, A., Flanagan, B.M., Shrestha, A.K., Gidley, M.J., Gilbert, E.P. (2008). Molecular rearrangement of starch during in vitro digestion: toward a better understanding of enzyme resistant starch formation in processed starches. Biomacromolecules., 9, 1951-1958.
[50] Cheetham, N.W., Tao, L. (1998). Variation in crystalline type with amylose content in maize starch granules: an X-ray powder diffraction study. Carbohydr. Polym., 36, 277-284.
[51] Xie, X.S., Liu, Q., Cui, S.W. (2006). Studies on the granular structure of resistant starches (type 4) from normal, high amylose and waxy corn starch citrates. Food Res Int., 39, 332-341.
[52] Chanvrier, H., Uthayakumaran, S., Appelqvist, I.A., Gidley, M.J., Gilbert, E.P., López-Rubio, A. (2007). Influence of storage conditions on the structure, thermal behavior, and formation of enzyme-resistant starch in extruded starches. J Agric Food Chem., 55, 9883-9890.
[53] Luckett, C.R., Wang, Y.J. (2012). Effects of β-amylolysis on the resistant starch formation of debranched corn starches. J Agric Food Chem., 60, 4751-4757.
[54] Gonzalez-Soto, R.A., Mora-Escobedo, R., Hernandez-Sanchez, H., Sanchez-Rivera, M., Bello-Perez, L.A. (2007). The influence of time and storage temperature on resistant starch formation from autoclaved debranched banana starch. Food Res Int., 40, 304-310.
[55] Miao, M., Jiang, B., Zhang, T. (2009). Effect of pullulanase debranching and recrystallization on structure and digestibility of waxy maize starch. Carbohydr. Polym., 76, 214-221.
[56] Bird, A.R., Lopez-Rubio, A., Shrestha, A.K., Gidley, M.J. (2009). Resistant starch in vitro and in vivo: Factors determining yield, structure, and physiological relevance, in: Kasapis, S., Norton, I.T., Johan, B. (Eds.), Modern biopolymer science, Academic Press, pp 449-510.
[57] Russell, P.L., Berry, C.S., Greenwell, P. (1989). Characterisation of resistant starch from wheat and maize. J. Cereal Sci., 9, 1-15.
[58] Siljeström, M., Eliasson, A.C., Björck, I. (1989). Characterization of resistant starch from autoclaved wheat starch. StarchStärke., 41, 147-151.
[59] Shi, M.M., Gao, Q.Y. (2011). Physicochemical properties, structure and in vitro digestion of resistant starch from waxy rice starch. Carbohydr. Polym., 84, 1151-1157.
[60] Shamai, K., Bianco-Peled, H., Shimoni, E. (2003). Polymorphism of resistant starch type III. Carbohydr. Polym., 54, 363-369.
[61] Hibi, Y., Matsumoto, T., Hagiwara, S. (1993). Effect of high pressure on the crystalline structure of various starch granules. Cereal Chem., 70, 671-671.
[62] Stute, R., Klingler, R.W., Boguslawski, S., Eshtiaghi, M.N., Knorr, D. (1996). Effects of high pressures treatment on starches. StarchStärke., 48, 399-408.
[63] Katopo, H., Song, Y., Jane, J.L. (2002). Effect and mechanism of ultrahigh hydrostatic pressure on the structure and properties of starches. Carbohydr. Polym., 47, 233-244.
[64] Bauer, B.A., Wiehle, T., Knorr, D. (2005). Impact of high hydrostatic pressure treatment on the resistant starch content of wheat starch. StarchStärke., 57, 124-133.
[65] French, D. (1984). Organization of starch granules, in: Whistler, R.L., BeMiller, J.N., Paschall, E.F. (Eds.), Starch: Chemistry and Technology (Second Edition). Academic Press, pp 183-247.
[66] Hasjim, J., Jane, J.L. (2009). Production of Resistant Starch by Extrusion Cooking of Acid‐Modified Normal‐Maize Starch. J. Food Sci., 74, 556-562.
[67] Godet, M.C., Bouchet, B., Colonna, P., Gallant, D.J., Buleon, A. (1996). Crystalline Amylose‐Fatty Acid Complexes: Morphology and Crystal Thickness. J. Food Sci., 61, 1196-1201.
[68] Shrestha, A.K., Lopez-Rubio, A., Blazek, J., Gilbert, E.P., Gidley, M.J.) 2010). Enzyme resistance and structural organization in extruded high amylose maize starch. Carbohydr. Polym., 80, 699-710.