Optimization of Phenolic Compound Extraction from Freeze-Dried Brassica oleracea Cultivars Using Response Surface Methodology
Source abstract
Abstract
Optimizing the recovery of bioactive compounds is critical for the accurate assessment of the quality of freeze-dried vegetables. In this context, Response Surface Methodology (RSM) was performed to optimize the ultrasound-assisted extraction (UAE) of phenolic compounds from freeze-dried broccoli (cv ‘Thassos’) and cauliflower (cv ‘Cercy’) florets. The influence of three process parameters, namely solvent-to-material ratio (20 to 60 mL/g), extraction time (10 to 40 min) and solvent mixture (methanol: water) composition (60 to 100% methanol) was evaluated. Multi-response optimization identified the optimal process conditions for both cultivars (composite desirability = 0.996) as a 60 mL/g ratio, 10 min extraction time and 76% methanol content. The application of the optimized extraction conditions to broccoli ‘Naxos’ and cauliflower ‘Guideline’ cultivars, confirmed the model applicability and revealed significant genotypic heterogeneity (p < 0.05). Pearson’s Correlation Analysis revealed a very high positive (r > 0.9) correlation between TPC and ABTS for both broccoli and cauliflower, high (r = 0.78) correlation between TPC and FRAP for broccoli and moderate (r = 0.63) for cauliflower. These findings confirm that process parameter optimization is crucial for the maximum recovery of phenolic compounds from freeze-dried broccoli and cauliflower, and UAE conditions should be carefully selected to ensure accurate cultivar evaluation.
Source: crossref · Quality: baseline
Research context
OpenAlex topics: Phytochemicals and Antioxidant Activities · Genomics, phytochemicals, and oxidative stress · Freezing and Crystallization Processes
SciVX discovery tags are terminology-based. OpenAlex topics are source-provided classifications.
Affiliations
Laboratory of Chemistry, Analysis & Design of Food Processes, Department of Food Science and Technology, University of West Attica, Agiou Spyridonos, 12243 Egaleo, Greece
References (56)
Show source-provided references
1. Zuluaga, D.L., D’Agostino, N., Blanco, E., Curci, P.L., and Sonnante, G. (2024). Genetic Relationships and Molecular Signatures of Divergence in Traditional Landraces and Morphotypes of Brassica Oleracea. Plants, 14.10.3390/plants14010020 ↗
2. Hasanuzzaman, M. (2020). Agricultural, Economic and Societal Importance of Brassicaceae Plants. The Plant Family Brassicaceae, Springer.10.1007/978-981-15-6345-4 ↗
3. Diversity of Sicilian Broccoli (Brassica oleracea Var. italica) and Cauliflower (Brassica oleracea Var. botrytis) Landraces and Their Distinctive Bio-Morphological, Antioxidant, and Genetic Traits10.1007/s10722-017-0547-8 ↗
4. Kole, C. (2007). Brassica Oleracea. Vegetables, Springer.10.1007/978-3-540-34536-7 ↗
5. Compositional Traits of Hybrid Populations of Brassica oleracea L. Var. italica (Broccoli) and Brassica oleracea L. Var. botrytis (Cauliflower) during Four Organic Breeding Cycles10.1016/j.jfca.2024.106209 ↗
6. The Value of Bioactive Compounds of Cruciferous Vegetables (Brassica) as Antimicrobials and Antioxidants: A Review
7. Lin, D., Xiao, M., Zhao, J., Li, Z., Xing, B., Li, X., Kong, M., Li, L., Zhang, Q., and Liu, Y. (2016). An Overview of Plant Phenolic Compounds and Their Importance in Human Nutrition and Management of Type 2 Diabetes. Molecules, 21.10.3390/molecules21101374 ↗
8. Ramirez, D., Abellán-Victorio, A., Beretta, V., Camargo, A., and Moreno, D.A. (2020). Functional Ingredients from Brassicaceae Species: Overview and Perspectives. Int. J. Mol. Sci., 21.10.3390/ijms21061998 ↗
9. Clean Recovery of Antioxidant Compounds from Plant Foods, by-Products and Algae Assisted by Ultrasounds Processing. Modeling Approaches to Optimize Processing Conditions10.1016/j.tifs.2015.01.002 ↗
10. Ultrasound: A Clean, Green Extraction Technology10.1016/j.trac.2015.04.013 ↗
11. Ultrasound Assisted Extraction of Food and Natural Products. Mechanisms, Techniques, Combinations, Protocols and Applications. A Review10.1016/j.ultsonch.2016.06.035 ↗
12. A Comprehensive Review of Ultrasonic Assisted Extraction (UAE) for Bioactive Components: Principles, Advantages, Equipment, and Combined Technologies10.1016/j.ultsonch.2023.106646 ↗
13. Recent Advances in Ultrasound-Assisted Extraction of Natural Products Using Novel Solvents: A Mini-Review10.1016/j.coche.2025.101132 ↗
14. Bleakley, S., and Hayes, M. (2017). Algal Proteins: Extraction, Application, and Challenges Concerning Production. Foods, 6.10.3390/foods6050033 ↗
15. Ultrasound Assisted Extraction (UAE) of Bioactive Compounds from Fruit and Vegetable Processing by-Products: A Review10.1016/j.ultsonch.2020.105325 ↗
16. Dispersion of Hydrophobic Magnetic Nanoparticles Using Ultarsonic-Assisted in Combination with Coacervative Microextraction for the Simultaneous Preconcentration and Determination of Tricyclic Antidepressant Drugs in Biological Fluids10.1016/j.ultsonch.2016.04.010 ↗
17. Ultrasound-Assisted Extraction for Food and Environmental Samples10.1016/j.trac.2012.12.005 ↗
18. Applications of Ultrasound in Food and Bioprocessing10.1016/j.ultsonch.2014.08.012 ↗
19. Sarker, S.D., and Nahar, L. (2018). An Introduction to Computational Phytochemistry. Computational Phytochemistry, Elsevier.10.1016/B978-0-12-812364-5.00001-8 ↗
20. Effect of Freeze-Thaw Cycles Pretreatment on the Vacuum Freeze-Drying Process and Physicochemical Properties of the Dried Garlic Slices10.1016/j.foodchem.2020.126883 ↗
21. Changes in Curcuminoids and Chemical Components of Turmeric (Curcuma longa L.) under Freeze-Drying and Low-Temperature Drying Methods10.1016/j.foodchem.2020.128121 ↗
22. Krakowska-Sieprawska, A., Kiełbasa, A., Rafińska, K., Ligor, M., and Buszewski, B. (2022). Modern Methods of Pre-Treatment of Plant Material for the Extraction of Bioactive Compounds. Molecules, 27.10.3390/molecules27030730 ↗
23. Maisl, C., Doppler, M., Seidl, B., Bueschl, C., and Schuhmacher, R. (2023). Untargeted Plant Metabolomics: Evaluation of Lyophilization as a Sample Preparation Technique. Metabolites, 13.10.3390/metabo13060686 ↗
24. Freeze-Drying Pretreatment of Watermelon Peel to Improve the Efficiency of Pectin Extraction: RSM Optimization, Extraction Mechanism, and Characterization10.1016/j.ijbiomac.2023.125944 ↗
25. Santos, A.A.D.L., Leal, G.F., Marques, M.R., Reis, L.C.C., Junqueira, J.R.D.J., Macedo, L.L., and Corrêa, J.L.G. (2025). Emerging Drying Technologies and Their Impact on Bioactive Compounds: A Systematic and Bibliometric Review. Appl. Sci., 15.10.3390/app15126653 ↗
26. Senevirathna, N., Hassanpour, M., O’Hara, I., and Karim, A. (2024). Investigation of the Effects of Energy-Efficient Drying Techniques and Extraction Methods on the Bioactive and Functional Activity of Banana Inflorescence. Energies, 17.10.3390/en17164119 ↗
27. Effect of Different Drying and Cooking Treatments on Phytochemicals and Antioxidant Activity in Broccoli: An Experimental in Vitro Study10.1590/fst.101622 ↗
28. Chemical Composition and Antioxidant Activity in Different Tissues of Brassica Vegetables10.3390/molecules20011228 ↗
29. Coşkun, N., Sarıtaş, S., Jaouhari, Y., Bordiga, M., and Karav, S. (2024). The Impact of Freeze Drying on Bioactivity and Physical Properties of Food Products. Appl. Sci., 14.10.20944/preprints202409.0950.v1 ↗
30. Uwineza, A., and Zhang, X. (2026). Application of Freeze-Drying Technology in the Food Industry: A Review. Foods, 15.10.3390/foods15040790 ↗
31. Herbal Distillates: A New Era of Grape Marc Distillates with Enriched Antioxidant Profile10.1016/j.foodchem.2018.01.162 ↗
32. Antiradical–Antimicrobial Activity and Phenolic Profile of Pomegranate (Punica granatum L.) Juices from Different Cultivars: A Comparative Study10.1039/C4RA11795F ↗
33. Tsiaka, T., Stavropoulou, N.A., Giannakourou, M.C., Strati, I.F., and Sinanoglou, V.J. (2023). Optimization of Ultrasound-Assisted Extraction and Characterization of the Phenolic Compounds in Rose Distillation Side Streams Using Spectrophotometric Assays and High-Throughput Analytical Techniques. Molecules, 28.10.3390/molecules28217403 ↗
34. Myers, R.H., Montgomery, D.C., and Anderson-Cook, C.M. (2016). Response Surface Methodology: Process and Product Optimization Using Designed Experiments, John Wiley & Sons, Incorporated. [4th ed.]. New York Academy of Sciences Series.
35. Modeling and Optimization I: Usability of Response Surface Methodology10.1016/j.jfoodeng.2005.11.024 ↗
36. Effects of Ultrasound-Assisted Bath, Probe, and Extraction Time on Bioactive Compounds and Antioxidant Activity in White Tea (Camellia Sinensis) Extracts from Purple- and Green-Leaf Cultivars10.1007/s44447-025-00014-x ↗
37. Aliaño-González, M.J., Jarillo, J.A., Carrera, C., Ferreiro-González, M., Álvarez, J.Á., Palma, M., Ayuso, J., Barbero, G.F., and Espada-Bellido, E. (2020). Optimization of a Novel Method Based on Ultrasound-Assisted Extraction for the Quantification of Anthocyanins and Total Phenolic Compounds in Blueberry Samples (Vaccinium corymbosum L.). Foods, 9.10.3390/foods9121763 ↗
38. Ultrasound Assisted Extraction of Bioactive Compounds in Fresh and Freeze-Dried Vitis Vinifera Cv Tannat Grape Pomace10.1016/j.fbp.2020.09.012 ↗
39. The Effect of Solvent Volume Ratio and Extraction Time on the Yield of Red Dye from Sappanwood10.1088/1757-899X/1053/1/012128 ↗
40. Hu, X., Zhang, B., Du, X., Zhang, H., Zhu, T., Zhang, S., Yang, X., Zhang, Z., Yang, T., and Wang, X. (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, 14.10.3390/foods14172966 ↗
41. European Parliament (2009). Council Directive 2009/32/EC of the European Parliament and of the Council of 23 April 2009 on the Approximation of the Laws of the Member States on Extraction Solvents Used in the Production of Foodstuffs and Food Ingredients, The European Parliament and the Council of the European Union.
42. Plaskova, A., and Mlcek, J. (2023). New Insights of the Application of Water or Ethanol-Water Plant Extract Rich in Active Compounds in Food. Front. Nutr., 10.10.3389/fnut.2023.1118761 ↗
43. Solvent Effects on the Phenolic Compounds and Antioxidant Activity Associated with Camellia Polyodonta Flower Extracts10.1021/acsomega.4c01321 ↗
44. Optimization of the Extraction Process of Polyphenols from Thymus serpyllum L. Herb Using Maceration, Heat- and Ultrasound-Assisted Techniques10.1016/j.seppur.2017.01.055 ↗
45. Antioxidant Properties and Sensory Preference of Broccoli Affected by Culinary Practices10.12944/CRNFSJ.12.3.33 ↗
46. Antioxidant Activity in Selected Brassicaceae Vegetables
47. Montaner, C., Mallor, C., Laguna, S., and Zufiaurre, R. (2023). Bioactive Compounds, Antioxidant Activity, and Mineral Content of Bróquil: A Traditional Crop of Brassica oleracea Var. italica. Front. Nutr., 9.10.3389/fnut.2022.1006012 ↗
48. Effect of Cooking Method on Antioxidant Compound Contents in Cauliflower10.3746/pnf.2019.24.2.210 ↗
49. Enhancing Phenolic Content in Dried Broccoli: Insights from Ultrasonic Assisted Extraction and Response Surface Methodology
50. A Comparative Study of Drying Methods on Physical Characteristics, Nutritional Properties and Antioxidant Capacity of Broccoli10.1080/07373937.2019.1656642 ↗
51. Drabińska, N., Jeż, M., and Nogueira, M. (2021). Variation in the Accumulation of Phytochemicals and Their Bioactive Properties among the Aerial Parts of Cauliflower. Antioxidants, 10.10.3390/antiox10101597 ↗
52. The Antioxidant Activity of Selected Cruciferous Vegetables Subjected to Aquathermal Processing10.1016/j.foodchem.2007.07.023 ↗
53. Carotenoids, Flavonoids, Chlorophylls, Phenolic Compounds and Antioxidant Activity in Fresh and Cooked Broccoli (Brassica oleracea Var. Avenger) and Cauliflower (Brassica oleracea Var. Alphina F1)10.1016/j.lwt.2015.03.089 ↗
54. Ross, I.A. (2024). The Bioactive Components of Brassicaceae. Plant-Based Therapeutics, Volume 2, Springer Nature.10.1007/978-3-031-63681-3 ↗
55. Martínez-Zamora, L., Hashemi, S., Cano-Lamadrid, M., Bueso, M.C., Aguayo, E., Kessler, M., and Artés-Hernández, F. (2024). Ultrasound-Assisted Extraction of Bioactive Compounds from Broccoli By-Products. Foods, 13.10.3390/foods13101441 ↗
56. González, F., Quintero, J., Del Río, R., and Mahn, A. (2021). Optimization of an Extraction Process to Obtain a Food-Grade Sulforaphane-Rich Extract from Broccoli (Brassica oleracea Var. italica). Molecules, 26.10.3390/molecules26134042 ↗