Comparison between freeze and spray drying to obtain powder Rubrivivax gelatinosus biomass

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

The potential for production of freeze-dried oral vaccines using alginate hydrogel microspheres as protein carriers

Oral administration of dry vaccine formulations is acknowledged to offer major clinical and logistical benefits by eliminating the cold chain required for liquid preparations. A model antigen, bovine serum albumin (BSA) was encapsulated in alginate microspheres using aerosolisation. Hydrated microspheres 25 to 65 μm in size with protein loading of 3.3 % w/w were obtained. Environmental scanning electron microscopy indicated a stabilizing effect of encapsulated protein on alginate hydrogels revealed by an increase in dehydration resistance. Freeze drying of alginate microspheres without use of a cryoprotectant resulted in fragmentation and subsequent rapid loss of the majority of the protein load in simulated intestinal fluid in 2 h, whereas intact microspheres were observed following freeze-drying of BSA-loaded microspheres in the presence of maltodextrin. BSA release from freeze-dried preparations was limited to less than 7 % in simulated gastric fluid over 2 h, while 90 % of the protein load was gradually released in simulated intestinal fluid over 10 h. SDS-PAGE analysis indicated that released BSA largely preserved its molecular weight. These findings demonstrate the potential for manufacturing freeze-dried oral vaccines using alginate microspheres.

Effect of drying, storage temperature and air exposure on astaxanthin stability from Haematococcus pluvialis

Astaxanthin is a powerful antioxidant with various health benefits such as prevention of age-related macular degeneration and improvement of the immune system, liver and heart function. To improve the post-harvesting stability of astaxanthin used in food, feed and nutraceutical industries, the biomass of the high astaxanthin producing alga Haematococcus pluvialis was dried by spray- or freeze-drying and under vacuum or air at − 20 °C to 37 °C for 20 weeks. Freeze-drying led to 41 higher astaxanthin recovery compared to commonly-used spray-drying. Low storage temperature (− 20 °C, 4 °C) and vacuum-packing also showed higher astaxanthin stability with as little as 12.3 ± 3.1 degradation during 20 weeks of storage. Cost-benefit analysis showed that freeze-drying followed by vacuum-packed storage at − 20 °C can generate AUD600 higher profit compared to spray-drying from 100 kg H. pluvialis powder. Therefore, freeze-drying can be suggested as a mild and more profitable method for ensuring longer shelf life of astaxanthin from H. pluvialis.

Effect of cooking and drying on carbonyls of oil sardine

Changes in the total as well as major individual carbonyls of oil sardine during steam cooking, oven drying, sun drying and freeze drying are presented. Carbonyls extracted with hexane were converted to their 2:4 dinitro phenyl hydrazone (DNPH) derivatives and were separated into major classes by column chromatography on celite/magnesia. Individual carbonyls were then identified by capillary gas chromatography of the DNPH derivatives. Dehydration and heating increase the carbonyl production from highly unsaturated fish lipids. The carbonyls produced react with other muscle constituents leading to complex changes. The influence of the mode of dehydration on these different aspects and their net effect on flavour are discussed.

Characterisation of freeze-dried wafers and solvent evaporated films as potential drug delivery systems to mucosal surfaces

Freeze-dried (lyophilised) wafers and solvent cast films from sodium alginate (ALG) and sodium carboxymethylcellulose (CMC) have been developed as potential drug delivery systems for mucosal surfaces including wounds. The wafers (ALG, CMC) and films (CMC) were prepared by freeze-drying and drying in air (solvent evaporation) respectively, aqueous gels of the polymers containing paracetamol as a model drug. Microscopic architecture was examined using scanning electron microscopy, hydration characteristics with confocal laser scanning microscopy and dynamic vapour sorption. Texture analysis was employed to investigate mechanical characteristics of the wafers during compression. Differential scanning calorimetry was used to investigate polymorphic changes of paracetamol occurring during formulation of the wafers and films. The porous freeze-dried wafers exhibited higher drug loading and water absorption capacity than the corresponding solvent evaporated films. Moisture absorption, ease of hydration and mechanical behaviour were affected by the polymer and drug concentration. Two polymorphs of paracetamol were observed in the wafers and films, due to partial conversion of the original monoclinic to the orthorhombic polymorph during the formulation process. The results showed the potential of employing the freeze-dried wafers and solvent evaporated films in diverse mucosal applications due to their ease of hydration and based on different physical mechanical properties exhibited by both type of formulations.

In vitro drug release studies of polymeric freeze-dried wafers and solvent-cast films using paracetamol as a model soluble drug

Drug dissolution and release characteristics from freeze-dried wafers and solvent-cast films prepared from sodium carboxymethylcellulose (CMC) have been investigated to determine the mechanisms of drug release from the two systems. The formulations were prepared by freeze-drying (wafers) or drying in air (films), the hydrated gel of the polymer containing paracetamol as a model soluble drug. Scanning electron microscopy (SEM) was used to examine differences between the physical structure of the wafers and films. Dissolution studies were performed using an exchange cell and drug release was measured by UV spectroscopy at 242 nm. The effects of drug loading, polymer content and amount of glycerol (films) on the release characteristics of paracetamol were investigated. The release profiles of paracetamol from the wafers and films were also compared. A digital camera was used to observe the times to complete hydration and dissolution of the wafers containing different amounts of CMC and how that impacts on drug release rates. Both formulations showed sustained type drug release that was modelled by the Korsmeyer–Peppas equation. Changes in the concentration of drug and glycerol (films) did not significantly alter the rate of drug release while increasing polymer content significantly decreased the rate of drug release from both formulations. The results show that the rate of paracetamol release was faster from the wafers than the corresponding films due to differences in their physical structures. The wafers which formed a porous network, hydrated faster than the more dense and continuous, (non-porous) sheet-like structure of the films.

Effect of composition, solvent exchange liquid and drying method on the porous structure of phenol-formaldehyde gels

Organic gels have been synthesized by sol–gel polycondensation of phenol (P) and formaldehyde (F) catalyzed by sodium carbonate (C). The effect of synthesis parameters such as phenol/catalyst ratio (P/C), solvent exchange liquid and drying method, on the porous structure of the gels have been investigated. The total and mesopore volumes of the PF gels increased with increasing P/C ratio in the range of P/C B 8, after this both properties started to decrease with P/C ratio for P/C[8 and the gel with P/C = 8 showed the highest total and mesopore volumes of 1.281 and 1.279 cm3 g-1 respectively. The gels prepared by freeze drying possessed significantly higher porosities than the vacuum dried gels. The pore volume and average pore diameter of the freeze dried gels were significantly higher than those of the vacuum dried gels. T-butanol emerged as the preferred solvent for the removal of water from the PF hydrogel prior to drying, as significantly higher pore volumes and specific surface areas were obtained in the corresponding dried gels. The results showed that freeze drying with t-butanol and lower P/C ratios were favourable conditions for the synthesis of highly mesoporous phenol–formaldehyde gels.

Development of liposome-based freeze-dried rods for vaginal vaccine delivery against HIV-1

The present investigation deals with development and characteriza- tion of the liposomes-based freeze-dried rods for the vaginal delivery of gp140 antigen in mice. Positively charged, negatively charged and neutral liposomes were prepared and characterized for various parameters e.g. morphology, size, polydispersity index, zeta potential and antigen encapsulation efficiency. To further improve the efficacy of vaccine delivery, antigen encapsulated liposomes were formulated as polymer gel-based freeze-dried rods, which were then characterized for moisture content. The redispersibility of the liposomes-based freeze- dried rods was determined in simulated vaginal fluid and liposome gel was investigated for mucoadhesion. The developed liposome-based freeze-dried rods systems could offer potential as stable and practical dosage form for the mucosal immunization against HIV-1 infection.

Freeze-dried strawberry powder improves lipid profile and lipid peroxidation in women with metabolic syndrome:baseline and post intervention effects

Strawberry flavonoids are potent antioxidants and anti-inflammatory agents that have been shown to reduce cardiovascular disease risk factors in prospective cohort studies. Effects of strawberry supplementation on metabolic risk factors have not been studied in obese populations. We tested the hypothesis that freeze-dried strawberry powder (FSP) will lower fasting lipids and biomarkers of oxidative stress and inflammation at four weeks compared to baseline. We also tested the tolerability and safety of FSP in subjects with metabolic syndrome. FSP is a concentrated source of polyphenolic flavonoids, fiber and phytosterols.

Effect of drying methods on the phenolic constituents of meadowsweet (Filipendula ulmaria) and willow (Salix alba)

The objective of this study was to investigate the effect of drying conditions on the phenolic constituents and colour of extracts of organically grown white willow and meadowsweet for incorporation into a functional beverage with potential anti-inflammatory properties. The herbs were freeze-dried, air-dried, oven or tray-dried at 30 or 70 °C. The drying kinetics of the herbs was first determined. Both drying temperature and method had a significant effect (p ≤ 0.05) on the drying rate, the samples tray-dried had a faster drying rate than those oven-dried. Results show that for meadowsweet and willow, freeze-drying and oven or tray drying at 30 °C had no significant effect on the phenolic constituents (e.g. total phenols, salicylates, quercetin) or the colour of the extracts in comparison to traditional air-drying. Although increasing the drying temperature to 70 °C resulted in an increase in the drying rate of both herbs it also led to the loss of some phenolic compounds. Also, the extracts from both herbs dried at 70 °C were significantly (p ≤ 0.05) redder than the other drying methods. Therefore, tray drying these herbs at low temperatures may reduce drying time without having a significant effect on the phenolic content and colour of the extracts.

EFFECT OF DRYING METHODS ON THE THERMODYNAMIC PROPERTIES OF BLACKBERRY PULP POWDER

Three different types of maltodextrin encapsulated dehydrated blackberry fruit powders were obtained using vibrofluidized bed drying (VF), spray drying (SD), vacuum drying (VD), and freeze drying (FD). Moisture equilibrium data of blackberry pulp powders with 18% maltodextrin were determined at 20, 30, 40, and 50 degrees C using the static gravimetric method for the water activity range of 0.06-0.90. Experimental equilibrium moisture content data versus water activity were fit to the Guggenheim-Anderson-de Boer (GAB) model. Agreement was found between experimental and calculated values. The isosteric heat of sorption of water was determined using the Clausius-Clapeyron equation from the equilibrium data; isosteric heats of sorption were found to increase with increasing temperature and could be adjusted by an exponential relationship. For freeze dried, vibrofluidized, and vacuum dried pulp powder samples, the isosteric heats of sorption were lower (more negative) than those calculated for spray dried samples. The enthalpy-entropy compensation theory was applied to sorption isotherms and plots of Delta H versus Delta S provided the isokinetic temperatures, indicating an enthalpy-controlled sorption process.

Fatty acid and sterol composition of frozen and freeze-dried New Zealand green lipped mussel (Perna canaliculus) from three sites in New Zealand

In view of previously reported anti-inflammatory bioactivity of the New Zealand Green Lipped Mussel (NZGLM), the overall lipid profile and fatty acid and sterol composition of the NZGLM from various sites in New Zealand (Hallam Cove, Port Ligar, Little Nikau) were investigated using thin layer  chromatography (TLC) and gas liquid chromatography (GLC). Samples were either frozen (F) or freeze-dried (FD) soon after collection. It was also thought prior to the study, there may be differences in the dietary sources of phytoplankton between the sites, responsible for the bioactivity, however data collected in New Zealand reported no difference in the type of phytoplankton, but a difference in the quantity. There were no major significant differences in the major components of the lipid, fatty acid and sterol composition between FD or frozen samples, nor were there any significant differences in the major composition between sites. The only major difference was between total lipid composition of the freeze-dried and frozen samples due to the removal of water during freeze-drying. Total lipid content on a dry weight basis in FD samples was 8.4 g/100g tissue and was significantly higher than frozen samples (P < 0.05) and there was no significant site variation. The lipid class content between sites was also not significantly different as judged by TLC. Triglyceride (TG) lipid fraction appeared to be the most prominent in the frozen and FD samples. The free fatty acid (FFA) band was the next most prominent band and was visually more prominent in the frozen samples. Sterol esters (SE) were detected in higher amounts in the frozen samples compared with the FD samples. Phospholipid (PL) and sterols (ST) were distributed throughout all samples. Polyunsaturated fatty acids (PUFA) were the main group of fatty acids in both FD and frozen samples (45-46%), most of which were omega-3 (n-3) fatty acids (40-41%). Saturated fatty acids (SFA) accounted for approximately one quarter of total fatty acids, with little variation between FD and frozen samples. The major fatty acids of the NZGLM were docosahexaenoic acid (DHA; 22:6n-3) (19% in both FD and frozen samples), eicosapentaenoic acid (EPA; 20:5n-3) and palmitic acid (16:0) (15% in both FD and frozen samples). Cholesterol was the most prominent sterol (31% of total sterols). Other major sterols included desmosterol/ brassicasterol (co-eluting), 24-methylenecholesterol, trans-22-dehydrocholesterol, 24- nordehydrocholesterol and occelasterol. This study is unique as it compares the lipid composition of the NZGLM from three sites in New Zealand with the additional effect of processing. This is the second comparative study investigating the lipid, fatty acid and sterol composition of the NZGLM with added interest in the effect of freeze drying on the lipid content of the mussel. This study showed that there were no major significant differences in lipid, sterol and fatty acid composition between the FD and frozen samples of the NZGLM for three sites in New Zealand. Food chain studies and further research is warranted to investigate the presence and role of major and minor lipid.
components of the NZGLM.

Fabrication of carbon nanofiber by pyrolysis of freeze-dried cellulose nanofiber

The possibility of fabricating carbon nanofibers from cellulose nanofibers was investigated. Cellulose nanofiber of ~50 nm in diameter was produced using ball milling in an eco-friendly manner. The effect of the drying techniques of cellulose nanofibers on the morphology of carbon residue was studied. After pyrolysis of freeze-dried cellulose nanofibers below 600 °C, amorphous carbon fibers of ~20 nm in diameter were obtained. The pyrolysis of oven-dried precursors resulted in the loss of original fibrous structures. The different results arising from the two drying techniques are attributed to the difference in the spatial distance between cellulose nanofiber precursors.

Role of enthalpy and entropy in moisture sorption behavior of pineapple pulp powder produced by different drying methods

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)