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At least 19 records

Excipient screening by lyophilization provides insights into spray drying formulations for nanoparticle vaccines

Nanoparticles have shown great promise as delivery platforms in the development of tunable and safe vaccines. Nanolipoprotein particles (NLPs), also known as nanodiscs, are discoidal nanoparticles composed of a lipid bilayer stabilized at their periphery by apolipoproteins. Under the right conditions, the NLP self-assembly process is highly customizable in terms of lipids and apolipoprotein constituents, allowing for tunable physical and chemical characteristics. This flexibility allows a wide range of vaccine antigens and adjuvants to be incorporated onto the NLP platform for tailored vaccine design. The stability of NLPs during long term storage is a very important factor in developing a vaccine delivery platform suitable for widespread global use. When stored in a solution for extended periods of time, NLPs dissociate into their corresponding lipids and protein constituents, leading to particle degradation. Proper stabilization of NLPs can often be achieved by lyophilization (i.e. freeze-drying), a method widely used for various applications including pharmaceuticals. This process, however, can be damaging to particles without the presence of lyoprotectants or excipients that help maintain particle stability during lyophilization. Another method used to stabilize vaccines and pharmaceuticals is spray drying, a process that converts liquid formulations into dry powders through controlled heating and airflow. While spray drying is rapid, scalable, and cost-effective, lyophilization is typically a gentler process that better retains biomolecule structure and function. Both processes use excipients for particle stabilization, so lyophilization can be used as a surrogate to test stability of NLPs, to down-select formulations that may withstand the harsher conditions of spray drying. To screen different formulations, NLPs were synthesized and purified to homogeneity by size exclusion chromatography (SEC) and samples were prepared with a wide range of lyoprotectants and/or excipients. To assess the protective effects of excipients on NLPs upon spray drying, both pre- and post-lyophilized samples were analyzed by SEC. To assess the protective effects upon heating (encountered during the spray drying process), NLP samples were incubated at elevated temperatures prior to SEC analysis. The lyoprotectants and excipients evaluated in this study had different efficiencies in protecting NLPs during lyophilization and heating tests. Trehalose, for example, exhibits stabilization on NLPs both upon lyophilization and heating whereas leucine accelerated NLP dissociation. Although some lyoprotectants are effective by themselves, different combinations can decrease the stabilization of NLPs. Shelf-stable vaccines that do not require cold-chain storage are essential for global accessibility and our findings provide fundamental insight into how to advance NLP-based vaccines for these applications.

Serrano, Litzay J [Lawrence Livermore National Lab↗

Lyophilization of ASFV vaccine candidate ASFV-G-ΔI177L offers long term stability

Abstract For over a century African swine fever (ASF) has been causing outbreaks leading to devastating losses for the swine industry. The current pandemic of ASF has shown no signs of stopping and continues to spread causing outbreaks in additional countries. Currently control relies mostly on culling infected farms, and strict biosecurity procedures. Recently a vaccine, ASFV-G-ΔI177L was approved for use in Vietnam. In this study we evaluate the long-term stability of lyophilized ASFV-G-ΔI177L. Understanding the stability of different formulations of vaccines is information necessary for deployment of vaccines to ASF outbreak areas, particularly those that do not have a reliable well established cold chain to ensure conservation of vaccine quality. In this report, we determined that ASFV-G-ΔI177L, when lyophilized under specific conditions, is stable for up to one year at 4 °C, with similar vaccine titers after storage. Next-generation sequencing analysis also determined that lyophilization and long-term storage under these conditions had no effect on the genome of ASFV as the genome remained genetically identical to the original non-lyophilized form.

Science & Technology - Other Topics↗

Stability and biocompatibility of photothermal gold nanorods after lyophilization and sterilization

Graphical abstract: - Highlights: • Morphological changes are observed for CTABr capped gold nanorods over time. • Polystyrenesulfonate (PSS) and polyethyleneglycol (PEG) coated nanorods are stable. • Re-suspendible and sterilizable colloids are prepared using those capping agents. • Those materials are efficient heat sinks potentially used in photothermal therapy. - Abstract: Suspensions in phosphate buffered saline (PBS) of gold nanorods stabilized with cetyltrimethyl ammonium chloride (CTABr), polystyrenesulfonate (PSS) and methyl-polyethyleneglycol-thiol (m-PEG-SH) have been prepared and the evolution of their colloidal stability and plasmonic response over time has been evaluated. Their performance after lyophilization, alcoholic sterilization and resuspension has also been characterized. Sub-cytotoxic doses on HeLa cells were calculated for the three surface functionalizations used. Their heating efficiency at different exposure times was also evaluated after being irradiated with near infrared light. The best results were obtained for m-PEG-SH stabilized rods, which were not only stable, sterilizable and lyophilizable, but also biocompatible at all doses tested, showing potential as a stable, re-suspendible and biocompatible hyperthermic agent.

36 MATERIALS SCIENCE↗

Combustion water purification techniques influence on OBT analysing using liquid scintillation counting method

In order to determine organically bound tritium (OBT) from environmental samples, these must be converted into water, measurable by liquid scintillation counting (LSC). For this purpose we conducted some experiments to determine OBT level of a grass sample collected from an uncontaminated area. The studied grass sample was combusted in a Parr bomb. However usual interfering phenomena were identified: color or chemical quench, chemiluminescence, overlap over tritium spectrum because of other radionuclides presence as impurities ({sup 14}C from organically compounds, {sup 36}Cl as chloride and free chlorine, {sup 40}K as potassium cations) and emulsion separation. So the purification of the combustion water before scintillation counting appeared to be essential. 5 purification methods were tested: distillation with chemical treatment (Na{sub 2}O{sub 2} and KMnO{sub 4}), lyophilization, chemical treatment (Na{sub 2}O{sub 2} and KMnO{sub 4}) followed by lyophilization, azeotropic distillation with toluene and treatment with a volcanic tuff followed by lyophilization. After the purification step each sample was measured and the OBT measured concentration, together with physico-chemical analysis of the water analyzed, revealed that the most efficient method applied for purification of the combustion water was the method using chemical treatment followed by lyophilization.

54 ENVIRONMENTAL SCIENCES↗

Effect of Storage Conditions on the Integrity of Human Umbilical Cord Mesenchymal Stromal Cell-Derived Microvesicles

We studied the effect of storage conditions on the safety of microvesicles produced by human multipotent umbilical cord mesenchymal stromal cells into the conditioned medium. It was found that microvesicles can be stored without serious degradation for up to 1 week at 4°С, but were almost completely destroyed during freezing and thawing cycles irrespective of the storage temperatures (-20°С, -70°С, or -196°С). Similar results were obtained for lyophilized medium conditioned by human multipotent umbilical cord mesenchymal stromal cells. Addition of a cryoprotectant (5-10% DMSO) followed by freezing and/or lyophilization preserved microvesicles at a nearly initial level. These findings indicate that during storage, microvesicles, being membrane structures, behave similar to living cells and require appropriate conditions for prolonged storage.

60 APPLIED LIFE SCIENCES↗

Wetting properties of molecularly rough surfaces

We employ molecular dynamics simulations to study the wettability of nanoscale rough surfaces in systems governed by Lennard-Jones (LJ) interactions. We consider both smooth and molecularly rough planar surfaces. Solid substrates are modeled as a static collection of LJ particles arranged in a face-centered cubic lattice with the (100) surface exposed to the LJ fluid. Molecularly rough solid surfaces are prepared by removing several strips of LJ atoms from the external layers of the substrate, i.e., forming parallel nanogrooves on the surface. We vary the solid-fluid interactions to investigate strongly and weakly wettable surfaces. We determine the wetting properties by measuring the equilibrium droplet profiles that are in turn used to evaluate the contact angles. Macroscopic arguments, such as those leading to Wenzel’s law, suggest that surface roughness always amplifies the wetting properties of a lyophilic surface. However, our results indicate the opposite effect from roughness for microscopically corrugated surfaces, i.e., surface roughness deteriorates the substrate wettability. Adding the roughness to a strongly wettable surface shrinks the surface area wet with the liquid, and it either increases or only marginally affects the contact angle, depending on the degree of liquid adsorption into the nanogrooves. For a weakly wettable surface, the roughness changes the surface character from lyophilic to lyophobic due to a weakening of the solid-fluid interactions by the presence of the nanogrooves and the weaker adsorption of the liquid into the nanogrooves.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Investigating the quaternary structure of a homomultimeric catechol 1,2-dioxygenase: An integrative structural biology study

The structural analysis of catechol 1,2 dioxygenase from Stutzerimonas frequens GOM2, SfC12DO, was conducted using various structural techniques. SEC-SAXS experiments revealed that SfC12DO, after lyophilization and reconstitution processes, can form multiple enzymatically active oligomers, including dimers, tetramers, and octamers. These findings differ from previous studies, which reported active dimers in homologous counterparts with available crystallographic structures, or trimers observed exclusively in solution for SfC12DO and its homologous isoA C12DO from Acinetobacter radioresistens under low ionic strength conditions. In some cases, tetramers were also reported, such as for the Rodococcus erythropolis C12DO. The combined results of Small-Angle X-ray Scattering, Dynamic Light Scattering, and Transmission Electron Microscopy experiments provided additional insights into these active oligomers’ shape and molecular organization in an aqueous solution. These results highlight the oligomeric structural plasticity of SfC12DO, proving that it can exist in different oligomeric forms depending on the physicochemical characteristics of the solutions in which the experiments were performed. Remarkably, regardless of its oligomeric state, SfC12DO maintains its enzymatic activity even after prior lyophilization. All these characteristics make SfC12DO a putative candidate for bioremediation applications in polluted soils or waters.

59 BASIC BIOLOGICAL SCIENCES↗

Effective Adsorption of Cr(VI) by High Strength Chitosan/Montmorillonite Composite Hydrogels Involving Spirulina Biomass/Microalgae

The “3-in-1 type” biopolymer composite (chitosan/montmorillonite clay/biosorbent) hydrogels were produced and used as adsorbents for Cr(VI) ion. Na-Montmorillonite (NaMMT) clay was modified with Spirulina (Sp) biosorbent by using lyophilization based “cryoscopic expansion” (C-XP) method. The Sp immobilized MMT (SpMMT) clay containing hydrogels were found to have an open/extended form of Sp structure on their pores’ walls, presenting all possible receptor groups for adsorption of Cr(VI) ions. SpMMT loaded hydrogels showed higher adsorption capacities than NaMMT loaded ones. The physically crosslinked hydrogel including only 1% SpMMT (1SpM-H) clay exhibited 150% higher adsorption capacity as compared to neat chitosan hydrogel even in 50 ppm Cr(VI) solution. The same composite hydrogel was found to adsorp about 780% Cr(VI) with respect to the clay’s weight while individual uses of Sp and MMT can remove only about 4.80 and 0.36% Cr(VI) with respect to their weights. The pseudo-first order model was found to be the most suitable for the kinetic data of NaMMT loaded hydrogels while that of SpMMT containing hydrogels followed the pseudo-second order kinetics. The isotherm data of all the hydrogels exhibited a better fit to the Freundlich and Sips model. The maximum adsorption capacity (3333 mg g{sup −1}) calculated by Sips model was achieved via the hydrogel having 1% SpMMT which is in good agreement with the experimental kinetic data. The highest adsorption with the lowest amount of SpMMT clay could be attributed to its looser Sp network structure whose functional groups are in long-distance, releasing more adsorption sites for the Cr(VI). The highest compression modulus and toughness were also obtained with the 1SpM-H hydrogel which is probably due to increased physical and reversible interactions between chitosan molecules and SpMMT clay layers at optimum clay loading (1%).

60 APPLIED LIFE SCIENCES↗

An All Hydrophilic Fluid Diode for Unidirectional Flow in Porous Systems

Abstract A fluid diode that allows fluid flow in one direction but blocks fluid flow in the opposite direction has wide applications including oil recovery, drug delivery, and lab‐on‐a‐chip microfluidics. Many studies are conducted to facilitate directional liquid motion on the solid surface or across thin porous layers. However, the self‐driven one‐way flow inside porous systems still remains a significant challenge. Here, a novel all‐hydrophilic fluid diode (AHFD) made of porous materials with asymmetric pores is reported, which allows capillary flow in a chosen direction. The direction‐dependent flow process and the breakthrough pressure are experimentally and theoretically examined. The proposed AHFD can have many potential applications such as functional protective clothing, microfluidic valve, and oil–water separator, and the idea can be extended to develop other all lyophilic fluid diodes such as oleophilic diode.

Shou, Dahua↗

Preparation of Chitin Nanofiber-Reinforced Xanthan Gum Hydrogels

In this study, chitin was nanofibrillated, cationized, and then used as a reinforcing agent for xanthan gum hydrogels. Amidinated chitin nanofibers (CNFs), which were prepared by partial deacetylation of the nanofibrillated chitin and the subsequent reaction of the generated amino groups with N,N-dimethylacetamide dimethyl acetal, were converted into an amidinium chitin bicarbonate with nanofiber morphology by CO{sub 2} gas bubbling and ultrasonic treatments in water. Xanthan gum hydrogels, which were prepared by exchange of disperse media from xantham gum ion gels with 1-butyl-3-methylimidazolium chloride, were then soaked in the resulting cationic CNF aqueous dispersions with different degrees of substitution (DSs) of amidinium groups to progress composition, giving rise to the CNF-reinforced xanthan gum hydrogels. The presence of CNFs in the hydrogels was confirmed by SEM measurement of the lyophilized samples. The amounts of CNFs in the hydrogels increased with increasing the DS values. The compression testing of the hydrogels suggested the reinforcing effect of CNFs, which were induced by electrostatic interaction owing to anionic nature of xanthan gum.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Crystallization of Trehalose in Frozen Solutions and its Phase Behavior during Drying

To study the crystallization of trehalose in frozen solutions and to understand the phase transitions during the entire freeze-drying cycle. Aqueous trehalose solution was cooled to -40 C in a custom-designed sample holder. The frozen solution was warmed to -18 C and annealed, and then dried in the sample chamber of the diffractometer. XRD patterns were continuously collected during cooling, annealing and drying. After cooling, hexagonal ice was the only crystalline phase observed. However, upon annealing, crystallization of trehalose dihydrate was evident. Seeding the frozen solution accelerated the solute crystallization. Thus, phase separation of the lyoprotectant was observed in frozen solutions. During drying, dehydration of trehalose dihydrate yielded a substantially amorphous anhydrous trehalose. Crystallization of trehalose, as trehalose dihydrate, was observed in frozen solutions. The dehydration of the crystalline trehalose dihydrate to substantially amorphous anhydrate occurred during drying. Therefore, analyzing the final lyophile will not reveal crystallization of the lyoprotectant during freeze-drying. The lyoprotectant crystallization can only become evident by continuous monitoring of the system during the entire freeze-drying cycle. In light of the phase separation of trehalose in frozen solutions, its ability to serve as a lyoprotectant warrants further investigation.

99 GENERAL AND MISCELLANEOUS↗

Trends in Light and Temperature Sensitivity Recommendations among Licensed Biotechnology Drug Products

Inherent structural and functional properties of biotechnology-derived therapeutic biologics make them susceptible to light- and temperature-induced degradation and consequently can influence their quality. Photosensitivity of therapeutic proteins continues to be examined, but the commonalities and trends of storage conditions and information about light and temperature sensitivity among currently licensed therapeutic proteins has not been previously surveyed. Using a comprehensive and relational database approach, we conducted a scientific survey of all licensed biotechnology-derived drug products with the goal of providing evidence-based information about recommended storage conditions of formulations sorted by light- and temperature-related attributes as described for each product at licensure. We report the prevalence of indications for light and temperature sensitivity in formulations categorized by their presentation type, number of doses, container type, dosage form and active molecule type. We also report the storage temperature range across formulations and diluents for reconstitution and dilution. Formulations with excipients that potentially facilitate light-induced and thermal degradation were also noted. The result of our analysis indicates that light and temperature sensitivity are prevalent across therapeutic protein formulations. However, when a formulation is reconstituted or diluted, both light and temperature sensitivity are less clear. In addition, light and temperature sensitivity are more well defined in liquid formulations than lyophilized powder formulations, and more well defined in products manufactured in autoinjectors, prefilled-syringes, and pens than products in vials. Overall, our report provides a data-driven summary of storage conditions among therapeutic protein formulations to support the development of future biologic drug products.

60 APPLIED LIFE SCIENCES↗

Cross-linked poly(methyl vinyl ether-co-maleic acid)/poly(ethylene glycol)/nanocellulosics foams via directional freezing

Aligned micro- and nanoporous materials have gained tremendous interest since they demonstrate great potential in organic electronics, absorbents, biomedicine and tissue engineering. Herein, cellulose nanofibrils (CNFs) and cellulose nanocrystals (CNCs) cross-linked with poly(methyl vinyl ether-co-maleic acid) (PMVEMA) and poly(ethylene glycol) (PEG) foams were prepared by both the directional and un-directional freezing techniques. Aligned three-dimensional porous structures were indicated for the directional frozen foams after lyophilization via scanning electron microscope (SEM). As a result, these highly organized structures exhibited enhanced mechanical performance properties. Particularly, for the 25% CNF foams, the compression modulus increased 60% compared with the un-directional frozen samples. These nanocellulosics-based foams could absorb up to 10-fold water of their initial weight with excellent water stability when immersed in water for more than 48 h. Overall, this study describes a novel process combining cross-linking and directional freezing which successfully fabricates naturally derived foams with anisotropic structure.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗