Freeze-drying Method Research Articles

Incorporating mesoporous SiO2-HA particles into chitosan/hydroxyapatite scaffolds: A comprehensive evaluation of bioactivity and biocompatibility

In this work, composite scaffolds with various composition ratios of chitosan (CS), hydroxyapatite (HA), and mesoporous SiO2 particles co-synthesized with hydroxyapatite (SiO2-HA) were fabricated via the freeze-drying method for bone tissue engineering applications. Morphological studies showed that adding mesoporous particles resulted in a structure with a more uniformly porous geometry, subsequently leading to reduced biodegradation rates and water absorption in the scaffolds. The bioactivity results showed the introduction of mesoporous particles notably enhanced the coverage of the scaffold surface with apatite films. Moreover, biocompatibility assessments using sarcoma osteogenic cell line (SAOS-2) highlighted mesoporous particles' positive impact on cell adhesion and growth. The fluorescence images showed spindle-shaped cells with a greater number and normal cell nuclei for the scaffolds containing mesoporous SiO2-HA particles. The MTT cytotoxicity results indicated that the scaffolds containing mesoporous particles showed approximately 25 % higher cell survival more than single chitosan-based ones. What is more, the mesoporous-containing scaffolds occurred to have the best alkaline phosphatase test (ALP) activity among all scaffolds. It is important to add that CS/HA/mesoporous SiO2-HA scaffolds including SAOS-2 cells showed no sign of either early or late apoptosis. These findings affirm the potential of CS/HA/mesoporous SiO2-HA scaffolds as promising implants for bone tissue engineering.

Unlocking the potential of pomegranate peels as a valuable source of bioactive compounds through effective drying strategies

Pomegranate peels are a great resource of bioactive compounds that have potential for various applications, including functional foods, pharmaceuticals, and cosmetics. However, the drying process is an important consideration that can affect the quality and properties of pomegranate peels. This investigation sought to assess the results of different drying procedures that affect the physicochemical, functional, and antioxidant properties of pomegranate peels. Four alternative drying techniques were used such as freeze drying, microwave drying at 900 W, oven drying at 50 °C, and sun drying. According to the findings, the freeze-drying method exhibited the highest total phenolic content (186.24 mg GAE/g DM), DPPH radical scavenging activity (77.86 %), vitamin C (77.5 mg AA/100 g DM), and ferric reducing antioxidant power (31.1 mg AAE/g DM). The sun-drying technique, on the other hand, had the lowest level of quality parameters. The oven and microwave drying methods exhibited comparable results. These findings provide essential information for the optimization of pomegranate peel drying conditions, enhancing its potential to use as a significant source of bioactive compounds for a range of industrial applications. The freeze-drying method is recommended for preserving the quality of pomegranate peels and can be applied in various industries to produce high-quality products.

Hydrogel-Transformable Antioxidant Poly-γ-Glutamic Acid/Polyethyleneimine Hemostatic Powder for Efficient Wound Hemostasis.

Hemostatic powder, which can absorb large amounts of water and tends to produce repeated hydration with tissue, has been clinically proven as an ideal engineering material for treating wounds and tissues. We herein designed a polypeptide-based hemostatic powder. A water-soluble polypeptide, γ-polyglutamic acid (γ-PGA), was mixed with the polyethyleneimine (PEI), N-hydroxysuccinimide, and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide. The solution of these polymers was lyophilized to harvest the γ-PGA/PEI powder (PP hemostatic powder). When deposited on a bleeding wound, the PP hemostatic powder can quickly absorb a large amount of blood and interstitial fluid, concentrate coagulation factors, coagulate blood cells, and eventually form a stable mechanical hydrogel. The wound bleeding time of the PP hemostatic powder group was 1.8 ± 0.4 min, significantly lower than that of the commercial chitosan hemostatic powder group (2.8 ± 0.4 min). The PP hemostatic powder was endowed with antioxidant capacity by introducing protocatechuic aldehyde, which can effectively inhibit inflammation and promote wound healing. Therefore, via preparation through a facile lyophilization method, the PP hemostatic powder is expected to find a wide application prospect as a qualified hemostatic powder.

Antimicrobial peptide-modified AIE visual composite wound dressing for promoting rapid healing of infected wounds.

Wound infection is a major problem faced during wound healing. Therefore, it is necessary to develop wound dressings with excellent antimicrobial properties. Here, a smart response system of PVA-TPE/HA-AMP/SF/ALG wound dressing was prepared by a combination of chemical cross-linking and freeze-drying methods. We grafted AMP onto HA to endow the wound dressing with bacterial resistance and slow release of AMP. At the same time, the system detects bacterial activity in real time for precise antimicrobial activity (through the use of PVA-TPE) and modulates inflammation to reduce bacterial infection (through the use of AMP). In addition, the PVA-TPE/HA-AMP/SF/ALG wound dressing has a good three-dimensional mesh structure, which promotes cell proliferation, enhances collagen deposition and angiogenesis, and thus effectively promotes rapid healing of infected wounds. Moreover, it can induce the expression of inflammatory factors such as VEGF, TNF-α, IFN-γ, IL-4 and TGF-β1 in infected wounds through the Wnt/CAMK/p-PKC signaling pathway, inhibit inflammatory responses, promote wound healing and reduce scar formation. Therefore, the PVA-TPE/HA-AMP/SF/ALG wound dressing smart response system shows great promise in infected wound healing.

Bimetallic phosphide wrapped in hierarchically structured P, N co-doped porous carbon nanocatalysts for enhanced rechargeable Li[sbnd]O2 batteries

Recently, transition-metal phosphides (TMPs) cathode materials possess tremendous prospects for lithium‑oxygen batteries (LOBs). However, designing highly efficient TMPs cathode materials achieving long-cycling stability still faces numerous obstacles. The hierarchical porous carbon is expected to be a remarkable substrate for transition-metal composites because of its high specific surface area and superior electrical conductivity. Herein, NiCoP@PNC hybrid catalysts consisting of NiCoP nanoparticles and heteroatom-doped carbon skeleton were prepared via simple freeze-drying and high-temperature pyrolysis methods. The NiCoP@PNC composites with a high specific surface area and rich interior porosity can effectively accelerate charge transfer and enhance electrocatalytic activity. Compared with either Co2P@PNC and PNC electrodes, the NiCoP@PNC cathode delivers an enhanced specific capacity of 14,028.1 mAh g−1 at 100 mA g−1. The NiCoP@PNC catalytic LOBs can reach 196 cycles with the fixed capacities of 500 mAh g−1 at 200 mA g−1 due to the increased electron transfer efficiency and improved electrochemical reaction kinetics. This approach provides a facile method to prepare TMP-based composite materials for developing high-performance LOBs.

Impact of drying techniques on the composition, physicochemical attributes, antioxidant capacity, antidiabetic potential, and ACE inhibition properties of Moringa oleifera pod pulp powder

Moringa oleifera, a medicinal plant of considerable interest, has been extensively studied for its leaves' functional properties, while its pods have received relatively less attention, despite being widely consumed in India and other regions. This study investigates the effect of various drying methods on the crude composition, color, ascorbic acid content, water solubility, water absorption, total phenol content, total flavonoid content, and in vitro antioxidant and antidiabetic activities of Moringa pod pulp powder (MPP). The study reveals significant variations in the proximate composition, color attributes, and bioactive compounds of MPP resulting from freeze drying, microwave drying, oven drying, and sun drying methods. Freeze drying preserves the highest moisture content, while oven drying results in the lowest. Carbohydrate, protein, fat, ash, and crude fiber contents remain consistent across all drying methods, confirming MPP's nutritional value. Furthermore, freeze drying leads to higher ascorbic acid retention, highlighting its effectiveness in preserving this essential vitamin. The study demonstrates that freeze drying enhances water solubility, water absorption, total phenol content, and total flavonoid content in MPP. Notably, freeze dried MPP exhibits the highest in vitro antioxidant activity and antidiabetic potential, with significant α-amylase, α-glucosidase, and ACE inhibition properties. The findings underscore the importance of drying methods in preserving the quality and bioactive compounds of MPP, making it a valuable ingredient for various applications in the food and pharmaceutical industries.

Constructing gradient reflection and scattering porous framework in composite aerogels for enhanced microwave absorption

Developing high-performance microwave absorption (MA) materials becomes an urgent concern in the field of electromagnetic protection. Constructing porous framework is an efficient approach to MA owing to the abilities of adjusting impedance matching and providing more reflection and scattering paths for electromagnetic waves. Herein, a cellulose nanofibril (CNF)/honeycomb-like carbon-shell encapsulated FeCoNi@C/carbon nanotube (CNT) composite aerogel was fabricated via a facile freeze-drying method. The super-lightweight composites showed a distinctive gradient structure for reflection and scattering inside aerogel pores, micrometer small pores, and nano-fillers on the pore walls. The composite aerogel showed an ideal minimum reflection loss (RLmin) of −43.6 dB and remarkable adjustable effective absorption bandwidth (EAB) of 12.18 GHz due to good impedance matching, unique gradient porous structure, and synergies of multiple loss mechanisms. Therefore, this work will provide a viable strategy to improve the MA capability of absorbers by taking full advantage of constructing gradient reflection and scattering porous structure.

Incorporation of CaZrO3 into calcium-based heat carriers for efficient solar thermochemical energy storage

Calcium-based materials (CaCO3/CaO) have shown significant potential for use in thermochemical energy storage systems for concentrated solar power generation due to their low-cost, high-energy storage efficiency, and operational temperature range. However, the energy storage performance of calcium-based heat carriers degrades rapidly over cycles due to high-temperature sintering, limiting practical applications. In this study, we incorporated Zr into CaO using both heat-drying and freeze-drying methods, forming CaZrO3 as a physical barrier to prevent agglomeration and sintering of calcium particles at elevated temperatures. Experimental results demonstrated that Zr incorporation markedly improved cyclic energy storage stability, particularly for heat carriers derived from freeze-drying. Cao incorporated with 10 % CaZrO3 (FD-Zr10) showed a high energy storage density of 2161.75 kJ/kg over ten storage/release cycles, which was 25.89 % higher than that of pure CaO sample. Even over an extended operation of 30 cycles, FD-Zr10 still possessed the high energy storage density of 1939.76 kJ/kg. CO2-containing harsh storage conditions caused more sintering for the heat carriers, thus resulting in the performance reduction, but FD-Zr10 performed much better than other samples in resisting sintering. Various characterization analyses were conducted to investigate the reasons for the samples' cyclic stability. It was discovered that freeze-drying incorporation generated a dendritic surface with a more abundant pore structure, and the incorporated CaZrO3 functioned as a metal skeleton to mitigate high-temperature sintering.

Sodium Alginate Aerogel as a Carrier of Organogelators for Effective Oil Spill Solidification and Recovery.

Marine oil spills pose a serious threat to the marine ecological environment. Phase-selective organogelators (PSOGs) are ideal candidates for oil spill gelation when used in combination with a mechanical recovery method. However, the toxicity of an organic solvent carrier has become a key problem when it is applied in the remediation of marine oil pollution. In this study, through an inexpensive and nontoxic ionic cross-linking and freeze-drying method, we successfully developed composite oil gelling agents that used a biomass sodium alginate aerogel as the carrier of 12-hydroxystearic acid (12-HSA). Simultaneously, carboxylated cellulose nanofibers (CNF-C) with large specific surface area and graphene oxide (GO) with excellent mechanical properties as reinforcing fillers were combined with an alginate matrix. 12-HSA, as a green and inexpensive organic gelator, was uniformly loaded on the aerogels by vacuum impregnation. The sodium alginate aerogel was capable of absorbing and storing oil due to its three-dimensional network skeleton and high porosity. Rheological studies have demonstrated that the organic gelator 12-HSA can be released from the aerogel substrate and self-assemble to form an oleogel with the absorbed oil quickly. The synergistic effect between absorption and congelation endows the composite oil gelling agent with efficient oil spill recovery capability. Based on eco-friendly, biodegradable, and simple synthesis methods, this composite oil gelling agent shows great potential for application in marine oil spill recovery.

Electrospun of polyvinyl alcohol composite hydrogel nanofibers prepared by in-situ polymerization: A novel approach to fabricate hydrogel nanofiber membrane for lithium-ion batteries

The increasing demand for high-performance lithium-ion batteries has propelled the exploration of advanced materials to overcome limitations associated with commercially available polyolefin-based separators. This study introduces a pioneering approach involving the synthesis of a crosslinked hydrogel nanofiber membrane (PDs) composed of polyvinyl alcohol (PVA) and N, N-dimethylacrylamide (DMAAm) through the combination of the photo-polymerization with electrospinning process. To address key drawbacks observed in existing separators—namely, low porosity, inadequate thermal stability, and insufficient electrolyte wettability—the porosity of the PDs hydrogel nanofibers was systematically controlled through both heating drying (PD12-HD) and freeze-drying (PD12-FD) methods. The separator’s properties and performance were thoroughly examined, focusing on its chemical, mechanical, thermal, swelling, morphological, conductivity, and electrochemical properties. Comprehensive characterization of the PD12-FD separator revealed remarkable attributes surpassing those of a commercial counterpart (Celgard). The PD12-FD separator demonstrated exceptional mechanical strength (16.3 MPa), robust thermal stability (no shrinkage or deformation at 170 °C), high porosity (84.66 %), substantial electrolyte uptake capacity (672.86 %), superior ionic conductivity (3.405 mS/cm), and high lithium-ion transfer number (tLi+ = 0.678). The improvement is attributed to the cross-linked structure formed between PVA and DMAAm. Importantly, coin cells assembled with the PD12-FD separator exhibited outstanding electrochemical performance. Even after 150 cycles at 1C, the PD12-FD separator maintained a capacity above 95 % (145.48 mAh/g), surpassing both PVA and Celgard separators. This study proposes a novel methodology for fabricating hydrogel nanofiber separators and introduces a customizable synthesis approach for producing separators with enhanced performance and controlled characteristics.

Biomineralization-Inspired Confined-Space Fabrication of Polyimide Aerogels.

The biomineralization process endows biominerals with unique hierarchically porous structures and physical-chemical properties by filling the restricted microreaction space with amorphous phases before the growth of inorganic crystals. In this paper, a confined-space fabrication method inspired by biomineralization for preparing hierarchically porous polyimide (PI) aerogels and PI-derived carbon aerogels is introduced. The confined structure is established through a self-assembly method of vacuum impregnation and ultrasound-assisted freeze-drying. The hierarchically porous structure is controlled by adjusting the structure characteristics of the confined space and secondary aerogels. Subsequently, a variety of performance demonstrations are conducted to demonstrate the mechanical properties and application prospects in the fields of thermal insulation and electromagnetic shielding of the prepared aerogel.

CsxWO3-doped PEG/sweet potato form-stable composites for light-thermal conversion and energy storage

Abstract Cesium tungsten bronze (CsxWO3)-doped PEG/sweet potato form-stable composites are fabricated through a facile two-step method of lyophilization and vacuum impregnation. Abundant starch microsphere enhances the PEG loading capacity above 72 % and also supplies capillary force as well as hydrogen bonding to improve the form-stability of the composites. Here, the latent heat, relative crystallinity (Xc), and light-thermal conversion efficiency of the system with 0.99 wt% CsxWO3 reach to 137.7 J/g, 97.7 %, and 83.5 %, respectively. The light-thermal conversion efficiency increases from 64.3 % to 91.1 % with 2.00 wt% CsxWO3. Besides, the composites exhibit improved thermal stability and excellent thermal reliability. The prepared bio-based composites with low-cost have broad application prospects in the field of energy storage.

Enhancing the solubility and dissolution rate of piperine via preparation of piperine–hydroxypropyl methylcellulose 2910 solid dispersion system using freeze-drying method

Context: Piperine is the main secondary metabolite isolated from the family Piperaceae. This biologically active ingredient has many pharmacological effects, though its low water solubility limits its absorption in gastrointestinal fluid. Aims: To improve piperine’s solubility and dissolution rate by incorporating it into a solid dispersion system with the hydrophilic polymer hydroxypropyl methylcellulose (HPMC) 2910 via the freeze-drying method. Methods: Three different piperine:polymer ratios – 1:1, 1:2, and 2:1 (w/w) – were prepared. A physical mixture was also prepared in a 1:1 (w/w) ratio for comparison. The physicochemical properties of the samples were characterized by differential scanning calorimetry (DSC), powder X-ray diffraction (PXRD) analysis, Fourier transform infrared (FTIR) spectroscopy, and scanning electron microscopy (SEM). The solubility and dissolution tests were conducted in distilled water. Results: The solid dispersion characterization indicated a decrease in the melting points and endothermic peaks in the DSC analysis, a decrease in peak intensity in the PXRD patterns, no chemical interactions between active substances and polymers in the FTIR analysis, and significant morphological changes in the SEM analysis. The solubility test revealed the highest increase in piperine solubility (7.88-fold increase) for the 1:2 solid dispersion. Moreover, the 1:2 solid dispersion in the dissolution test led to the greatest amount of dissolved piperine (56.445 ± 1.13%). Conclusions: The piperine–HPMC solid dispersion system improved the solubility and dissolution rate of piperine.

Optimizing the micro/mesoporous structure of hierarchical graphene aerogel for CO2 capture by controlling the oxygen functional groups of graphene oxide

BackgroundGraphene aerogels as solid porous adsorbents are great candidates for CO2 adsorption based on their tunable hierarchical pore structure and oxygenated groups on graphene oxide can control the self-assembly and pore structure of graphene aerogels. MethodsModified Hummer's method was used to synthesize graphene oxides by using various levels of H2SO4, KMnO4, and H2O2 and 3D graphene aerogels were synthesized via the hydrothermal and freeze-drying method. FTIR, RAMAN, XRD, FE-SEM, and BET analysis were used for characterizations. Significance findingsThe effect of graphite oxidation conditions on the hierarchical porous structure of graphene aerogel for CO2 adsorption was investigated. The graphene aerogel with the high meso and micro surface areas and the highest Sm/ST value (micro surface area/total micro and meso surface area) of 33% and also, the adequate macropores was achieved using high dosage of H2SO4 in the graphene oxidation process led to the highest CO2 adsorption capacity of 1.72 mmol/g. increasing the H2O2 dosages increased the macropores in the aerogel structure and improved the value of Sm/ST leading to an increase in the CO2 adsorption capacity. The high content of KMnO4 led to low Sm/ST value and fewer macropores and decreased the CO2 adsorption capacity (1.04 mmol/g).

Confined CO in a sandwich structure promotes C-C coupling in electrocatalytic CO2 reduction.

Microenvironment regulation near the catalyst surface plays a critical role in heterogeneous electrocatalytic reactions. The local concentration of reactants and intermediates significantly affects the reaction kinetics and product selectivity. Herein, we propose an innovative strategy of utilizing the spatial confinement effect in a sandwich-structured C/Cu/C assembly to regulate kinetic mass transport during the electrocatalytic CO2 reduction reaction. The sandwich C/Cu/C assembly catalyst was successfully prepared using a simple bidirectional freezing and freeze-drying method. The sandwich structure changes the free diffusion pathway of the CO intermediate within the sandwich interlayer and helps confine CO with locally increased CO concentration near the catalyst surface, which in turn promotes C-C coupling and thus improves the reaction activity and doubles the C2 product selectivity compared to its disordered mixture counterpart. This kinetics regulation in the sandwich structure may provide a new insight into the catalyst design and inspire the understanding of the structure-performance relationship in electrocatalysis.

THE EFFECT OF DIFFERENT DRYING TECHNIQUES ON SOME BIOACTIVE COMPOUNDS AND ANTIBACTERIAL PROPERTIES OF Polygonum sivasicum

Turkey has several endemic edible plant species having health benefits. Polygonum sivasicum is widely consumed as fresh or dried throughout the year by rural people in Sivas province. This study aimed to reveal the health benefits of P. sivasicum and to assess the effects of different drying methods on nutritional, phytochemical, and biological activities. P. sivasicum leaves were collected from Sivas province and dried freeze, oven, microwave, and shade treatments. For each sample, total phenolic content and profile, antioxidant activity, mineral analysis and antibacterial properties were investigated. The highest phenolic content and antioxidant activity were observed in freeze-dried samples (p<0.05). Rutin was detected as a major phenolic compound, followed by chlorogenic acid, kaempferol-3-O-glucoside, isorhamnetin-3-O-glucoside, ferulic acid, luteolin, and caffeic acid, respectively. The P. sivasicum leaves seem to be rich in potassium, phosphorus, and magnessium. P. sivasicum extracts showed antimicrobial activity against S. aureus and L. innocua depending on the extraction solvent. Freeze-drying methods can be used as a convenient drying method due to preserve the total phenolic content and individual phenolic compounds.

Improved antimicrobial activities of Boswellia sacra essential oils nanoencapsulated into hydroxypropyl-beta-cyclodextrins.

Natural antimicrobials have recently gained increasing interest over synthetic antimicrobials to overcome foodborne pathogens and food microbial contamination. Essential oils (EOs) obtained from Boswellia sacra resins (BO) were utilized for respiratory disorders, rheumatoid arthritis, malignant tumors, and viral infections. Like other EOs, the therapeutic potential of BO is hindered by its low solubility and bioavailability, poor stability, and high volatility. Several studies have shown excellent physicochemical properties and outstanding therapeutic capabilities of EOs encapsulated into various nanocarriers. This study extracted BO from B. sacra resins via hydrodistillation and encapsulated it into hydroxypropyl-beta-cyclodextrins (HPβCD) using the freeze-drying method. The developed inclusion complexes of BO (BO-ICs) had high encapsulation efficiency (96.79 ± 1.17%) and a polydispersity index of 0.1045 ± 0.0006. BO-ICs showed presumably spherical vesicles (38.5 to 59.9 nm) forming multiple agglomerations (136.9 to 336.8 nm), as determined by UHR-TEM. Also, the formation and stability of BO-ICs were investigated using DSC, FTIR, FE-SEM, UHR-TEM, 1H NMR, and 2D HNMR (NOESY). BO-ICs showed greater thermal stability (362.7 °C). Moreover, compared to free BO, a remarkable enhancement in the antimicrobial activities of BO-ICs was shown against three different bacteria: Escherichia coli, Staphylococcus aureus, and Pseudomonas aeruginosa. BO-ICs displayed significant antibacterial activity against Pseudomonas aeruginosa with an MIC90 of 3.93 mg mL-1 and an MIC50 of 0.57 mg mL-1. Also, BO-ICs showed an increase in BO activity against Escherichia coli with an MIC95 of 3.97 mg mL-1, compared to free BO, which failed to show an MIC95. Additionally, BO-ICs showed a more significant activity against Staphylococcus aureus with an MIC95 of 3.92 mg mL-1. BO encapsulation showed significantly improved antimicrobial activities owing to the better stability, bioavailability, and penetration ability imparted by encapsulation into HPβCD.

Inclusion complex of berberine hydrochloride with serine-β-cyclodextrin: construction, characterization, inclusion mechanisms, and bioactivity

Ser-β-CD was synthesized and a BBH/Ser-β-CD IC was prepared via the freeze-drying method. Ser-β-CD and IC show good biocompatibility. The IC exhibits sustained BBH release efficiency and excellent antibacterial activity against E. coli and S. aureus.

Biological activity of lyophilized chitosan scaffolds with inclusion of chitosan and zinc oxide nanoparticles.

The constant demand for biocompatible and non-invasive materials for regenerative medicine in accidents and various diseases has driven the development of innovative biomaterials that promote biomedical applications. In this context, using sol-gel and ionotropic gelation methods, zinc oxide nanoparticles (NPs-ZnO) and chitosan nanoparticles (NPs-CS) were synthesized with sizes of 20.0 nm and 11.98 nm, respectively. These nanoparticles were incorporated into chitosan scaffolds through the freeze-drying method, generating a porous morphology with small (<100 μm), medium (100-200 μm), and large (200-450 μm) pore sizes. Moreover, the four formulations showed preliminary bioactivity after hydrolytic degradation, facilitating the formation of a hydroxyapatite (HA) layer on the scaffold surface, as evidenced by the presence of Ca (4%) and P (5.1%) during hydrolytic degradation. The scaffolds exhibited average antibacterial activity of F1 = 92.93%, F2 = 99.90%, F3 = 74.10%, and F4 = 88.72% against four bacterial strains: K. pneumoniae, E. cloacae, S. enterica, and S. aureus. In vivo, evaluation confirmed the biocompatibility of the functionalized scaffolds, where F2 showed accelerated resorption attributed to the NPs-ZnO. At the same time, F3 exhibited controlled degradation with NPs-CS acting as initiation points for degradation. On the other hand, F4 combined NPs-CS and NPs-ZnO, resulting in progressive degradation, reduced inflammation, and an organized extracellular matrix. All the results presented expand the boundaries in tissue engineering and regenerative medicine by highlighting the crucial role of nanoparticles in optimizing scaffold properties.

Interactions of Cyclodextrins and their Hydroxyl Derivatives with Etodolac: Solubility and Dissolution Enhancement.

Poor solubility and dissolution rate of drugs are largely responsible for erratic drug absorption and limited oral bioavailability. Etodolac (ETO) is a non-steroidal anti-inflammatory drug (NSAID) that is classified as BCS class II (dissolution rate-dependent absorption). ETO has high safety and efficacy in pain relief and control of inflammation. ETO is commercially available as (400- 600 mg) tablets; poor solubility and dissolution rate of ETO could result in variable oral absorption and inconsistent analgesic responses. The aim of this study was to improve solubility and dissolution rates of ETO by complexation with cyclodextrins (CDs). Four different CDs namely β-, γ-, HP β-CDs, and HP γ-CDs were prepared using three different methods; solvent evaporation (CO), freeze-drying (FD), and physical mixing (PM). The prepared drug: excipient mixtures were investigated for aqueous solubility, as well as via</i> DSC, XRD, FTIR, SEM, dissolution, and docking. The results revealed a solubility phase diagram of the AL type, indicating a 1:1 complexation of ETO: CD. These results agreed with our molecular docking calculations. DSC, FTIR, XRD, and SEM results confirmed the formation of an inclusion complex. The complexation efficiency, solubility, and dissolution enhancement were in the order of HPγ-CD > γ -CD > HPβ-CD > β-CD. FD method was superior to both CO and PM. Superior dissolution enhancements of ETO were recorded for the FD mixture (up to 90% dissolved in less than 10 min). In conclusion, γ- and hydroxypropyl γ-derivative of cyclodextrins can be considered a promising excipient for enhancement of dissolution rates concerned for ETO.