Vol. 25, No. 3 (2026), Alim26768 https://doi.org/10.24275/rmiq/Alim26768

Development, evaluation, and kinetic modeling of blueberry (Vaccinium corymbosum L.) freeze‑drying considering osmotic pretreatments and freezing methods

 

Authors

C. Michel-Cuello, J.L. Luna-Gallegos, N. Aguilar-Rivera, C. López-Palacios

Abstract

Blueberries (Vaccinium corymbosum L.) that do not meet export standards offer potential for valorization through advanced dehydration processes. This study developed, evaluated, and kinetically modeled a freeze-drying process for blueberries, incorporating osmotic dehydration (OD) with sucrose solutions at 50, 60, and 70% (w/v), along with conventional freezing and liquid nitrogen ultrafreezing. The effects on water loss, moisture evolution, and drying efficiency were analyzed. OD was performed at 45 °C, followed by freeze-drying at 0.420 mbar and −51 °C. No significant differences were observed among sucrose concentrations during the initial OD stages; however, the 70% solution enhanced water loss at later stages, requiring more time to approach osmotic equilibrium. Water loss evolution during OD and freeze-drying was successfully described using empirical kinetic models, with the Midilli–Küçük model providing the best fit. Final moisture content showed no statistically significant differences among treatments, indicating that freeze-drying is the dominant unit operation governing overall dehydration. Liquid nitrogen ultrafreezing did not offer clear advantages over conventional freezing. These findings demonstrate that simple, low-cost osmotic pretreatments combined with freeze-drying represent a viable strategy for valorizing off-grade blueberries.

Keywords

blueberry, freeze‑drying, kinetic modeling, osmotic dehydration, moisture loss.

References
  • Al-Faruq, A., Farahnaky, A., Dokouhaki, M., Khatun, H.A., Trujillo, F.J. and Majzoobi, M. (2025). Technological Innovations in Freeze Drying: Enhancing Efficiency, Sustainability, and Food Quality. Food Engineering Reviews 17, 859–883. https://doi.org/10.1007/s12393-025-09415-8
  • AOAC International. (2019). Official methods of analysis (21st ed.). Gaithersburg, MD: AOAC International.
  • Assegehegn, G., Brito‑de la Fuente, E., Franco, J. M., and Gallegos, C. (2019). The importance of understanding the freezing step and its impact on freeze‑drying process performance. Journal of Pharmaceutical Sciences, 108(4), 1378–1395. https://doi.org/10.1016/j.xphs.2018.11.039
  • Bhatta, S., Stevanovic Janezic, T. and Ratti, C. (2020). Freeze-drying of plant-based foods. Foods 9(1), 87. https://doi.org/10.3390/foods9010087
  • Botello‑Álvarez, J.E., Ríos‑Fuentes, B., Pérez‑Pérez, M.C.I., Rico‑Baeza, G., Flores‑Martínez, N.L. and Fausto‑Castro, L. (2026). Valorization of dehydrated broccoli agroindustrial residues. Revista Mexicana de Ingeniería Química, 25(1). https://doi.org/10.24275/rmiq/Alim26644
  • Buceta, J.P., Passot, S., Scutellà, B., Bourlés, E., Fonseca, F. and Trelea, I.C. (2022). Use of 3D mathematical modelling to understand the heat transfer mechanisms during freeze-drying using high-throughput vials. Applied Thermal Engineering 207, 118099. https://doi.org/10.1016/j.applthermaleng.2022.118099
  • Buzrul, S. (2022). Reassessment of thin‑layer drying models for foods: A critical short communication. Processes, 10(1), 118. https://doi.org/10.3390/pr10010118
  • Cheng, X.F., Zhang, M., Adhikari, B. and Islam, M.N. (2014). Effect of Power Ultrasound and Pulsed Vacuum Treatments on the Dehydration Kinetics, Distribution, and Status of Water in Osmotically Dehydrated Strawberry: a Combined NMR and DSC Study. Food and Bioprocess Technology 7, 1328–1342. https://doi.org/10.1007/s11947-014-1355-1
  • Ciurzyńska, A. and Lenart, A. (2010). Structural Impact of Osmotically Pretreated Freeze-Dried Strawberries On Their Mechanical Properties. International Journal of Food Properties 12(4), 805–816. https://doi.org/10.1080/10942910903013134
  • Ciurzyńska, A. and Lenart, A. (2011). Freeze-Drying - Application in Food Processing and Biotechnology - a Review. Polish Journal of Food and Nutrition Sciences 61(3), 165–171. https://doi.org/10.2478/v10222-011-0017-5
  • Ciurzyńska, A., Kowalska, H., Czajkowska, K. and Lenart, A. (2016). Osmotic dehydration in production of sustainable and healthy food. Trends in Food Science and Technology 50, 186–192. https://doi.org/10.1016/j.tifs.2016.01.017
  • Dermesonlouoglou, E.K., Giannakourou, M.C. and Taoukis, P.S. (2007). Kinetic modelling of the quality degradation of frozen watermelon tissue: effect of the osmotic dehydration as a pre-treatment. International Journal of Food Science and Technology 42(7), 790–798. https://doi.org/10.1111/j.1365-2621.2006.01280.x
  • Donno, D., Neirotti, G., Fioccardi, A., Razafindrakoto, Z.R., Tombozara, N., Mellano, M.G., Beccaro, G.L. and Gamba, G. (2025). Freeze-Drying for the Reduction of Fruit and Vegetable Chain Losses: A Sustainable Solution to Produce Potential Health-Promoting Food Applications. Plants 14(2), 168. https://doi.org/10.3390/plants14020168
  • Egas‑Astudillo, L.A., Camacho, M.M. and Martínez‑Navarrete, N. (2021). Impact of shelf temperature on a grapefruit puree temperature evolution during freeze-drying. International Journal of Food Science and Technology 56(1), 413–419. https://doi.org/10.1111/ijfs.14656
  • Faber, F., Vorhauer‑Huget, N., Thomik, M., Gruber, S., Först, P. and Tsotsas, E. (2025). Pore-scale study of coupled heat and mass transfer during primary freeze-drying using an irregular pore network model. Drying Technology 43(1–2), 162–182. https://doi.org/10.1080/07373937.2024.2407062
  • García‑Noguera, J., Oliveira, F.I.P., Gallão, M.I., Weller, C.L., Rodrigues, S. and Fernandes, F.A.N. (2010). Ultrasound-Assisted Osmotic Dehydration of Strawberries: Effect of Pretreatment Time and Ultrasonic Frequency. Drying Technology 28(2), 294–303. https://doi.org/10.1080/07373930903530402
  • Ghellam, M., Zannou, O., Galanakis, C.M., Aldawoud, T.M.S., Ibrahim, S.A. and Koca, I. (2021). Vacuum-Assisted Osmotic Dehydration of Autumn Olive Berries: Modeling of Mass Transfer Kinetics and Quality Assessment. Foods 10(10), 2286. https://doi.org/10.3390/foods10102286
  • González‑Pérez, J.E., Ramírez‑Corona, N. and López‑Malo, A. (2021). Mass Transfer During Osmotic Dehydration of Fruits and Vegetables: Process Factors and Non-Thermal Methods. Food Engineering Reviews 13, 344–374. https://doi.org/10.1007/s12393-020-09276-3
  • Hu, X., Zhang, B., Du, X., Zhang, H., Zhu, T., Zhang, S., Yang, X., Zhang, Z. and Wu, C. (2025). Recent Advances and Future Perspectives on Heat and Mass Transfer Mechanisms Enhanced by Preformed Porous Media in Vacuum Freeze-Drying of Agricultural and Food Products. Foods 14(17), 2966. https://doi.org/10.3390/foods14172966
  • Jamshidian, M., Tehrany, E.A., Imran, M., Jacquot, M. and Desobry, S. (2010). Polylactic acid: Production, applications, nanocomposites, and release studies. Comprehensive Reviews in Food Science and Food Safety 9(5), 552–571. https://doi.org/10.1111/j.1541-4337.2010.00126.x
  • Kalt, W., Cassidy, A., Howard, L.R., Krikorian, R., Stull, A.J., Tremblay, F. and Zamora‑Ros, R. (2020). Recent Research on the Health Benefits of Blueberries and Their Anthocyanins. Advances in Nutrition 11(2), 224–236. https://doi.org/10.1093/advances/nmz065
  • Kono, S., Kon, M., Araki, T. and Sagara, Y. (2017). Effects of relationships among freezing rate, ice crystal size and color on surface color of frozen salmon fillet. Journal of Food Engineering 214, 158-165. https://doi.org/10.1016/j.jfoodeng.2017.06.023
  • Kucner, A., Klewicki, R. and Sójka, M. (2012). The influence of selected osmotic dehydration and pretreatment parameters on dry matter and polyphenol content in highbush blueberry (Vaccinium corymbosum L.) fruits. Food and Bioprocess Technology 6, 2031–2047. https://doi.org/10.1007/s11947-012-0997-0
  • Kucuk, H., Kilic, A., and Midilli, A. (2014). Common applications of thin‑layer drying curve equations and their evaluation criteria. In: Dincer, I., Midilli, A., Kucuk, H. (eds) Progress in Exergy, Energy, and the Environment. Springer, Cham. https://doi.org/10.1007/978-3-319-04681-5_63 
  • Ma, Y., Yi, J., Jin, X., Li, X., Feng, S. and Bi, J. (2023). Freeze-Drying of Fruits and Vegetables in Food Industry: Effects on Phytochemicals and Bioactive Properties Attributes - A Comprehensive Review. Food Reviews International 39(9), 6611–6629. https://doi.org/10.1080/87559129.2022.2122992
  • Mari, A., Parisouli, D.N. and Krokida, M. (2024). Exploring osmotic dehydration for food preservation: Methods, modelling, and modern applications. Foods 13(17), 2783. https://doi.org/10.3390/foods13172783
  • Montgomery, D.C. (2017). Design and analysis of experiments (9th ed.). Wiley.
  • Mousavi, R., Miri, T., Cox, P.W. and Fryer, P.J. (2007). Imaging food freezing using X-ray microtomography. International Journal of Food Science and Technology 42(6), 714–727. https://doi.org/10.1111/j.1365-2621.2007.01514.x
  • Mujumdar, A.S. (2015). Handbook of industrial drying (4th ed.). CRC Press. https://doi.org/10.1201/b17208
  • Munzenmayer, P., Ulloa, J., Pinto, M., Ramírez, C., Valencia, P., Simpson, R. and Almonacid, S. (2020). Freeze-Drying of Blueberries: Effects of Carbon Dioxide (CO2) Laser Perforation as Skin Pretreatment to Improve Mass Transfer, Primary Drying Time, and Quality. Foods 9(2), 211. https://doi.org/10.3390/foods9020211
  • Nakagawa, K. (2025). Studies on the development and modeling of food freeze-drying processes. Japan Journal of Food Engineering 26(1), 1–9. https://doi.org/10.11301/jsfe.24658
  • Nowak, D., and Jakubczyk, E. (2020). The freeze‑drying of foods—The characteristic of the process course and the effect of its parameters on the physical properties of food materials. Foods, 9(10), 1488. https://doi.org/10.3390/foods9101488
  • Pavkov, I., Stamenković, Z., Radojčin, M., Krstan, K., Bikić, S., Lutovska, M. and Ponjičan, O. (2019). Air drying of blueberry fruits: Drying kinetics, mathematical modeling and physical properties. Journal on Processing and Energy in Agriculture, 23(4), 151–157. https://doi.org/10.5937/jpea1904151p
  • Pedregosa, F., Varoquaux, G., Gramfort, A., Michel, V., Thirion, B., Grisel, O., Blondel, M., Prettenhofer, P., Weiss, R., Dubourg, V., Vanderplas, V., Passos, A., Cournnapeau, D., Brucher, M., Perrot, M. and Duchesnay É. (2011). Scikit‑learn: Machine learning in Python. Journal of Machine Learning Research, 12, 2825–2830. https://jmlr.csail.mit.edu/papers/volume12/pedregosa11a/pedregosa11a.pdf
  • Pobiega, K., Matys, A., Trusinska, M., Rybak, K., Witrowa‑Rajchert, D. and Nowacka, M. (2023). The Effect of Ultrasound and Pulsed Electric Field on the Osmotic Dehydration Process of Strawberries. Applied Sciences 13(22), 12335. https://doi.org/10.3390/app132212335
  • Prawiranto, K., Defraeye, T., Derome, D., Bühlmann, A., Hartmann, S., Verboven, P., Nicolai, B. and Carmeliet, J. (2019). Impact of drying methods on the changes of fruit microstructure unveiled by X-ray micro-computed tomography. RSC Advances 9, 10606–10624. https://doi.org/10.1039/C9RA00648F
  • Prosapio, V. and Norton, I. (2017). Influence of osmotic dehydration pre-treatment on oven drying and freeze drying performance. LWT – Food Science and Technology 80, 401–408. https://doi.org/10.1016/j.lwt.2017.03.012
  • Prosapio, V. and Norton, I. (2018). Simultaneous application of ultrasounds and firming agents to improve the quality properties of osmotic + freeze-dried foods. LWT – Food Science and Technology 96, 402–410. https://doi.org/10.1016/j.lwt.2018.05.068
  • Rajashree, V., Vijay, S.K.S., Muthuvel, I., Kavitha, S.G.G., Bharathi, A., Senthil Kumar, M. and Rajiv, P. (2024). An extensive investigation of combined freeze-drying technologies for fruit conservation. Plant Science Today 11(sp4), 1–16. https://doi.org/10.14719/pst.5515
  • Ratti, C. (2001). Hot air and freeze-drying of high-value foods: A review. Journal of Food Engineering 49(4), 311–319. https://doi.org/10.1016/S0260-8774(00)00228-4
  • Ratti, C. (2013). Freeze-drying process design. In: Handbook of Food Processing, (Ahmed J. and Shafiur-Rahman M. eds.) Pp. 371–389. CRC Press. https://doi.org/10.1002/9781444398274.ch22
  • Rurush, E., Alvarado, M., Palacios, P., Flores, Y., Rojas, M.L. and Miano, A.C. (2022). Drying kinetics of blueberry pulp and mass transfer parameters: Effect of hot air and refractance window drying at different temperatures. Journal of Food Engineering, 320, 110929. https://doi.org/10.1016/j.jfoodeng.2021.110929
  • Semenov, G.V., Krasnova, I.S., Khvylia, S.I. and Balabolin, D.N. (2021). Freezing and freeze-drying of strawberries with an additional effect of micro-vibrations. Journal of Food Science and Technology 58, 3192–3198. https://doi.org/10.1007/s13197-020-04822-7
  • Silva‑Espinoza, M.A., Ayed, C., Foster, T., Camacho, M.M. and Martínez‑Navarrete, N. (2020). The Impact of Freeze-Drying Conditions on the Physico-Chemical Properties and Bioactive Compounds of a Freeze-Dried Orange Puree. Foods 9(1), 32. https://doi.org/10.3390/foods9010032
  • Silva‑Espinoza, M.A., Camacho, M.M., Martínez‑Monzó, J. and Martínez‑Navarrete, N. (2021). Impact of the Freeze-Drying Conditions Applied to Obtain an Orange Snack on Energy Consumption. Foods 10(11), 2756. https://doi.org/10.3390/foods10112756
  • Stratta, L., Capozzi, L.C., Franzino, S. and Pisano, R. (2020). Economic analysis of a freeze‑drying cycle. Processes 8(11), 1399. https://doi.org/10.3390/pr8111399
  • Uribe, E., Vega‑Gálvez, A., Pasten, A., Ah‑Hen, K.S., Mejías, N., Sepúlveda, L., Poblete, J. and Gomez‑Perez, L.S. (2024). Drying: A Practical Technology for Blueberries (Vaccinium corymbosum L.)—Processes and their Effects on Selected Health‑Promoting Properties. Antioxidants 13(12), 1554. https://doi.org/10.3390/antiox13121554
  • Vega‑Gálvez, A., Lara, E., Flores, V., Di Scala, K. and Lemus‑Mondaca, R. (2012). Effect of selected pretreatments on convective drying process of blueberries (var. o’neil). Food and Bioprocess Technology 5(7), 1-8. https://doi.org/10.1007/s11947-011-0656-x
  • Virtanen, P., Gommers, R., Oliphant, T.E., Haberland, M., Reddy, T., Cournapeau, D., Burovski, E., Peterson, P., Weckesser, W., Bright, J., Van der Walt, S.J., Brett, M., Wilson, J., K. Millman, J., Mayorov, N., Nelson, A., Jones, E., Kern, R., Larson, E… Van Mulbregt, P. (2020). SciPy 1.0: Fundamental algorithms for scientific computing in Python. Nature Methods, 17(3), 261–272. https://doi.org/10.1038/s41592-019-0686-2
  • Yadav, A.K. and Singh, S.V. (2014). Osmotic dehydration of fruits and vegetables: A review. Journal of Food Science and Technology 51(9), 1654–1673. https://doi.org/10.1007/s13197-012-0659-2
  • Yang, D.H., Li, X.Y., Zhao, Y.F., Hou, Q.M., Meng, Q.Y. and Li, L. (2021). Osmotic dehydration kinetics of fresh and frozen blueberries considering volume shrinkage in a novel ternary solution. Food Science and Technology (Campinas) 41(3). https://doi.org/10.1590/fst.21621
  • Yao, J., Chen, W. and Fan, K. (2023). Novel Efficient Physical Technologies for Enhancing Freeze Drying of Fruits and Vegetables: A Review. Foods 12(23), 4321. https://doi.org/10.3390/foods12234321
  • Yu, Y., Jin, T.Z., Fan, X. and Xu, Y. (2017). Osmotic dehydration of blueberries pretreated with pulsed electric fields: Effects on dehydration kinetics, and microbiological and nutritional qualities. Drying Technology 35(13), 1543–1551. https://doi.org/10.1080/07373937.2016.1260583