β-环糊精改性硅藻土载体的制备、表征及其对肉桂精油的负载与缓释性能研究
Preparation and Characterisation of β-Cyclodextrin-Modified Diatomaceous Earth Carriers and Investigation of Their Loading and Controlled-Release Properties for Cinnamon Essential Oil
DOI: 10.12677/amc.2026.142016, PDF,    科研立项经费支持
作者: 张舒婷, 滕桂香*, 王洪雨, 俞梦圆, 蒙延赞, 赵 萌, 杨 燕：兰州交通大学生物与制药工程学院，甘肃 兰州；张 春：兰州交通大学化学化工学院，甘肃 兰州
关键词: 硅藻土；β-环糊精；肉桂精油；负载；缓释；动力学；Diatomaceous Earth； β-Cyclodextrin； Cinnamon Essential Oil； Loading； Sustained Release； Kinetics
摘要: 本研究以天然硅藻土(D)为基材，通过碱处理与β-环糊精(β-CD)功能化修饰，成功制备了一种新型多孔载体材料(β-CD-AMD)。采用扫描电子显微镜(SEM)、傅里叶变换红外光谱(FTIR)、X射线衍射(XRD)、热重分析(TGA)及氮气吸附–脱附(BET)等手段对载体结构进行表征。系统考察了β-CD-AMD对肉桂精油(CEO)的负载行为，通过响应面法优化了负载条件，并利用动力学模型、等温吸附模型及热力学参数探究其负载机理。进一步研究了不同温度下CEO从载体中的释放特性，并结合释放动力学模型分析其缓释行为。结果表明，β-CD-AMD具有规整的多级孔结构，活性位点增多；在最优条件(时间120 min、温度25℃、精油与载体比1.5 mL/g)下，CEO包封率可达85.3%，最大理论负载容量为1462 mg/g。负载过程符合准二级动力学和Langmuir等温模型，为自发、放热的物理化学协同作用。体外释放实验显示，β-CD-AMD能显著延缓CEO释放，在20℃和30℃下分别于21天和17天内实现97%以上的累积释放，释放行为遵循Korsmeyer-Peppas模型。该载体展现出优异的缓释性能和热稳定性，为疏水性活性物质的包载与控释提供了新策略。
Abstract: This study successfully prepared a novel porous carrier material (β-CD-AMD) using natural diatomaceous earth (D) as the substrate, through alkaline treatment and functionalisation with β-cyclodextrin (β-CD). The structure of the carrier was characterised using scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), thermogravimetric analysis (TGA), and nitrogen adsorption-desorption (BET) techniques. The loading behaviour of cinnamon essential oil (CEO) onto β-CD-AMD was systematically investigated. Loading conditions were optimised using response surface methodology, and the loading mechanism was explored through kinetic models, isothermal adsorption models, and thermodynamic parameters. The release characteristics of CEO from the carrier at different temperatures were further studied, with sustained-release behaviour analysed using release kinetic models. The results indicate that β-CD-AMD exhibits a regular multi-level pore structure with an increased number of active sites. Under optimal conditions (120 min loading time, 25˚C temperature, 1.5 mL/g oil-to-carrier ratio), the CEO encapsulation rate reached 85.3%, with a maximum theoretical loading capacity of 1462 mg/g. The loading process conformed to pseudo-second-order kinetics and the Langmuir isotherm model, representing a spontaneous, exothermic physicochemical synergistic interaction. In vitro release studies demonstrated that β-CD-AMD significantly retards CEO release, achieving over 97% cumulative release within 21 days at 20˚C and 17 days at 30˚C. The release behaviour conformed to the Korsmeyer-Peppas model. This carrier exhibits excellent sustained-release properties and thermal stability, offering a novel strategy for the encapsulation and controlled release of hydrophobic active substances.
文章引用：张舒婷, 滕桂香, 王洪雨, 俞梦圆, 蒙延赞, 赵萌, 杨燕, 张春. β-环糊精改性硅藻土载体的制备、表征及其对肉桂精油的负载与缓释性能研究[J]. 材料化学前沿, 2026, 14(2): 140-152. https://doi.org/10.12677/amc.2026.142016

参考文献

[1] Almasi, L., Radi, M., Amiri, S. and McClements, D.J. (2021) Fabrication and Characterization of Antimicrobial Biopolymer Films Containing Essential Oil-Loaded Microemulsions or Nanoemulsions. Food Hydrocolloids, 117, Article ID: 106733. [Google Scholar] [CrossRef] 
[2] Randrianarivelo, R., Sarter, S., Odoux, E., BRAT, P., Lebrun, M., Romestand, B., et al. (2009) Composition and Antimicrobial Activity of Essential Oils of Cinnamosma fragrans. Food Chemistry, 114, 680-684. [Google Scholar] [CrossRef] 
[3] Yildiz, Z.I., Kilic, M.E., Durgun, E. and Uyar, T. (2019) Molecular Encapsulation of Cinnamaldehyde within Cyclodextrin Inclusion Complex Electrospun Nanofibers: Fast-Dissolution, Enhanced Water Solubility, High Temperature Stability, and Antibacterial Activity of Cinnamaldehyde. Journal of Agricultural and Food Chemistry, 67, 11066-11076. [Google Scholar] [CrossRef] [PubMed]
[4] Liu, T., Chen, Y., Zhao, S., Guo, J., Wang, Y., Feng, L., et al. (2023) The Sustained-Release Mechanism of Citrus Essential Oil from Cyclodextrin/cellulose-Based Pickering Emulsions. Food Hydrocolloids, 144, Article ID: 109023. [Google Scholar] [CrossRef] 
[5] Bariana, M., Aw, M.S., Kurkuri, M. and Losic, D. (2013) Tuning Drug Loading and Release Properties of Diatom Silica Microparticles by Surface Modifications. International Journal of Pharmaceutics, 443, 230-241. [Google Scholar] [CrossRef] [PubMed]
[6] Hădărugă, N.G., Bandur, G.N., David, I. and Hădărugă, D.I. (2019) A Review on Thermal Analyses of Cyclodextrins and Cyclodextrin Complexes. Environmental Chemistry Letters, 17, 349-373. [Google Scholar] [CrossRef] 
[7] Shu, C., Yusufali, Z., Ho, K.K.H.Y. and Sun, X. (2025) Nanoencapsulated Cinnamaldehyde@β-Cyclodextrin Inclusion Complexes as a Sustained Release Strategy for Postharvest Rambutan Preservation. Food Hydrocolloids, 159, Article ID: 110724. [Google Scholar] [CrossRef] 
[8] Sprynskyy, M., Kovalchuk, I. and Buszewski, B. (2010) The Separation of Uranium Ions by Natural and Modified Diatomite from Aqueous Solution. Journal of Hazardous Materials, 181, 700-707. [Google Scholar] [CrossRef] [PubMed]
[9] Xue, B., Yi, T., Li, D., Li, F. and Luo, F. (2022) The Effect of Alkali Treatment and Organic Modification of Diatomite on the Properties of Diatomite Composite Separators. New Journal of Chemistry, 46, 23268-23275. [Google Scholar] [CrossRef] 
[10] Shi, S., Ocampo-Pérez, R., Lv, J., Liu, Q., Nan, F., Liu, X., et al. (2021) Diatomite Cross-Linked β-Cyclodextrin Polymers: A Novel Vision of Diatomite Adsorbent for the Removal of Bisphenol A. Environmental Technology & Innovation, 23, Article ID: 101602. [Google Scholar] [CrossRef] 
[11] Zhao, Y., Geng, J., Cai, J., Cai, Y. and Cao, C. (2020) Adsorption Performance of Basic Fuchsin on Alkali-Activated Diatomite. Adsorption Science & Technology, 38, 151-167. [Google Scholar] [CrossRef] 
[12] Alfassam, H.E., Al Othman, S.I., Al-Waili, M.A., Allam, A.A. and Abukhadra, M.R. (2023) Characterization of Β-Cyclodextrin Hybridized Diatomite as Potential Delivery Systems of Oxaliplatin and 5-Fluorouracil Drugs; Equilibrium Modeling of Loading and Release Kinetics. Journal of Macromolecular Science, Part B, 62, 478-503. [Google Scholar] [CrossRef] 
[13] Hu, D., Xu, Y., Gao, C., Meng, L., Feng, X., Wang, Z., et al. (2024) Preparation and Characterization of Starch/PBAT Film Containing Hydroxypropyl-β-Cyclodextrin/Ethyl Lauroyl Arginate/Cinnamon Essential Oil Microcapsules and Its Application in the Preservation of Strawberry. International Journal of Biological Macromolecules, 259, Article ID: 129204. [Google Scholar] [CrossRef] [PubMed]
[14] Alfassam, H.E., Ashraf, M., Al Othman, S.I., Al-Waili, M.A., Allam, A.A. and Abukhadra, M.R. (2023) Insight into the Physiochemical and Cytotoxic Properties of β-Cyclodextrin Hybridized Zeoilitic Diatomite as an Enhanced Carrier of Oxaliplatin Drug: Loading, Release, and Equilibrium Studies. Journal of Inorganic and Organometallic Polymers and Materials, 33, 2984-3001. [Google Scholar] [CrossRef] 
[15] Yao, J., Zhang, G., Zhang, Y., Wu, X., Liu, C. and Rao, Z. (2025) Fabrication and Thermal Properties of Composite Phase Change Materials Based on Modified Diatomite for Thermal Energy Storage. Journal of Energy Storage, 113, Article ID: 115749. [Google Scholar] [CrossRef] 
[16] Gao, Q., Sun, Y., He, R., Zheng, J., Zhang, B., Tan, C.P., et al. (2023) Molecular Encapsulation of Cinnamaldehyde in V-Type Starch: The Role of Solvent and Temperature. Food Hydrocolloids, 136, Article ID: 108285. [Google Scholar] [CrossRef] 
[17] Yang, S., Miao, Q., Huang, Y., Jian, P., Wang, X. and Tu, M. (2020) Preparation of Cinnamaldehyde-Loaded Polyhydroxyalkanoate/Chitosan Porous Microspheres with Adjustable Controlled-Release Property and Its Application in Fruit Preservation. Food Packaging and Shelf Life, 26, Article ID: 100596. [Google Scholar] [CrossRef] 
[18] Lin, X., Xie, Y., Lu, H., Xin, Y., Altaf, R., Zhu, S., et al. (2021) Facile Preparation of Dual La-Zr Modified Magnetite Adsorbents for Efficient and Selective Phosphorus Recovery. Chemical Engineering Journal, 413, Article ID: 127530. [Google Scholar] [CrossRef] 
[19] Alfassam, H.E., Ashraf, M., Al Othman, S.I., Al-Waili, M.A., Allam, A.A. and Abukhadra, M.R. (2023) Synthesis and Characterization of Cellulose Functionalized Zeolitic Diatomite as an Enhanced Carrier of Oxaliplatin Drug; Loading, Release, and Cytotoxicity. International Journal of Biological Macromolecules, 235, Article ID: 123825. [Google Scholar] [CrossRef] [PubMed]
[20] Lu, L., Xu, J., Huang, X., Hu, L., Ji, K., Jiang, C., et al. (2025) Mussel Foot Protein Membrane‐Enclosed Crystalline Drug with Zero‐order Release Kinetics for Long‐acting Therapy. Angewandte Chemie International Edition, 64, Article ID: 2502205. [Google Scholar] [CrossRef] [PubMed]
[21] Rezaeinia, H., Ghorani, B., Emadzadeh, B. and Tucker, N. (2019) Electrohydrodynamic Atomization of Balangu (Lallemantia royleana) Seed Gum for the Fast-Release of Mentha longifolia L. Essential Oil: Characterization of Nano-Capsules and Modeling the Kinetics of Release. Food Hydrocolloids, 93, 374-385. [Google Scholar] [CrossRef] 
[22] Janatova, A., Bernardos, A., Smid, J., Frankova, A., Lhotka, M., Kourimská, L., et al. (2015) Long-Term Antifungal Activity of Volatile Essential Oil Components Released from Mesoporous Silica Materials. Industrial Crops and Products, 67, 216-220. [Google Scholar] [CrossRef] 
[23] Liu, J., Wu, D., Zhu, N., Wu, Y. and Li, G. (2021) Antibacterial Mechanisms and Applications of Metal-Organic Frameworks and Their Derived Nanomaterials. Trends in Food Science & Technology, 109, 413-434. [Google Scholar] [CrossRef] 
[24] Hosseini, S.F., Zandi, M., Rezaei, M. and Farahmandghavi, F. (2013) Two-Step Method for Encapsulation of Oregano Essential Oil in Chitosan Nanoparticles: Preparation, Characterization and in Vitro Release Study. Carbohydrate Polymers, 95, 50-56. [Google Scholar] [CrossRef] [PubMed]
[25] Zhang, D., Lv, P., Zhou, C., Zhao, Y., Liao, X. and Yang, B. (2019) Cyclodextrin-Based Delivery Systems for Cancer Treatment. Materials Science and Engineering: C, 96, 872-886. [Google Scholar] [CrossRef] [PubMed]