Freeze drying apparatus

DOEpatents

Coppa, Nicholas V.; Stewart, Paul; Renzi, Ernesto

2001-01-01

The present invention provides methods and apparatus for freeze drying in which a solution, which can be a radioactive salt dissolved within an acid, is frozen into a solid on vertical plates provided within a freeze drying chamber. The solid is sublimated into vapor and condensed in a cold condenser positioned above the freeze drying chamber and connected thereto by a conduit. The vertical positioning of the cold condenser relative to the freeze dryer helps to help prevent substances such as radioactive materials separated from the solution from contaminating the cold condenser. Additionally, the system can be charged with an inert gas to produce a down rush of gas into the freeze drying chamber to also help prevent such substances from contaminating the cold condenser.

Drying effects on the antioxidant properties of polysaccharides obtained from Agaricus blazei Murrill.

PubMed

Wu, Songhai; Li, Feng; Jia, Shaoyi; Ren, Haitao; Gong, Guili; Wang, Yanyan; Lv, Zesheng; Liu, Yong

2014-03-15

Three polysaccharides (ABMP-F, ABMP-V, ABMP-A) were obtained from Agaricus blazei Murrill via methods such as freeze drying, vacuum drying and air drying, respectively. Their chemical compositions were examined, and antioxidant activities were investigated on the basis of assay for hydroxyl radical, DPPH radical, ABTS free radical scavenging ability and assay for Fe(2+)-chelating ability. Results showed that the three ABMPs have different physicochemical and antioxidant properties. Compared with air drying and vacuum drying methods, freeze drying method resulted to ABMP with higher neutral sugar, polysaccharide yield, uronic acid content, and stronger antioxidant abilities of hydroxyl radical, DPPH radical, ABTS radical scavenging and Fe(2+)-chelating. As a result, Agaricus blazei Murrill polysaccharides are natural antioxidant and freeze drying method serves as a good choice for the preparation of such polysaccharides and should be used to produce antioxidants for food industry. Copyright © 2014. Published by Elsevier Ltd.

Variation of the Phytochemical Constituents and Antioxidant Activities of Zingiber officinale var. rubrum Theilade Associated with Different Drying Methods and Polyphenol Oxidase Activity.

PubMed

Ghasemzadeh, Ali; Jaafar, Hawa Z E; Rahmat, Asmah

2016-06-17

The effects of different drying methods (freeze drying, vacuum oven drying, and shade drying) on the phytochemical constituents associated with the antioxidant activities of Z. officinale var. rubrum Theilade were evaluated to determine the optimal drying process for these rhizomes. Total flavonoid content (TFC), total phenolic content (TPC), and polyphenol oxidase (PPO) activity were measured using the spectrophotometric method. Individual phenolic acids and flavonoids, 6- and 8-gingerol and shogaol were identified by ultra-high performance liquid chromatography method. Ferric reducing antioxidant potential (FRAP) and 1,1-diphenyl-2-picrylhydrazyl (DPPH) assays were used for the evaluation of antioxidant activities. The highest reduction in moisture content was observed after freeze drying (82.97%), followed by vacuum oven drying (80.43%) and shade drying (72.65%). The highest TPC, TFC, and 6- and 8-shogaol contents were observed in samples dried by the vacuum oven drying method compared to other drying methods. The highest content of 6- and 8-gingerol was observed after freeze drying, followed by vacuum oven drying and shade drying methods. Fresh samples had the highest PPO activity and lowest content of flavonoid and phenolic acid compounds compared to dried samples. Rhizomes dried by the vacuum oven drying method represent the highest DPPH (52.9%) and FRAP activities (566.5 μM of Fe (II)/g DM), followed by freeze drying (48.3% and 527.1 μM of Fe (II)/g DM, respectively) and shade drying methods (37.64% and 471.8 μM of Fe (II)/g DM, respectively) with IC50 values of 27.2, 29.1, and 34.8 μg/mL, respectively. Negative and significant correlations were observed between PPO and antioxidant activity of rhizomes. Vacuum oven dried rhizomes can be utilized as an ingredient for the development of value-added food products as they contain high contents of phytochemicals with valuable antioxidant potential.

Vacuum Freeze-Drying, a Method Used To Salvage Water-Damaged Archival and Library Materials: A RAMP Study with Guidelines.

ERIC Educational Resources Information Center

McCleary, John M.

This Records and Archives Management Programme (RAMP) study covers the conservation of archival documents and the application of freeze-drying to the salvage of documents damaged by flood. Following an introductory discussion of the hazards of water, the study presents a broad summary of data on freeze-drying, including the behavior of…

A freeze-dried injectable form of ibuprofen: development and optimisation using response surface methodology.

PubMed

Kagkadis, K A; Rekkas, D M; Dallas, P P; Choulis, N H

1996-01-01

In this study a complex of Ibuprofen and b-Hydroxypropylcyclodextrin was prepared employing a freeze drying method. The production parameters and the final specifications of this product were optimized by using response surface methodology. The results show that the freeze dried complex meets the requirements for solubility to be considered as a possible injectable form.

Comparison of three-dimensional printing and vacuum freeze-dried techniques for fabricating composite scaffolds

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sun, Kai; Li, Ruixin; Jiang, Wenxue, E-mail: jiangortholivea@sina.cn

In this study, the performances of different preparation methods of the scaffolds were analyzed for chondrocyte tissue engineering. Silk fibroin/collagen (SF/C) was fabricated using a vacuum freeze-dried technique and by 3D printing. The porosity, water absorption expansion rates, mechanical properties, and pore sizes of the resulting materials were evaluated. The proliferation and metabolism of the cells was detected at different time points using an MTT assay. Cell morphologies and distributions were observed by histological analysis and scanning electron microscopy (SEM). The porosity, water absorption expansion rate, and Young’s modulus of the material obtained via 3D printing were significantly higher thanmore » those obtained by the freeze-dried method, while the pore size did not differ significantly between the two methods. MTT assay results showed that the metabolism of cells seeded on the 3D printed scaffolds was more viable than the metabolism on the freeze-dried material. H&E staining of the scaffolds revealed that the number of cells in the 3D printed scaffold was higher in comparison to a similar measurement on the freeze-dried material. Consequently, stem cells grew well inside the 3D printed scaffolds, as measured by SEM, while the internal structure of the freeze-dried scaffold was disordered. Compared with the freeze-dried technique, the 3D printed scaffold exhibited better overall performance and was more suitable for cartilage tissue engineering. - Highlights: • Silk fibroin/collagen was fabricated using 3D printing. • Physical characterization and Cell compatibility were compared. • 3D printed scaffold exhibited better overall performance.« less

Physicochemical interaction mechanism between nanoparticles and tetrasaccharides (stachyose) during freeze-drying.

PubMed

Kamiya, Seitaro; Nakashima, Kenichiro

2017-12-01

Nanoparticle suspensions are thermodynamically unstable and subject to aggregation. Freeze-drying on addition of saccharides is a useful method for preventing aggregation. In the present study, tetrasaccharides (stachyose) was employed as an additive. In addition, we hypothesize the interactive mechanism between stachyose and the nanoparticles during freeze-drying for the first time. The mean particle size of the rehydrated freeze-dried stachyose-containing nanoparticles (104.7 nm) was similar to the initial particle size before freeze-drying (76.8 nm), indicating that the particle size had been maintained. The mean particle size of the rehydrated normal-dried stachyose-containing nanoparticles was 222.2 nm. The powder X-ray diffraction of the freeze-dried stachyose-containing nanoparticles revealed a halo pattern. The powder X-ray diffraction of the normally dried stachyose-containing nanoparticles produced mainly a halo pattern and a partial peak. These results suggest an interaction between the nanoparticles and stachyose, and that this relationship depends on whether the mixture is freeze-dried or dried normally. In the case of normal drying, although most molecules cannot move rapidly thereby settling irregularly, some stachyose molecules can arrange regularly leading to some degree of crystallization and potentially some aggregation. In contrast, during freeze-drying, the moisture sublimed, while the stachyose molecules and nanoparticles were immobilized in the ice. After sublimation, stachyose remained in the space occupied by water and played the role of a buffer material, thus preventing aggregation.

Determination of the dried product resistance variability and its influence on the product temperature in pharmaceutical freeze-drying.

PubMed

Scutellà, Bernadette; Trelea, Ioan Cristian; Bourlès, Erwan; Fonseca, Fernanda; Passot, Stephanie

2018-07-01

During the primary drying step of the freeze-drying process, mass transfer resistance strongly affects the product temperature, and consequently the final product quality. The main objective of this study was to evaluate the variability of the mass transfer resistance resulting from the dried product layer (R p ) in a manufacturing batch of vials, and its potential effect on the product temperature, from data obtained in a pilot scale freeze-dryer. Sublimation experiments were run at -25 °C and 10 Pa using two different freezing protocols: with spontaneous or controlled ice nucleation. Five repetitions of each condition were performed. Global (pressure rise test) and local (gravimetric) methods were applied as complementary approaches to estimate R p . The global method allowed to assess variability of the evolution of R p with the dried layer thickness between different experiments whereas the local method informed about R p variability at a fixed time within the vial batch. A product temperature variability of approximately ±4.4 °C was defined for a product dried layer thickness of 5 mm. The present approach can be used to estimate the risk of failure of the process due to mass transfer variability when designing freeze-drying cycle. Copyright © 2018 Elsevier B.V. All rights reserved.

Effects of stepwise dry/wet-aging and freezing on meat quality of beef loins.

PubMed

Kim, Yuan H Brad; Meyers, Brandon; Kim, Hyun-Wook; Liceaga, Andrea M; Lemenager, Ronald P

2017-01-01

The objective of this study was to evaluate the effects of stepwise dry/wet-aging and freezing method on quality attributes of beef loins. Paired loins (M. Longissimus lumborum) from eight carcasses were assigned to either stepwise dry/wet-aging (carcass dry-aging for 10days then further wet-aging for 7days in vacuum bags) or carcass dry-aging only for 17days. Then, each loin was divided into three sections for freezing (never-frozen, blast or cryogenic freezing). Stepwise dry/wet-aged loin had lower purge/drip loss and shear force than conventionally dry-aged loin (P<0.05), but similar color and sensory characteristics (P>0.05). The cryogenic freezing resulted in a significant decrease in shear force values and a significant improvement in water-holding capacity (WHC). These findings indicate that the stepwise dry/wet-aging coupled with cryogenic freezing could provide beneficial impacts to the local meat industry by providing equivalent quality attributes as conventional dry-aging and improving WHC of frozen/thawed meat, while reducing the time needed for dry-aging. Copyright © 2016 Elsevier Ltd. All rights reserved.

Ice nucleation temperature influences recovery of activity of a model protein after freeze drying.

PubMed

Cochran, Teresa; Nail, Steven L

2009-09-01

The objective of this study was to determine whether a relationship exists between ice nucleation temperature and recovery of activity of a model protein, lactate dehydrogenase, after freeze drying. Aqueous buffer systems containing 50 microg/mL of protein were frozen in vials with externally mounted thermocouples on the shelf of a freeze dryer, then freeze dried. Various methods were used to establish a wide range of ice nucleation temperatures. An inverse relationship was found between the extent of supercooling during freezing and recovery of activity in the reconstituted solution. The data are consistent with a mechanism of inactivation resulting from adsorption of protein at the ice/freeze-concentrate interface during the freezing process.

Freeze-drying of yeast cultures.

PubMed

Bond, Chris

2007-01-01

A method is described that allows yeast species to be stored using a variation on the standard freeze-drying method, which employs evaporative cooling in a two-stage process. Yeast cultures are placed in glass ampoules after having been mixed with a lyoprotectant. Primary drying is carried out using a centrifuge head connected to a standard freeze-dryer. Once the centrifuge head is running, air is removed and evaporated liquid is captured in the freeze-dryer. Centrifugation continues for 15 min and primary drying for a further 3 h. The ampoules are constricted using a glass blowing torch. They are then placed on the freeze-dryer manifold for secondary drying under vacuum overnight, using phosphorus pentoxide as a desiccant. The ampoules are sealed and removed from the manifold by melting the constricted section. Although the process causes an initial large drop in viability, further losses after storage are minimal. Yeast strains have remained viable for more than 30 yr when stored using this method and sufficient cells are recovered to produce new working stocks. Although survival rates are strain specific, nearly all National Collection of Yeast Cultures strains covering most yeast genera, have been successfully stored with little or no detectable change in strain characteristics.

Freeze-drying of “pearl milk tea”: A general strategy for controllable synthesis of porous materials

PubMed Central

Zhou, Yingke; Tian, Xiaohui; Wang, Pengcheng; Hu, Min; Du, Guodong

2016-01-01

Porous materials have been widely used in many fields, but the large-scale synthesis of materials with controlled pore sizes, pore volumes, and wall thicknesses remains a considerable challenge. Thus, the controllable synthesis of porous materials is of key general importance. Herein, we demonstrate the “pearl milk tea” freeze-drying method to form porous materials with controllable pore characteristics, which is realized by rapidly freezing the uniformly distributed template-containing precursor solution, followed by freeze-drying and suitable calcination. This general and convenient method has been successfully applied to synthesize various porous phosphate and oxide materials using different templates. The method is promising for the development of tunable porous materials for numerous applications of energy, environment, and catalysis, etc. PMID:27193866

Mineralization of carbon and nitrogen from freeze- and over-dried plant material added to soil

DOE Office of Scientific and Technical Information (OSTI.GOV)

Moorhead, K.K.; Graetz, D.A.; Reddy, K.R.

Drying organic material before soil incorporation is a common procedure used in mineralization or decomposition studies. A laboratory study was conducted to determine the effect of drying methods on plant C and N and associated mineralization patterns in soil. Freeze- and oven-dried water hyacinth (Eichhornia crassipes (Mart) Solms) was added to a Kendrick soil (loamy, siliceous, hyperthermic Arenic Paleudults) at a rate of 5 g kg{sup {minus}1} and incubated in the dark at 27{degree}C for 90 d. Oven drying in paper bags significantly increased the lignin content and decreased the mineral content of the plant material compared to freeze drying.more » The total C and N was not significantly different for the two materials. The mineralization of C from freeze-dried plant material was more rapid during the initial stage of decomposition and remained significantly higher throughout the incubation. At 90 d, 50, and 41% of the plant C had evolved as CO{sub 2} for the freeze- and oven-dried plant material, respectively. Mineralization of {sup 15}N from the plant material accounted for 33% of the applied N of the freeze-dried material and 23% of the applied N of the oven-dried material. Nitrogen mineralization and CO{sub 2} evolution were linearly correlated (r=0.998) for the oven-dried plant material, but less correlated (r=0.770) for the freeze-dried material.« less

The influence of additives and drying methods on quality attributes of fish protein powder made from saithe (Pollachius virens).

PubMed

Shaviklo, Gholam Reza; Thorkelsson, Gudjon; Arason, Sigurjon; Kristinsson, Hordur G; Sveinsdottir, Kolbrun

2010-09-01

Fish protein powder (FPP) is used in the food industry for developing formulated food products. This study investigates the feasibility of increasing the value of saithe (Pollachius virens) by producing a functional FPP. Quality attributes of spray and freeze-dried saithe surimi containing lyoprotectants were studied. A freeze-dried saithe surimi without lyoprotectants was also prepared as a control sample. The amount of protein, moisture, fat and carbohydrate in the FPPs were 745-928, 39-58, 21-32 and 10-151 g kg(-1). Quality attributes of FPPs were influenced by the two drying methods and lyoprotectants. The highest level of lipid oxidation was found in the control and the second highest in the spray-dried FPP. The spray-dried fish protein had the lowest viscosity among all FPPs. Gel-forming ability of samples with lyoprotectants was higher than that of the control. Water-binding capacity, emulsion properties and solubility of the freeze-dried fish protein containing lyoprotectants were significantly higher than spray-dried and control samples. However, functional properties of spray-dried FPP were higher than the control sample. It is feasible to develop value-added FPP from saithe surimi using spray- and freeze-drying processes, but freeze-dried FPP containing lyoprotectant had superior functional properties and stability compared with spray-dried sample. Both products might be used as functional protein ingredients in various food systems. Copyright 2010 Society of Chemical Industry.

Modelling and simulation of a moving interface problem: freeze drying of black tea extract

NASA Astrophysics Data System (ADS)

Aydin, Ebubekir Sıddık; Yucel, Ozgun; Sadikoglu, Hasan

2017-06-01

The moving interface separates the material that is subjected to the freeze drying process as dried and frozen. Therefore, the accurate modeling the moving interface reduces the process time and energy consumption by improving the heat and mass transfer predictions during the process. To describe the dynamic behavior of the drying stages of the freeze-drying, a case study of brewed black tea extract in storage trays including moving interface was modeled that the heat and mass transfer equations were solved using orthogonal collocation method based on Jacobian polynomial approximation. Transport parameters and physical properties describing the freeze drying of black tea extract were evaluated by fitting the experimental data using Levenberg-Marquardt algorithm. Experimental results showed good agreement with the theoretical predictions.

The Production of a Stable Infliximab Powder: The Evaluation of Spray and Freeze-Drying for Production.

PubMed

Kanojia, Gaurav; Have, Rimko Ten; Bakker, Arjen; Wagner, Koen; Frijlink, Henderik W; Kersten, Gideon F A; Amorij, Jean-Pierre

2016-01-01

In prospect of developing an oral dosage form of Infliximab, for treatment of Crohn's disease and rheumatoid arthritis, freeze-drying (vial vs Lyoguard trays) and spray-drying were investigated as production method for stable powders. Dextran and inulin were used in combination with sucrose as stabilizing excipients. The drying processes did not affect Infliximab in these formulations, i.e. both the physical integrity and biological activity (TNF binding) were retained. Accelerated stability studies (1 month at 60°C) showed that the TNF binding ability of Infliximab was conserved in the freeze-dried formulations, whereas the liquid counterpart lost all TNF binding. After thermal treatment, the dried formulations showed some chemical modification of the IgG in the dextran-sucrose formulation, probably due to Maillard reaction products. This study indicates that, with the appropriate formulation, both spray-drying and freeze-drying may be useful for (bulk) powder production of Infliximab.

The human milk oligosaccharides are not affected by pasteurization and freeze-drying.

PubMed

Hahn, Won-Ho; Kim, Jaehan; Song, Seunghyun; Park, Suyeon; Kang, Nam Mi

2017-11-06

Human milk oligosaccharides (HMOs) are known as important factors in neurologic and immunologic development of neonates. Moreover, freeze-drying seems to be a promising storage method to improve the processes of human milk banks. However, the effects of pasteurization and freeze-drying on HMOs were not evaluated yet. The purpose of this study is to analyze and compare the HMOs profiles of human milk collected before and after the pasteurization and freeze-drying. Totally nine fresh human milk samples were collected from three healthy mothers at the first, second, and third week after delivery. The samples were treated with Holder pasteurization and freeze-drying. HMOs profiles were analyzed by matrix-assisted laser desorption/ionization (MALDI) time-of-flight/time-of-flight (TOF/TOF) mass spectrometry and compared between samples collected before and after the treatments. Human milk samples showed significantly different HMO patterns between mothers. However, HMOs were not affected by lactation periods within 3 weeks after delivery (r 2  = 0.972-0.999, p < .001). Moreover, both of pasteurization and freeze-drying were found not to affect HMO patterns in a correlation analysis (r 2  = 0.989-0.999, p < .001). HMO patterns were found not to be affected by pasteurization and freeze-drying of donor milks. We hope that introducing freeze-drying to the human milk banks would be encouraged by the present study. However, the storage length without composition changes of HMOs after freeze-drying needs to be evaluated in the further studies.

A New Freezing Method Using Pre-Dehydration by Microwave-Vacuum Drying

NASA Astrophysics Data System (ADS)

Tsuruta, Takaharu; Hamidi, Nurkholis

Partial dehydration by microwave-vacuum drying has been applied to tuna and strawberry in order to reduce cell-damages caused by the formation of large ice-crystals during freezing. The samples were subjected to microwave vacuum drying at pressure of 5 kPa and temperature less than 27°C to remove small amount of water prior to freezing. The tuna were cooled by using the freezing chamber at temperature -50°C or -150°C, while the strawberries were frozen at temperature -30°C or -80°C, respectively. The temperature transients in tuna showed that removing some water before freezing made the freezing time shorter. The observations of ice crystal clearly indicated that rapid cooling and pre-dehydration prior to freezing were effective in minimizing the size of ice crystal. It is also understood that the formation of large ice crystals has a close relation to the cell damages. After thawing, the observation of microstructure was done on the tuna and strawberry halves. The pre-dehydrated samples showed a better structure than the un-dehydrated one. It is concluded that the pre-dehydration by microwave-vacuum drying is one promising method for the cryo-preservation of foods.

Drying effects on the antioxidant properties of tomatoes and ginger.

PubMed

Gümüşay, Özlem Aktürk; Borazan, Alev Akpınar; Ercal, Nuran; Demirkol, Omca

2015-04-15

In this study, the effects of four different drying processes, sun drying (SD), oven drying (OD), vacuum oven drying (VOD) and freeze drying (FD) for tomatoes (Solanum lycopersicum) and ginger (Zingiber officinale) in terms of thiolic and phenolic contents have been studied. Thiol content, total phenolic content (TPC), ascorbic acid (AA) content, and cupric ion reducing antioxidant capacity (CUPRAC) were determined in fresh and dried samples. Glutathione (GSH) and cysteine (Cys) were determined as the thiol contents of tomatoes and ginger. Significant losses were observed in the contents of TPC, AA, GSH and Cys and CUPRAC values in all samples that were dried using the thermal method. There was a statistically significant difference in the losses of the TPC, AA, and thiol contents between the use of thermal drying and freeze drying (except Cys in tomatoes) methods. Freeze dried tomato and ginger samples have been found to have better antioxidant properties. Copyright © 2014 Elsevier Ltd. All rights reserved.

Preservation of EDTA-expanded grid-mounted chromosomes and nuclei for electron microscopy using a specially designed freeze-dryer.

PubMed

Woods, P S; Ledbetter, M C; Tempel, N

1991-06-01

We describe methods for freezing and drying EDTA-expanded, fixed metaphase chromosomes and nuclei, attached to grids as whole-mounts, for transmission electron microscopy. These methods use a special apparatus that is simple to construct. While separate freezers and dryers are commercially available, one for freezing blocks of tissue by slamming them against a cold metal surface, and the other for vacuum drying the frozen tissue, our apparatus is designed for gentler, cryogenic liquid plunge freezing and drying, sequentially, in the same apparatus, thus avoiding any compression or damage to the specimen. Use of a cryoprotectant is not essential; however, good results are obtained more often when 20% ethanol is used. Freezing is accomplished by rapid propulsion of the grid, with specimens attached, into slushy N2 (-210 degrees C) within the drying chamber; drying is automatic, by either sublimation under vacuum or by solvent substitution using absolute ethanol followed by acetone, which, in turn, is removed with a critical-point dryer. The apparatus offers a means of drying chromosomes and nuclei in an expanded state, and avoids the shrinkage of these structures that occurs during stepwise passage through increasing concentrations of ethanol or acetone.

Preparation of High-Grade Powders from Tomato Paste Using a Vacuum Foam Drying Method.

PubMed

Sramek, Martin; Schweiggert, Ralf Martin; van Kampen, Andreas; Carle, Reinhold; Kohlus, Reinhard

2015-08-01

We present a rapid and gentle drying method for the production of high-grade tomato powders from double concentrated tomato paste, comparing results with powders obtained by foam mat air drying and freeze dried powders. The principle of this method consists of drying tomato paste in foamed state at low temperatures in vacuum. The formulations were dried at temperatures of 50, 60, and 70 °C and vacuum of 200 mbar. Foam stability was affected by low serum viscosity and the presence of solid particles in tomato paste. Consequently, serum viscosity was increased by maltodextrin addition, yielding optimum stability at tomato paste:maltodextrin ratio of 2.4:1 (w/w) in dry matter. Material foamability was improved by addition of 0.5% (w/w, fresh weight) egg white. Because of solid particles in tomato paste, foam air filling had to be limited to critical air volume fraction of Φ = 0.7. The paste was first pre-foamed to Φ = 0.2 and subsequently expanded in vacuo. After drying to a moisture content of 5.6% to 7.5% wet base (w.b.), the materials obtained were in glassy state. Qualities of the resulting powders were compared with those produced by freeze and air drying. Total color changes were the least after vacuum drying, whereas air drying resulted in noticeable color changes. Vacuum foam drying at 50 °C led to insignificant carotenoid losses, being equivalent to the time-consuming freeze drying method. In contrast, air drying caused lycopene and β-carotene losses of 18% to 33% and 14% to 19% respectively. Thus, vacuum foam drying enables production of high-grade tomato powders being qualitatively similar to powders obtained by freeze drying. © 2015 Institute of Food Technologists®

Effect of drying methods on total antioxidant capacity of bitter gourd (momordica charantia) fruit

NASA Astrophysics Data System (ADS)

Tan, Ee Shian; Abdullah, Aminah; Maskat, Mohammad Yusof

2013-11-01

The effect of thermal and non-thermal drying methods on hydrophilic and lipophilic antioxidant capacities of bitter gourd fruit was investigated in this study. The bitter gourd fruits were dried by following methods: (i) oven drying 40°C, (ii) oven drying 50°C, (iii) oven drying 60°C, (iv) microwave drying (medium low power), (v) microwave drying (medium power) and (vi) freeze drying. Pure acetone and hexane were used to extract the hydrophilic and lipophilic antioxidant compounds from dried bitter gourd fruits. Freeze dried extracts reported to have highest values in DPPH scavenging activity (hydrophilic and lipophilic fractions), FRAP (lipophilic fraction) and TPC (hydrophilic and lipophilic fraction). Thermal drying slightly increased the values of DPPH scavenging activity, FRAP and TPC assays for hydrophilic extracts. Results concluded bitter gourd fruit is a good source of natural antioxidants and its total antioxidant quality was most preserved by freeze drying. Additionally, the higher value reported in DPPH scavenging activity, FRAP and TPC assays for lipophilic extracts than the hydrophilic extracts suggested that the lipophilic antioxidant compounds of bitter gourd fruit might possess stronger antioxidant power than its counterpart.

Microplate freeze-dried cyanobacterial bioassay for fresh-waters environmental monitoring.

PubMed

Martín-Betancor, Keila; Durand, Marie-José; Thouand, Gérald; Leganés, Francisco; Fernández-Piñas, Francisca; Rodea-Palomares, Ismael

2017-12-01

Microorganisms have been very useful in environmental monitoring due to their constant sensing of the surrounding environment, their easy maintenance and low cost. Some freeze-dried toxicity kits based on naturally bioluminescent bacteria are commercially available and commonly used to assess the toxicity of environmental samples such as Microtox (Aliivibrio fischeri) or ToxScreen (Photobacterium leiognathi), however, due to the marine origin of these bacteria, they could not be the most appropriate for fresh-waters monitoring. Cyanobacteria are one of the most representative microorganisms of aquatic environments, and are well suited for detecting contaminants in aqueous samples. This study presents the development and application of the first freeze-dried cyanobacterial bioassay for fresh-water contaminants detection. The effects of different cell growth phases, cryoprotectant solutions, freezing protocols, rehydration solutions and incubation conditions methods were evaluated and the best combination of these parameters for freeze-drying was selected. The study includes detailed characterization of sensitivity towards reference pollutants, as well as, comparison with the standard assays. Moreover, long-term viability and sensitivity were evaluated after 3 years of storage. Freeze-dried cyanobacteria showed, in general, higher sensitivity than the standard assays and viability of the cells remained after 3 years of storage. Finally, the validation of the bioassay using a wastewater sample was also evaluated. Freeze-drying of cyanobacteria in 96-well plates presents a simple, fast and multi-assay method for environmental monitoring. Copyright © 2017 Elsevier Ltd. All rights reserved.

Effects of six substances on the growth and freeze-drying of Lactobacillus delbrueckii subsp. bulgaricus.

PubMed

Chen, He; Huang, Jie; Shi, Xiaoyu; Li, Yichao; Liu, Yu

2017-01-01

The efficacy of Lactobacillus delbrueckii subsp. bulgaricus as starter cultures for the dairy industry depends largely on the number of viable and active cells. Freeze-drying is the most convenient and successful method to preserve the bacterial cells. However, not all strains survived during freeze-drying. The effects of six substances including NaCl, sorbitol, mannitol, mannose, sodium glutamate, betaine added to the MRS medium on the growth and freeze-drying survival rate and viable counts of Lb. delbrueckii subsp. bulgaricus were studied through a single-factor test and Plackett-Burman design. Subsequently, the optimum freeze-drying conditions of Lb. delbrueckii subsp. bulgaricus were determined. Lb. delbrueckii subsp. bulgaricus survival rates were up to the maximum of 42.7%, 45.4%, 23.6%, while the concentrations of NaCl, sorbitol, sodium glutamate were 0.6%, 0.15%, 0.09%, respectively. In the optimum concentration, the viable counts in broth is 6.1, 6.9, 5.13 (×108 CFU/mL), respectively; the viable counts in freeze-drying power are 3.09, 5.2, 2.7 (×1010 CFU/g), respectively. Three antifreeze factors including NaCl, sorbitol, sodium glutamate have a positive effect on the growth and freeze-drying of Lb. delbrueckii subsp. bulgaricus. The results are beneficial for developing Lb. delbrueckii subsp. bulgaricus.

Detection of Collapse and Crystallization of Saccharide, Protein, and Mannitol Formulations by Optical Fibers in Lyophilization

PubMed Central

Horn, Jacqueline; Friess, Wolfgang

2018-01-01

The collapse temperature (Tc) and the glass transition temperature of freeze-concentrated solutions (Tg') as well as the crystallization behavior of excipients are important physicochemical characteristics which guide the cycle development in freeze-drying. The most frequently used methods to determine these values are differential scanning calorimetry (DSC) and freeze-drying microscopy (FDM). The objective of this study was to evaluate the optical fiber system (OFS) unit as alternative tool for the analysis of Tc, Tg' and crystallization events. The OFS unit was also tested as a potential online monitoring tool during freeze-drying. Freeze/thawing and freeze-drying experiments of sucrose, trehalose, stachyose, mannitol, and highly concentrated IgG1 and lysozyme solutions were carried out and monitored by the OFS. Comparative analyses were performed by DSC and FDM. OFS and FDM results correlated well. The crystallization behavior of mannitol could be monitored by the OFS during freeze/thawing as it can be done by DSC. Online monitoring of freeze-drying runs detected collapse of amorphous saccharide matrices. The OFS unit enabled the analysis of both Tc and crystallization processes, which is usually carried out by FDM and DSC. The OFS can hence be used as novel measuring device. Additionally, detection of these events during lyophilization facilitates online-monitoring. Thus the OFS is a new beneficial tool for the development and monitoring of freeze-drying processes. PMID:29435445

Detection of Collapse and Crystallization of Saccharide, Protein and Mannitol Formulations by Optical Fibers in Lyophilization

NASA Astrophysics Data System (ADS)

Horn, Jacqueline; Friess, Wolfgang

2018-01-01

The collapse temperature (Tc) and the glass transition temperature of freeze-concentrated solutions (Tg’) as well as the crystallization behavior of excipients are important physicochemical characteristics which guide the cycle development in freeze-drying. The most frequently used methods to determine these values are differential scanning calorimetry (DSC) and freeze-drying microscopy (FDM). The objective of this study was to evaluate the optical fiber system (OFS) unit as alternative tool for the analysis of Tc, Tg’ and crystallization events. The OFS unit was also tested as a potential online monitoring tool during freeze-drying. Freeze/thawing and freeze-drying experiments of sucrose, trehalose, stachyose, mannitol and highly concentrated IgG1 and lysozyme solutions were carried out and monitored by the OFS. Comparative analyses were performed by DSC and FDM. OFS and FDM results correlated well. The crystallization behavior of mannitol could be monitored by the OFS during freeze/thawing as it can be done by DSC. Online monitoring of freeze-drying runs detected collapse of amorphous saccharide matrices. The OFS unit enabled the analysis of both Tc and crystallization processes, which is usually carried out by FDM and DSC. The OFS can hence be used as novel measuring device. Additionally, detection of these events during lyophilization facilitate online-monitoring. Thus the OFS is a new beneficial tool for the development and monitoring of freeze-drying processes.

Stabilization of Live Attenuated Influenza Vaccines by Freeze Drying, Spray Drying, and Foam Drying.

PubMed

Lovalenti, Phillip M; Anderl, Jeff; Yee, Luisa; Nguyen, Van; Ghavami, Behnaz; Ohtake, Satoshi; Saxena, Atul; Voss, Thomas; Truong-Le, Vu

2016-05-01

The goal of this research is to develop stable formulations for live attenuated influenza vaccines (LAIV) by employing the drying methods freeze drying, spray drying, and foam drying. Formulated live attenuated Type-A H1N1 and B-strain influenza vaccines with a variety of excipient combinations were dried using one of the three drying methods. Process and storage stability at 4, 25 and 37°C of the LAIV in these formulations was monitored using a TCID50 potency assay. Their immunogenicity was also evaluated in a ferret model. The thermal stability of H1N1 vaccine was significantly enhanced through application of unique formulation combinations and drying processes. Foam dried formulations were as much as an order of magnitude more stable than either spray dried or freeze dried formulations, while exhibiting low process loss and full retention of immunogenicity. Based on long-term stability data, foam dried formulations exhibited a shelf life at 4, 25 and 37°C of >2, 1.5 years and 4.5 months, respectively. Foam dried LAIV Type-B manufactured using the same formulation and process parameters as H1N1 were imparted with a similar level of stability. Foam drying processing methods with appropriate selection of formulation components can produce an order of magnitude improvement in LAIV stability over other drying methods.

Freeze-dried dog sperm: Dynamics of DNA integrity.

PubMed

Olaciregui, M; Luño, V; Gonzalez, N; De Blas, I; Gil, L

2015-10-01

Freeze-drying (FD) has been proposed as an alternative method to preserve spermatozoa. During the FD procedure, sperm DNA might become damaged by both freezing and drying stresses caused by the endonucleases, the oxidative stress and the storage conditions. We examined the DNA integrity of dog sperm freeze-dried with two kinds of chelating agents in FD buffers and storage at two different temperatures. Ejaculated sperm from four dogs were suspended in basic medium (10 mM Tris-HCl buffer+50 mM NaCl) supplemented with 50 mM EGTA or with 50 mM EDTA and then freeze-dried. Sperm samples were stored at 4°C as room temperature, and the analysis of DNA damage was performed after a month and 5 months of storage using a Sperm Chromatin Dispersion test. We found four different sperm populations according to the size of the halos around the sperm head: (1) absent halo, (2) <6 μm, (3) 6-10 μm, (4) >10 μm. All of them coexisted in each freeze-dried dog semen samples and differed significantly among different treatments. The highest percentage of spermatozoa with halo >10 μm was obtained when the semen samples were freeze-dried in EDTA medium and stored at room temperature for five months. Results suggested that both, the kind of chelating agent as well as storage temperature and period, influenced DNA integrity of freeze-dried dog sperm. Copyright © 2015 Elsevier Inc. All rights reserved.

The impact of freeze-drying infant fecal samples on measures of their bacterial community profiles and milk-derived oligosaccharide content.

PubMed

Lewis, Zachery T; Davis, Jasmine C C; Smilowitz, Jennifer T; German, J Bruce; Lebrilla, Carlito B; Mills, David A

2016-01-01

Infant fecal samples are commonly studied to investigate the impacts of breastfeeding on the development of the microbiota and subsequent health effects. Comparisons of infants living in different geographic regions and environmental contexts are needed to aid our understanding of evolutionarily-selected milk adaptations. However, the preservation of fecal samples from individuals in remote locales until they can be processed can be a challenge. Freeze-drying (lyophilization) offers a cost-effective way to preserve some biological samples for transport and analysis at a later date. Currently, it is unknown what, if any, biases are introduced into various analyses by the freeze-drying process. Here, we investigated how freeze-drying affected analysis of two relevant and intertwined aspects of infant fecal samples, marker gene amplicon sequencing of the bacterial community and the fecal oligosaccharide profile (undigested human milk oligosaccharides). No differences were discovered between the fecal oligosaccharide profiles of wet and freeze-dried samples. The marker gene sequencing data showed an increase in proportional representation of Bacteriodes and a decrease in detection of bifidobacteria and members of class Bacilli after freeze-drying. This sample treatment bias may possibly be related to the cell morphology of these different taxa (Gram status). However, these effects did not overwhelm the natural variation among individuals, as the community data still strongly grouped by subject and not by freeze-drying status. We also found that compensating for sample concentration during freeze-drying, while not necessary, was also not detrimental. Freeze-drying may therefore be an acceptable method of sample preservation and mass reduction for some studies of microbial ecology and milk glycan analysis.

Method For Removing Volatile Components From A Gel-Cast Ceramic Article

DOEpatents

Klug, Frederic Joseph; DeCarr, Sylvia Marie

2004-09-07

A method of removing substantially all of the volatile component in a green, volatile-containing ceramic article is disclosed. The method comprises freezing the ceramic article; and then subjecting the frozen article to a vacuum for a sufficient time to freeze-dry the article. Frequently, the article is heated while being freeze-dried. Use of this method efficiently reduces the propensity for any warpage of the article. The article is often formed from a ceramic slurry in a gel-casting process. A method for fabricating a ceramic core used in investment casting is also described.

Method for removing volatile components from a ceramic article, and related processes

DOEpatents

Klug, Frederic Joseph; DeCarr, Sylvia Marie

2002-01-01

A method of removing substantially all of the volatile component in a green, volatile-containing ceramic article is disclosed. The method comprises freezing the ceramic article; and then subjecting the frozen article to a vacuum for a sufficient time to freeze-dry the article. Frequently, the article is heated while being freeze-dried. Use of this method efficiently reduces the propensity for any warpage of the article. The article is often formed from a ceramic slurry in a gel-casting process. A method for fabricating a ceramic core used in investment casting is also described.

The influence of lysozyme on mannitol polymorphism in freeze-dried and spray-dried formulations depends on the selection of the drying process.

PubMed

Grohganz, Holger; Lee, Yan-Ying; Rantanen, Jukka; Yang, Mingshi

2013-04-15

Freeze-drying and spray-drying are often applied drying techniques for biopharmaceutical formulations. The formation of different solid forms upon drying is often dependent on the complex interplay between excipient selection and process parameters. The purpose of this study was to investigate the influence of the chosen drying method on the solid state form. Mannitol-lysozyme solutions of 20mg/mL, with the amount of lysozyme varying between 2.5% and 50% (w/w) of total solid content, were freeze-dried and spray-dried, respectively. The resulting solid state of mannitol was analysed by near-infrared spectroscopy in combination with multivariate analysis and further, results were verified with X-ray powder diffraction. It was seen that the prevalence of the mannitol polymorphic form shifted from β-mannitol to δ-mannitol with increasing protein concentration in freeze-dried formulations. In spray-dried formulations an increase in protein concentration resulted in a shift from β-mannitol to α-mannitol. An increase in final drying temperature of the freeze-drying process towards the temperature of the spray-drying process did not lead to significant changes. It can thus be concluded that it is the drying process in itself, rather than the temperature, that leads to the observed solid state changes. Copyright © 2013 Elsevier B.V. All rights reserved.

Effect of whey protein isolate and β-cyclodextrin wall systems on stability of microencapsulated vanillin by spray-freeze drying method.

PubMed

Hundre, Swetank Y; Karthik, P; Anandharamakrishnan, C

2015-05-01

Vanillin flavour is highly volatile in nature and due to that application in food incorporation is limited; hence microencapsulation of vanillin is an ideal technique to increase its stability and functionality. In this study, vanillin was microencapsulated for the first time by non-thermal spray-freeze-drying (SFD) technique and its stability was compared with other conventional techniques such as spray drying (SD) and freeze-drying (FD). Different wall materials like β-cyclodextrin (β-cyd), whey protein isolate (WPI) and combinations of these wall materials (β-cyd + WPI) were used to encapsulate vanillin. SFD microencapsulated vanillin with WPI showed spherical shape with numerous fine pores on the surface, which in turn exhibited good rehydration ability. On the other hand, SD powder depicted spherical shape without pores and FD encapsulated powder yielded larger particle sizes with flaky structure. FTIR analysis confirmed that there was no interaction between vanillin and wall materials. Moreover, spray-freeze-dried vanillin + WPI sample exhibited better thermal stability than spray dried and freeze-dried microencapsulated samples. Copyright © 2014 Elsevier Ltd. All rights reserved.

Protein spheres prepared by drop jet freeze drying.

PubMed

Eggerstedt, Sören N; Dietzel, Mathias; Sommerfeld, Martin; Süverkrüp, Richard; Lamprecht, Alf

2012-11-15

In spray freeze drying (SFD) solutions are frozen by spraying into a very cold environment and subsequently dried by sublimation. In contrast to conventional freeze drying, spray freeze drying has the possibility to produce flowable lyophilizates which offers a variety of new pharmaceutical applications. Here, a drop jet nozzle is proposed as liquid dispenser that is able to produce droplets with a very narrow size distribution compared to standard methods. The drop jet nozzle is mounted in a spray tower designed to prevent direct contact of the product with the freezing medium. Various formulations have been tested containing lysozyme as model protein and stabilizers such as bovine serum albumin, polyvinylpyrrolidone or dextran in various concentrations and mannitol. Excellent free flowing and nearly monodispersed, porous particles are produced where particle properties can be controlled by formulation and process conditions. The particle diameter varied between 231 ± 3 μm and 310 ± 10 μm depending on the formulation composition. The lysozyme activity was >94 ± 5% for all formulations exhibiting a full preservation of enzyme activity. This new method is very promising for the production of nearly monodisperse particulate lyophilizates in various therapeutic applications. Copyright © 2012 Elsevier B.V. All rights reserved.

Effect of Drying Methods on Protein and DNA Conformation Changes in Lactobacillus rhamnosus GG Cells by Fourier Transform Infrared Spectroscopy.

PubMed

Hlaing, Mya M; Wood, Bayden R; McNaughton, Don; Ying, DanYang; Dumsday, Geoff; Augustin, Mary Ann

2017-03-01

Microencapsulation protects cells against environmental stress encountered during the production of probiotics, which are used as live microbial food ingredients. Freeze-drying and spray-drying are used in the preparation of powdered microencapsulated probiotics. This study examines the ability of Fourier transform infrared (FTIR) spectroscopy to detect differences in cells exposed to freeze-drying and spray-drying of encapsulated Lactobacillus rhamnosus GG cells. The FTIR analysis clearly demonstrated there were more significant molecular changes in lipid, fatty acid content, protein, and DNA conformation of nonencapsulated compared to encapsulated bacterial cells. The technique was also able to differentiate between spray-dried and freeze-dried cells. The results also revealed the extent of protection from a protein-carbohydrate-based encapsulant matrix on the cells depending on the type drying process. The extent of this protection to the dehydration stress was shown to be less in spray-dried cells than in freeze-dried cells. This suggests that FTIR could be used as a rapid, noninvasive, and real-time measurement technique to detect detrimental drying effects on cells.

Application of the Quality by Design Approach to the Freezing Step of Freeze-Drying: Building the Design Space.

PubMed

Arsiccio, Andrea; Pisano, Roberto

2018-06-01

The present work shows a rational method for the development of the freezing step of a freeze-drying cycle. The current approach to the selection of freezing conditions is still empirical and nonsystematic, thus resulting in poor robustness of control strategy. The final aim of this work is to fill this gap, describing a rational procedure, based on mathematical modeling, for properly choosing the freezing conditions. Mechanistic models are used for the prediction of temperature profiles during freezing and dimension of ice crystals being formed. Mathematical description of the drying phase of freeze-drying is also coupled with the results obtained by freezing models, thus providing a comprehensive characterization of the lyophilization process. In this framework, deep understanding of the phenomena involved is required, and according to the Quality by Design approach, this knowledge can be used to build the design space. The step-by-step procedure for building the design space for freezing is thus described, and examples of applications are provided. The calculated design space is validated upon experimental data, and we show that it allows easy control of the freezing process and fast selection of appropriate operating conditions. Copyright © 2018 American Pharmacists Association®. Published by Elsevier Inc. All rights reserved.

The Production of a Stable Infliximab Powder: The Evaluation of Spray and Freeze-Drying for Production

PubMed Central

Kanojia, Gaurav; Have, Rimko ten; Bakker, Arjen; Wagner, Koen; Frijlink, Henderik W.; Kersten, Gideon F. A.; Amorij, Jean-Pierre

2016-01-01

In prospect of developing an oral dosage form of Infliximab, for treatment of Crohn’s disease and rheumatoid arthritis, freeze-drying (vial vs Lyoguard trays) and spray-drying were investigated as production method for stable powders. Dextran and inulin were used in combination with sucrose as stabilizing excipients. The drying processes did not affect Infliximab in these formulations, i.e. both the physical integrity and biological activity (TNF binding) were retained. Accelerated stability studies (1 month at 60°C) showed that the TNF binding ability of Infliximab was conserved in the freeze-dried formulations, whereas the liquid counterpart lost all TNF binding. After thermal treatment, the dried formulations showed some chemical modification of the IgG in the dextran-sucrose formulation, probably due to Maillard reaction products. This study indicates that, with the appropriate formulation, both spray-drying and freeze-drying may be useful for (bulk) powder production of Infliximab. PMID:27706175

Protein crowding in solution, frozen and freeze-dried states: small-angle neutron and X-ray scattering study of lysozyme/sorbitol/water systems

NASA Astrophysics Data System (ADS)

Krueger, Susan; Khodadadi, Sheila; Clark, Nicholas; McAuley, Arnold; Cristiglio, Viviana; Theyencheri, Narayanan; Curtis, Joseph; Shalaev, Evgenyi

2015-03-01

For effective preservation, proteins are often stored as frozen solutions or in glassy states using a freeze-drying process. However, aggregation is often observed after freeze-thaw or reconstitution of freeze-dried powder and the stability of the protein is no longer assured. In this study, small-angle neutron and X-ray scattering (SANS and SAXS) have been used to investigate changes in protein-protein interaction distances of a model protein/cryoprotectant system of lysozyme/sorbitol/water, under representative pharmaceutical processing conditions. The results demonstrate the utility of SAXS and SANS methods to monitor protein crowding at different stages of freezing and drying. The SANS measurements of solution samples showed at least one protein interaction peak corresponding to an interaction distance of ~ 90 Å. In the frozen state, two protein interaction peaks were observed by SANS with corresponding interaction distances at 40 Å as well as 90 Å. On the other hand, both SAXS and SANS data for freeze-dried samples showed three peaks, suggesting interaction distances ranging from ~ 15 Å to 170 Å. Possible interpretations of these interaction peaks will be discussed, as well as the role of sorbitol as a cryoprotectant during the freezing and drying process.

Freeze-dried, mucoadhesive system for vaginal delivery of the HIV microbicide, dapivirine: optimisation by an artificial neural network.

PubMed

Woolfson, A David; Umrethia, Manish L; Kett, Victoria L; Malcolm, R Karl

2010-03-30

Dapivirine mucoadhesive gels and freeze-dried tablets were prepared using a 3x3x2 factorial design. An artificial neural network (ANN) with multi-layer perception was used to investigate the effect of hydroxypropyl-methylcellulose (HPMC): polyvinylpyrrolidone (PVP) ratio (X1), mucoadhesive concentration (X2) and delivery system (gel or freeze-dried mucoadhesive tablet, X3) on response variables; cumulative release of dapivirine at 24h (Q(24)), mucoadhesive force (F(max)) and zero-rate viscosity. Optimisation was performed by minimising the error between the experimental and predicted values of responses by ANN. The method was validated using check point analysis by preparing six formulations of gels and their corresponding freeze-dried tablets randomly selected from within the design space of contour plots. Experimental and predicted values of response variables were not significantly different (p>0.05, two-sided paired t-test). For gels, Q(24) values were higher than their corresponding freeze-dried tablets. F(max) values for freeze-dried tablets were significantly different (2-4 times greater, p>0.05, two-sided paired t-test) compared to equivalent gels. Freeze-dried tablets having lower values for X1 and higher values for X2 components offered the best compromise between effective dapivirine release, mucoadhesion and viscosity such that increased vaginal residence time was likely to be achieved. Copyright (c) 2009 Elsevier B.V. All rights reserved.

Influence of drying method on the material properties of nanocellulose I: thermostability and crystallinity

Treesearch

Yucheng Peng; Douglas J. Gardner; Yousoo Han; Alper Kiziltas; Zhiyong Cai; Mandla A. Tshabalala

2013-01-01

The effect of drying method on selected material properties of nanocellulose was investigated. Samples of nanofibrillated cellulose (NFC) and cellulose nanocrystals (CNC) were each subjected to four separate drying methods: air-drying, freeze-drying, spray-drying, and supercritical-drying. The thermal stability and crystallinity of the dried nanocellulose were...

Assessing storage of stability and mercury reduction of freeze-dried Pseudomonas putida within different types of lyoprotectant

NASA Astrophysics Data System (ADS)

Azoddein, Abdul Aziz Mohd; Nuratri, Yana; Azli, Faten Ahada Mohd; Bustary, Ahmad Bazli

2017-12-01

Pseudomonas putida is a potential strain in biological treatment to remove mercury contained in the effluent of petrochemical industry due to its mercury reductase enzyme that able to reduce ionic mercury to elementary mercury. Freeze-dried P. putida allows easy, inexpensive shipping, handling and high stability of the product. This study was aimed to freeze dry P. putida cells with addition of lyoprotectant. Lyoprotectant was added into the cells suspension prior to freezing. Dried P. putida obtained was then mixed with synthetic mercury. Viability of recovery P. putida after freeze dry was significantly influenced by the type of lyoprotectant. Among the lyoprotectants, tween 80/ sucrose was found to be the best lyoprotectant. Sucrose was able to recover more than 78% (6.2E+09 CFU/ml) of the original cells (7.90E+09CFU/ml) after freeze dry and able to retain 5.40E+05 viable cells after 4 weeks storage at 4 °C without vacuum. Polyethylene glycol (PEG) pre-treated freeze dried cells and broth pre-treated freeze dried cells after the freeze-dry process recovered more than 64% (5.0 E+09CFU/ml) and >0.1% (5.60E+07CFU/ml). Freeze-dried P. putida cells in PEG and broth cannot survive after 4 weeks storage. Freeze dry also does not really change the pattern of growth P. putida but extension of lag time was found 1 hour after 3 weeks of storage. Additional time was required for freeze-dried P. putida cells to recover before introducing freeze-dried cells to more complicated condition such as mercury solution. The maximum mercury reduction of PEG pre-treated freeze-dried cells after freeze dry and after storage of 3 weeks was 17.91 %. The maximum of mercury reduction of tween 80/sucrose pre-treated freeze-dried cells after freeze dry and after storage 3 weeks was 25.03%. Freeze dried P. putida was found to have lower mercury reduction compare to the fresh P. putida that has been grown in agar. Result from this study may be beneficial and useful as initial reference before commercialized freeze-dried P. putida.

Effects of drying-wetting and freezing-thawing cycle on leachability of metallic elements in mine soils

NASA Astrophysics Data System (ADS)

Bang, H.; Kim, J.; Hyun, S.

2016-12-01

Mine leachate derived from contaminated mine sites with metallic elements can pose serious risks on human society and environment. Only labile fraction of metallic elements in mine soils is subject to leaching and movement by rainfall. Lability of metallic element in soil is a function of bond strengths between metal and soil surfaces, which is influenced by environmental condition (e.g., rainfall intensity, duration, temperature, etc.) The purpose of this study was to elucidate the effects of various climate conditions on the leaching patterns and lability of metallic elements in mine soils. To do this, two mine soils were sampled from two abandoned mine sites located in Korea. Leaching test were conducted using batch decant-refill method. Various climatic conditions were employed in leaching test such as (1) oven drying (40oC) - wetting cycles, (2) air drying (20oC) - wetting cycle, and (3) freezing (-40oC) - thawing cycles. Duration of drying and freezing were varied from 4 days to 2 weeks. Concentration of metallic elements, pH, Eh and concentration of dissolved iron and sulfate in leachate from each leaching process was measured. To identify the changes of labile fraction in mine soils after each of drying or freezing period, sequential extraction procedure (five fraction) was used to compare labile fraction (i.e., F1 + F2) of metallic elements. The concentration of metallic elements in mine leachate was increased after drying and freezing procedure. The amounts of released metallic element from mine soils was changed depending on their drying or freezing period. In addition, labile fraction of metallic elements in soil was also changed after drying and freezing. The changes in labile fraction after drying and freezing might be due to the increased soil surface area by pore water volume expansion. Further study is therefore needed to evaluate the impact of altered physical properties of soils such as hydration of soil surface area and shrinking by drying and freezing cycles.

Scanning electron microscopy of high-pressure-frozen sea urchin embryos.

PubMed

Walther, P; Chen, Y; Malecki, M; Zoran, S L; Schatten, G P; Pawley, J B

1993-12-01

High-pressure-freezing permits direct cryo-fixation of sea urchin embryos having a defined developmental state without the formation of large ice crystals. We have investigated preparation protocols for observing high-pressure-frozen and freeze-fractured samples in the scanning electron microscope. High-pressure-freezing was superior to other freezing protocols, because the whole bulk sample was reasonably well frozen and the overall three-dimensional shape of the embryos was well preserved. The samples were either dehydrated by freeze-substitution and critical-point-drying, or imaged in the partially hydrated state, using a cold stage in the SEM. During freeze-substitution the samples were stabilized by fixatives. The disadvantage of this method was that shrinking and extraction effects, caused by the removal of the water, could not be avoided. These disadvantages were avoided when the sample was imaged in the frozen-hydrated state using a cold-stage in the SEM. This would be the method of choice for morphometric studies. Frozen-hydrated samples, however, were very beam sensitive and many structures remained covered by the ice and were not visible. Frozen-hydrated samples were partially freeze-dried to make visible additional structures that had been covered by ice. However, this method also caused drying artifacts when too much water was removed.

Effects of hot air and freeze drying methods on antioxidant activity, colour and some nutritional characteristics of strawberry tree (Arbutus unedo L) fruit.

PubMed

Orak, H H; Aktas, T; Yagar, H; İsbilir, S Selen; Ekinci, N; Sahin, F Hasturk

2012-08-01

Antioxidant activity, colour and some nutritional properties of hot air and freeze-dried strawberry tree (Arbutus unedo L.) fruits were investigated. Additionally, the effects of two pre-treatments, namely ethyl oleate and water blanching, were compared in terms of drying characteristics. For determination of antioxidant activities in ethanol extracts, two different analytical methods were used: 1,1-diphenyl-2-picrylhydrazyl scavenging activity and β-carotene bleaching activity. As a result, the ethyl oleate pre-treatment shortened the drying time by hot air method and gave a higher 1,1-diphenyl-2-picrylhydrazyl scavenging activity (82.16 ± 0.34%), total phenolic content (7.62 ± 1.09 µg GAE/g extract), ascorbic acid content (236.93 ± 20.14 mg/100 g), besides hydromethylfurfural was not observed. Freeze-dried fruits exhibited higher ascorbic acid content (368.63 ± 17.16 mg/100 g) than those fresh fruits (231.33 ± 19.51 mg/100 g) and nearly 1,1-diphenyl-2-picrylhydrazyl activity (93.52 ± 0.41 %) to fresh fruits (94.03 ± 1.18%). Colour characteristics, sugar content and mineral contents of fruits were significantly affected by pre-treatments and drying methods (p < 0.05). It is concluded that the drying of strawberry tree fruits should bring a valuable and attractive foodstuff to food industry due to the rich nutritional components, antioxidant activity and colour. Another conclusion from this study is that the freeze-drying is the best drying method to keep the nutritional value, antioxidant activity and sensory properties of fruits.

Electronic Nose Characterization of the Quality Parameters of Freeze-Dried Bacteria

NASA Astrophysics Data System (ADS)

Capuano, R.; Santonico, M.; Martinelli, E.; Paolesse, R.; Passot, S.; Fonseca, F.; Cenard, S.; Trelea, C.; Di Natale, C.

2011-09-01

Freeze-drying is the method of choice for preserving heat sensitive biological products such as microorganisms. The development of a fast analytical method for evaluating the properties of the dehydrated bacteria is then necessary for a proper utilization of the product in several food processes. In this paper, dried bacteria headspace is analyzed by a GC-MS and an electronic nose. Results indicate that headspace contains enough information to assess the products quality.

Influence of drying treatments on antioxidant capacity of forage legume leaves.

PubMed

Sang, Saw Yei; Jamharee, Fazrina; Prasad, K Nagendra; Azlan, Azrina; Maliki, Nurzillah

2014-05-01

This study was aimed to investigate the antioxidant capacities of four common forage legume leaves namely, Arachis pintoi (Pintoi), Calapogonium mucunoides (Calapo), Centrosema pubescens (Centro), and Stylosanthes guanensis (Stylo). Two different drying methods (oven-drying and freeze-drying) were employed and antioxidant activities were determined by DPPH, Ferric Reducing Antioxidant Power (FRAP) and β-carotene bleaching assays. Total phenolic content (TPC) was determined using Folin-Ciocalteu assay. Freeze-dried extract showed the highest antioxidant activities by DPPH (EC50 values 1.17-2.13 mg/ml), FRAP (147.08-246.42 μM of Fe(2+)/g), and β-carotene bleaching (57.11-78.60%) compared to oven drying. Hence, freeze drying treatment could be considered useful in retention of antioxidant activity and phenolic content.

New Processes for Freeze-Drying in Dual-Chamber Systems.

PubMed

Werk, T; Ludwig, I S; Luemkemann, J; Huwyler, J; Mahler, H-C; Haeuser, C R; Hafner, M

2016-01-01

Dual-chamber systems can offer self-administration and home care use for lyophilized biologics. Only a few products have been launched in dual-chamber systems so far-presumably due to dual-chamber systems' complex and costly drug product manufacturing process. Within this paper, two improved processes (both based on tray filling technology) for freeze-drying pharmaceuticals in dual-chamber systems are described. Challenges with regards to heat transfer were tackled by (1) performing the freeze-drying step in a needle-down orientation in combination with an aluminum block, or (2) freeze-drying the drug product "externally" in a metal cartridge with subsequent filling of the lyophilized cake into the dual-chamber system. Metal-mediated heat transfer was shown to be efficient in both cases and batch (unit-to-unit) homogeneity with regards to sublimation rate was increased. It was difficult to influence ice crystal size using different methods when in use with an aluminum block due to its heat capacity. Using such a metal carrier implies a large heat capacity leading to relatively small ice crystals. Compared to the established process, drying times were reduced by half using the new processes. The drying time was, however, longer for syringes compared to vials due to the syringe design (long and slim). The differences in drying times were less pronounced for aggressive drying cycles. The proposed processes may help to considerably decrease investment costs into dual-chamber system fill-finish equipment. Dual-chamber syringes offer self-administration and home care use for freeze-dried pharmaceuticals. Only a few products have been launched in dual-chamber syringes so far-presumably due to their complex and costly drug product manufacturing process. In this paper two improved processes for freeze-drying pharmaceuticals in dual-chamber syringes are described. The major challenge of freeze-drying is to transfer heat through a vacuum. The proposed processes cope with this challenge by (1) freeze-drying the drug product in the syringe in an orientation in which the product is closest to the heat source, or (2) freeze-drying the drug product outside the syringe in a metal tube. The latter requires filling the freeze-dried product subsequently into the dual-chamber syringe. Both processes were very efficient and promised to achieve similar freeze-drying conditions for all dual-chamber syringes within one production run. The proposed processes may help to considerably decrease investment costs into dual-chamber syringe fill-finish equipment. © PDA, Inc. 2016.

Evaluation of Heat Flux Measurement as a New Process Analytical Technology Monitoring Tool in Freeze Drying.

PubMed

Vollrath, Ilona; Pauli, Victoria; Friess, Wolfgang; Freitag, Angelika; Hawe, Andrea; Winter, Gerhard

2017-05-01

This study investigates the suitability of heat flux measurement as a new technique for monitoring product temperature and critical end points during freeze drying. The heat flux sensor is tightly mounted on the shelf and measures non-invasively (no contact with the product) the heat transferred from shelf to vial. Heat flux data were compared to comparative pressure measurement, thermocouple readings, and Karl Fischer titration as current state of the art monitoring techniques. The whole freeze drying process including freezing (both by ramp freezing and controlled nucleation) and primary and secondary drying was considered. We found that direct measurement of the transferred heat enables more insights into thermodynamics of the freezing process. Furthermore, a vial heat transfer coefficient can be calculated from heat flux data, which ultimately provides a non-invasive method to monitor product temperature throughout primary drying. The end point of primary drying determined by heat flux measurements was in accordance with the one defined by thermocouples. During secondary drying, heat flux measurements could not indicate the progress of drying as monitoring the residual moisture content. In conclusion, heat flux measurements are a promising new non-invasive tool for lyophilization process monitoring and development using energy transfer as a control parameter. Copyright © 2017 American Pharmacists Association®. Published by Elsevier Inc. All rights reserved.

Changes of hydrogen peroxide and radical-scavenging activity of raspberry during osmotic, convective, and freeze-drying.

PubMed

Novaković, Miroslav M; Stevanović, Snežana M; Gorjanović, Stanislava Ž; Jovanovic, Predrag M; Tešević, Vele V; Janković, Miodrag A; Sužnjević, Desanka Ž

2011-05-01

This study was conducted to investigate the influence of different drying treatments on antioxidant (AO) activity and phenolic content of raspberry (Rubus idaeus), cultivar Willamette. Whole raspberry fruits were dried convectively (air-drying), osmotically, and freeze-dried. Acetone-water extracts of fresh and dried raspberries were assessed for total phenolic content by standard Folin-Ciocalteau method. Two AO assays were applied, a recently developed direct current (DC) polarographic assay based on decrease of anodic oxidation current of hydrogen peroxide and widely used radical scavenge against the 1,1-diphenyl-2-picrylhydrazyl (DPPH). Strong correlation has been obtained between both AO assays and total phenolic content. In addition, some individual phenolic compounds present in raspberry have been assessed using DPPH and DC polarographic assay. Comparison and evaluation of drying methods has been based on preservation of AO activity and total phenolic content. Obtained results confirmed superiority of freeze-drying; convective drying caused slight changes while osmotic dehydration showed a significant decrease of phenolic compounds and AO activity. © 2011 Institute of Food Technologists®

Controlled ice nucleation in the field of freeze-drying: fundamentals and technology review.

PubMed

Geidobler, R; Winter, G

2013-10-01

In the scientific community as well as in commercial freeze-drying, controlled ice nucleation has received a lot of attention because increasing the ice nucleation temperature can significantly reduce primary drying duration. Furthermore, controlled ice nucleation enables to reduce the randomness of the ice nucleation temperature, which can be a serious scale-up issue during process development. In this review, fundamentals of ice nucleation in the field of freeze-drying are presented. Furthermore, the impact of controlled ice nucleation on product qualities is discussed, and methods to achieve controlled ice nucleation are presented. Copyright © 2013 Elsevier B.V. All rights reserved.

Long Term Storage of Ascosphaera aggregata and A. apis Pathogens of the Leafcutting Bee (Megachile rotundata) and the Honey Bee (Apis mellifera)

USDA-ARS?s Scientific Manuscript database

Survival of Ascosphaera aggregata and A. apis over the course of a year were tested using different storage treatments. For spores, the methods tested were freeze drying and ultra-low temperature storage, and for hyphae, freeze drying, agar slants covered with water, and two methods of ultra-low tem...

Evaluation of manometric temperature measurement, a process analytical technology tool for freeze-drying: part II measurement of dry-layer resistance.

PubMed

Tang, Xiaolin Charlie; Nail, Steven L; Pikal, Michael J

2006-01-01

The purpose of this work was to study the factors that may cause systematic errors in the manometric temperature measurement (MTM) procedure used to determine product dry-layer resistance to vapor flow. Product temperature and dry-layer resistance were obtained using MTM software installed on a laboratory freeze-dryer. The MTM resistance values were compared with the resistance values obtained using the "vial method." The product dry-layer resistances obtained by MTM, assuming fixed temperature difference (DeltaT; 2 degrees C), were lower than the actual values, especially when the product temperatures and sublimation rates were low, but with DeltaT determined from the pressure rise data, more accurate results were obtained. MTM resistance values were generally lower than the values obtained with the vial method, particularly whenever freeze-drying was conducted under conditions that produced large variations in product temperature (ie, low shelf temperature, low chamber pressure, and without thermal shields). In an experiment designed to magnify temperature heterogeneity, MTM resistance values were much lower than the simple average of the product resistances. However, in experiments where product temperatures were homogenous, good agreement between MTM and "vial-method" resistances was obtained. The reason for the low MTM resistance problem is the fast vapor pressure rise from a few "warm" edge vials or vials with low resistance. With proper use of thermal shields, and the evaluation of DeltaT from the data, MTM resistance data are accurate. Thus, the MTM method for determining dry-layer resistance is a useful tool for freeze-drying process analytical technology.

Accurate prediction of collapse temperature using optical coherence tomography-based freeze-drying microscopy.

PubMed

Greco, Kristyn; Mujat, Mircea; Galbally-Kinney, Kristin L; Hammer, Daniel X; Ferguson, R Daniel; Iftimia, Nicusor; Mulhall, Phillip; Sharma, Puneet; Kessler, William J; Pikal, Michael J

2013-06-01

The objective of this study was to assess the feasibility of developing and applying a laboratory tool that can provide three-dimensional product structural information during freeze-drying and which can accurately characterize the collapse temperature (Tc ) of pharmaceutical formulations designed for freeze-drying. A single-vial freeze dryer coupled with optical coherence tomography freeze-drying microscopy (OCT-FDM) was developed to investigate the structure and Tc of formulations in pharmaceutically relevant products containers (i.e., freeze-drying in vials). OCT-FDM was used to measure the Tc and eutectic melt of three formulations in freeze-drying vials. The Tc as measured by OCT-FDM was found to be predictive of freeze-drying with a batch of vials in a conventional laboratory freeze dryer. The freeze-drying cycles developed using OCT-FDM data, as compared with traditional light transmission freeze-drying microscopy (LT-FDM), resulted in a significant reduction in primary drying time, which could result in a substantial reduction of manufacturing costs while maintaining product quality. OCT-FDM provides quantitative data to justify freeze-drying at temperatures higher than the Tc measured by LT-FDM and provides a reliable upper limit to setting a product temperature in primary drying. Copyright © 2013 Wiley Periodicals, Inc.

Rehydration properties of hybrid method dried fruit enriched by natural components

NASA Astrophysics Data System (ADS)

Kowalska, Hanna; Marzec, Agata; Kowalska, Jolanta; Ciurzyńska, Agnieszka; Samborska, Kinga; Bialik, Michał; Lenart, Andrzej

2018-04-01

The aim of the study was to determine the impact of osmotic pre-dehydration and drying of fruit on the rehydration properties of dried fruit. Herein, the effect of fruit juice, applied as a natural enriching substance was very important. In addition, the properties of dried fruits obtained through combined air-drying and subsequent microwave-vacuum drying with `puffing' effect were similar to the freeze-dried fruits, but showed other rehydration properties. As raw material, frozen strawberry (Honeoye variety) and fresh apples (Idared variety) were used in the study. The apples and partially defrosted strawberries were prior dehydrated in solutions of sucrose and a mixture of sucrose with chokeberry juice concentrate at 50°C for 2 h. Next, the fruit samples were dried by one of two ways: air-drying (50°C, 5 h) and microwavevacuum drying for about 360 s; and freeze-drying (30°C, 63 Pa, 24 h). The rehydration was carried out in distilled water (20°C, 5 h). The osmotic pre-dehydration hindered fruit drying process. The impact of drying method became particularly evident while examining the kinetics of rehydration. During the rehydration of the pre-dehydrated dried fruit a slower hydration could be observed. Freeze-dried strawberries absorbed 2-3 times more water than those dried by the `puffing' effect.

Applications of Headspace Moisture Analysis for Investigating the Water Dynamics within a Sealed Vial Containing Freeze-dried Material.

PubMed

Cook, Isobel Ann; Ward, Kevin Richard

2011-01-01

We compare frequency modulation spectroscopy (FMS) as a method of headspace water analysis with the method of Karl Fischer coulometric titration (KF), which is widely used in the analysis of residual water in a freeze-dried material. Parameters relating to the type of formulation (amorphous, crystalline) and the freeze-drying cycle (temperature, pressure, time) were investigated in relation to the resulting headspace moisture (HSM) and total water. We describe the effect of stopper treatment and storage conditions on the HSM levels observed using FMS as a non-destructive method, which also allowed individual vials to be reanalyzed at a series of time points as part of a long-term monitoring exercise. The results of this study enabled a better understanding of the effect of stopper type and pre-lyophilization treatment on the HSM levels both immediately after freeze-drying and upon subsequent storage of the sealed vials of lyophilized material at different temperatures. A clear, linear relationship was observed between HSM and KF values for vials containing freeze-dried sucrose, implying a relatively straightforward interaction between water and the lyophilized cake for this material. Moisture mapping of all vials on one shelf of the freeze-dryer enabled further information to be obtained on the relationship of the formulation, vial, process conditions, equipment geometry, and performance on the intra-batch variability in HSM level and dynamics. It is believed that this could therefore represent a potentially useful technique for quality assurance and in the validation of lyophilization cycles, equipment, and scale-up. Lyophilization, also known as "freeze-drying," is a relatively old technique that has been used in its most basic form for thousands of years (e.g., preservation of fish and meat products). In its more advanced form it is used to preserve many medical products, for example, many vaccines are not stable in solution and therefore need to be dried to allow long-term storage. In order to produce a freeze-dried vaccine a complex understanding of the processes and critical temperatures is required. Once these have been understood the material is dried to give relatively low moisture content (e.g., 2% w/w). This low moisture content is critical for the long-term stability of the product, allowing doctors/chemists to store these goods on site for use when required. This research paper provides further information on a technique called frequency modulation spectroscopy (FMS) that could be used to further our knowledge of the water dynamics within a freeze-dried product, enabling us to increase our understanding of the role various materials and processing conditions play; this in turn could assist in improving quality assurance and ultimately the final product that reaches the consumer.

A novel freeze-dried storage and preparation method for the determination of mycophenolic acid in plasma by high-performance liquid chromatography.

PubMed

Wang, Lei; Qiang, Wei; Li, Ying; Cheng, Zeneng; Xie, Mengmeng

2017-09-01

Plasma samples were conventionally stored at freezing conditions until the time of detection. Such a technique, when carried out over an extended period, is energy consuming; in addition, preparation and transportation of stored samples is inconvenient. In this study, a freeze-dried storage and preparation method was proposed to determine the presence of mycophenolic acid (MPA) in plasma. Fresh plasma samples were freeze-dried using a device, and then stored at ambient temperature. After the stored samples were soaked with methanol spiked with the internal standard, high-performance liquid chromatography was conducted to detect MPA. The proposed method was demonstrated to be precise and accurate over the linear range of 0.5-50 μg mL -1 , with both intra- and inter-day precision being <7% and biases <10%. The freeze-dried samples were stable at ambient temperature for at least 40 days. This method was also successfully applied to the pharmacokinetic study of MPA in healthy volunteers. Pharmacokinetic parameters, such as maximum plasma concentration, time point of maximum plasma concentration and elimination half-life, among others, were consistent with the results in the published study. This proposed technique was proved to be simple, reproducible and energy saving. This approach could also simplify the storage and analysis of samples in clinical and scientific drug research. Copyright © 2017 John Wiley & Sons, Ltd.

Characteristics of sugar surfactants in stabilizing proteins during freeze-thawing and freeze-drying.

PubMed

Imamura, Koreyoshi; Murai, Katsuyuki; Korehisa, Tamayo; Shimizu, Noriyuki; Yamahira, Ryo; Matsuura, Tsutashi; Tada, Hiroko; Imanaka, Hiroyuki; Ishida, Naoyuki; Nakanishi, Kazuhiro

2014-06-01

Sugar surfactants with different alkyl chain lengths and sugar head groups were compared for their protein-stabilizing effect during freeze-thawing and freeze-drying. Six enzymes, different in terms of tolerance against inactivation because of freeze-thawing and freeze-drying, were used as model proteins. The enzyme activities that remained after freeze-thawing and freeze-drying in the presence of a sugar surfactant were measured for different types and concentrations of sugar surfactants. Sugar surfactants stabilized all of the tested enzymes both during freeze-thawing and freeze-drying, and a one or two order higher amount of added sugar surfactant was required for achieving protein stabilization during freeze-drying than for the cryoprotection. The comprehensive comparison showed that the C10-C12 esters of sucrose or trehalose were the most effective through the freeze-drying process: the remaining enzyme activities after freeze-thawing and freeze-drying increased at the sugar ester concentrations of 1-10 and 10-100 μM, respectively, and increased to a greater extent than for the other surfactants at higher concentrations. Results also indicate that, when a decent amount of sugar was also added, the protein-stabilizing effect of a small amount of sugar ester through the freeze-drying process could be enhanced. © 2014 Wiley Periodicals, Inc. and the American Pharmacists Association.

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

PubMed

Ahmed, Faruq; Li, Yan; Fanning, Kent; Netzel, Michael; Schenk, Peer M

2015-08-01

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 20weeks. 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 20weeks of storage. Cost-benefit analysis showed that freeze-drying followed by vacuum-packed storage at -20°C can generate AUD$600 higher profit compared to spray-drying from 100kgH. 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. Copyright © 2015 Elsevier Ltd. All rights reserved.

The surface area of soil organic matter

USGS Publications Warehouse

Chiou, C.T.; Lee, J.-F.; Boyd, S.A.

1990-01-01

The previously reported surface area for soil organic matter (SOM) of 560-800 m2/g as determined by the ethylene glycol (EG) retention method was reexamined by the standard BET method based on nitrogen adsorption at liquid nitrogen temperature. Test samples consisted of two high organic content soils, a freeze-dried soil humic acid, and an oven-dried soil humic acid. The measured BET areas for these samples were less than 1 m2/g, except for the freeze-dried humic acid. The results suggest that surface adsorption of nonionic organic compounds by SOM is practically insignificant in comparison to uptake by partition. The discrepancy between the surface areas of SOM obtained by BET and EG methods was explained in terms of the 'free surface area' and the 'apparent surface area' associated with these measurements.The previously reported surface area for soil organic matter (SOM) of 560-800 m2/g as determined by the ethylene glycol (EG) retention method was reexamined by the standard BET method based on nitrogen adsorption at liquid nitrogen temperature. Test samples consisted of two high organic content soils, a freeze-dried soil humic acid, and an oven-dried soil humic acid. The measured BET areas for these samples were less than 1 m2/g, except for the freeze-dried humic acid. The results suggest that surface adsorption of nonionic organic compounds by SOM is practically insignificant in comparison to uptake by partition. The discrepancy between the surface areas of SOM obtained by BET and EG methods was explained in terms of the 'free surface area' and the 'apparent surface area' associated with these measurements.

Determination of end point of primary drying in freeze-drying process control.

PubMed

Patel, Sajal M; Doen, Takayuki; Pikal, Michael J

2010-03-01

Freeze-drying is a relatively expensive process requiring long processing time, and hence one of the key objectives during freeze-drying process development is to minimize the primary drying time, which is the longest of the three steps in freeze-drying. However, increasing the shelf temperature into secondary drying before all of the ice is removed from the product will likely cause collapse or eutectic melt. Thus, from product quality as well as process economics standpoint, it is very critical to detect the end of primary drying. Experiments were conducted with 5% mannitol and 5% sucrose as model systems. The apparent end point of primary drying was determined by comparative pressure measurement (i.e., Pirani vs. MKS Baratron), dew point, Lyotrack (gas plasma spectroscopy), water concentration from tunable diode laser absorption spectroscopy, condenser pressure, pressure rise test (manometric temperature measurement or variations of this method), and product thermocouples. Vials were pulled out from the drying chamber using a sample thief during late primary and early secondary drying to determine percent residual moisture either gravimetrically or by Karl Fischer, and the cake structure was determined visually for melt-back, collapse, and retention of cake structure at the apparent end point of primary drying (i.e., onset, midpoint, and offset). By far, the Pirani is the best choice of the methods tested for evaluation of the end point of primary drying. Also, it is a batch technique, which is cheap, steam sterilizable, and easy to install without requiring any modification to the existing dryer.

Optimization of protectant, salinity and freezing condition for freeze-drying preservation of Edwardsiella tarda

NASA Astrophysics Data System (ADS)

Yu, Yongxiang; Zhang, Zheng; Wang, Yingeng; Liao, Meijie; Li, Bin; Xue, Liangyi

2017-10-01

Novel preservation condition without ultra-low temperature is needed for the study of pathogen in marine fishes. Freeze-drying is such a method usually used for preservation of terrigenous bacteria. However, studies using freeze-drying method to preserving marine microorganisms remain very limited. In this study, we optimized the composition of protectants during the freeze-drying of Edwardsiella tarda, a fish pathogen that causes systemic infection in marine fishes. We found that the optimal composition of protectant mixture contained trehalose (8.0%), skim milk (12.0%), sodium citrate (2.0%), serum (12.0%) and PVP (2.0%). Orthogonal and interaction analyses demonstrated the interaction between serum and skim milk or sodium citrate. The highest survival rate of E. tarda was observed when the concentration of NaCl was 10.0, 30.0 and between 5.0 and 10.0 g L-1 for preparing TSB medium, E. tarda suspension and protectant mixture, respectively. When E. tarda was frozen at -80°C or -40°C for 6 h, its survival rate was higher than that under other tested conditions. Under the optimized conditions, when the protectant mixture was used during freeze-drying process, the survival rate (79.63%-82.30%) of E. tarda was significantly higher than that obtained using single protectant. Scanning electron microscopy (SEM) image indicated that E. tarda was embedded in thick matrix with detectable aggregation. In sum, the protectant mixture may be used as a novel cryoprotective additive for E. tarda.

Product mass transfer resistance directly determined during freeze-drying cycle runs using tunable diode laser absorption spectroscopy (TDLAS) and pore diffusion model.

PubMed

Kuu, Wei Y; O'Bryan, Kevin R; Hardwick, Lisa M; Paul, Timothy W

2011-08-01

The pore diffusion model is used to express the dry layer mass transfer resistance, [Formula: see text], as a function of the ratio r(e)/?, where r(e) is the effective pore radius and ? is the tortuosity factor of the dry layer. Using this model, the effective pore radius of the dry layer can be estimated from the sublimation rate and product temperature profiles measured during primary drying. Freeze-drying cycle runs were performed using the LyoStar II dryer (FTS Systems), with real-time sublimation rate profiles during freeze drying continuously measured by tunable diode laser absorption spectroscopy (TDLAS). The formulations chosen for demonstration of the proposed approach include 5% mannitol, 5% sucrose, 5% lactose, 3% mannitol plus 2% sucrose, and a parenteral nutrition formulation denoted VitaM12. The three different methods used for determination of the product resistance are: (1) Using both the sublimation rate and product temperature profiles, (2) using the sublimation rate profile alone, and (3) using the product temperate profile alone. Unlike the second and third methods, the computation procedure of first method does not need solution of the complex heat and mass transfer equations.

Optimization of the freeze-drying cycle: adaptation of the pressure rise analysis model to non-instantaneous isolation valves.

PubMed

Chouvenc, P; Vessot, S; Andrieu, J; Vacus, P

2005-01-01

The principal aim of this study is to extend to a pilot freeze-dryer equipped with a non-instantaneous isolation valve the previously presented pressure rise analysis (PRA) model for monitoring the product temperature and the resistance to mass transfer of the dried layer during primary drying. This method, derived from the original MTM method previously published, consists of interrupting rapidly (a few seconds) the water vapour flow from the sublimation chamber to the condenser and analysing the resulting dynamics of the total chamber pressure increase. The valve effect on the pressure rise profile observed during the isolation valve closing period was corrected by introducing in the initial PRA model a valve characteristic function factor which turned out to be independent of the operating conditions. This new extended PRA model was validated by implementing successively the two types of valves and by analysing the pressure rise kinetics data with the corresponding PRA models in the same operating conditions. The coherence and consistency shown on the identified parameter values (sublimation front temperature, dried layer mass transfer resistance) allowed validation of this extended PRA model with a non-instantaneous isolation valve. These results confirm that the PRA method, with or without an instantaneous isolation valve, is appropriate for on-line monitoring of product characteristics during freeze-drying. The advantages of PRA are that the method is rapid, non-invasive, and global. Consequently, PRA might become a powerful and promising tool not only for the control of pilot freeze-dryers but also for industrial freeze-dryers equipped with external condensers.

Determination of mass and heat transfer parameters during freeze-drying cycles of pharmaceutical products.

PubMed

Hottot, A; Vessot, S; Andrieu, J

2005-01-01

The principal aim of this study was to evaluate the water vapour mass transfer resistance of the dried layer and the vial heat transfer coefficient values of a pharmaceutical product during the primary drying period. First, overall vial heat transfer coefficient values, Kv, were determined by a gravimetric method based on pure ice sublimation experiments. Thus, it was possible to set up a map of the total heat flux received by each vial throughout the plate surface of our pilot scale freeze-dryer. Important heterogeneities were observed for the vials placed at the plate edges and for the vials placed at the center of the plate. As well, the same gravimetric method was also used to precisely determine the influence of main lyophilization operating parameters (shelf temperature and gas total pressure) or the vial types and sizes on these overall heat transfer coefficient values. A semi-empirical relationship as a function of total gas pressure was proposed. The transient method by pressure rise analysis (PRA method) after interrupting the water vapour flow between the sublimation chamber and the condenser, previously set up and validated in our laboratory, was then extensively used with an amorphous BSA-based formulation to identify the dried layer mass transfer resistance values, Rp, the ice front temperature, and the total heat transfer coefficient values, Kv, with or without annealing treatment. It was proved that this method gave accurate and coherent data only during the first half of the sublimation period when the totality of the vials of the set was still sublimating. Thus, this rapid method allowed estimation of, on line and in situ, the sublimation front temperature and the characterization of the morphology and structure of the freeze-dried layer, all along the first part of the sublimation period. The estimated sublimation temperatures shown by the PRA model were about 2 degrees C lower than the experimental values obtained using thermocouples inserted inside the vial, in accordance with previous data given by this method for similar freeze-drying conditions. As well, by using this method we could confirm the homogenization of the dried layer porous structure by annealing treatment after the freezing step. Furthermore, frozen matrix structure analysis (mean pore diameter) using optical microscopy and mass transfer modelling of water vapour by molecular diffusion (Knudsen regime) allowed, in some cases, to predict the experimental values of this overall mass transfer resistance directly related to the freeze-dried cake permeability.

Freeze drying for morphological control of inter-penetrating polymer networks

NASA Technical Reports Server (NTRS)

Hansen, Marion G.; Pater, Ruth H.

1990-01-01

The intrinsic brittleness of BMI resins can be reduced through the creation of an interpenetrating network (IPN) of BMI with a reactive-encapped thermoplastic, such as the presently considered polyimidesulfone, PISO2. The PISO2 and BMI were dissolved in a common solvent, which was then removed from the constituents by freeze drying; in an alternative method, an IPN was formed through dissolution of the constituent in a common solvent with either high or low melting point, followed by evaporative removal of the solvent. The effectiveness of the freeze-drying approach for morphological control is evaluated.

Vitamin A Activity of Rice-based Weaning Foods Enriched with Germinated Cowpea Flour, Banana, Pumpkin and Milk Powder.

PubMed

Hashim, N; Pongjata, J

2000-03-01

The objective of this study was to identify the effect of different drying methods on vitamin A activity of formulated weaning food. Weaned foods on vitamin A activity of formulated using treated cowpea flour, locally available rice flour, banana-pumpkin, skim milk powder and sugar in the ratio 35:35:15:15:5. Treated cowpea flour consisted of original cowpea flour, 24 h germinated cowpea flour. Each treated flour was mixed separately with the other ingredients and cooked into a slurry. Each mixture was either oven-dried or freeze-dried to produce a dry flaky mixture. The carotenoid composition of the product was determined by HPLC. Vitamin A activity of oven-dried weaning food was significantly reduced (p<0.05) compared to freeze-dried weaning food. The freeze-dried weaning foods showed a higher retinol equivalent than oven-dried weaning foods for all treatments. The results of the study found that an intake of 100 g of freeze-dried weaning foods enriched with banana-pumpkin and cowpea flour provided an adequate amount of the recommended daily allowance (RDA) of vitamin A for infants.

Biologically active antimicrobial and antioxidant substances in the Helianthus annuus L. bee pollen.

PubMed

Fatrcová-Šramková, Katarína; Nôžková, Janka; Máriássyová, Magda; Kačániová, Miroslava

2016-01-01

The objective of this study was to measure the content of flavonoids, polyphenols, and carotenoids in the Helianthus annuus L. bee pollen. It was also to evaluate the ability of the dried, frozen, and freeze-dried extracts of sunflower (H. annuus) pollen, its scavenged free radicals and reducing action. Another aim of this study was to investigate the antimicrobial in vitro action of the H. annuus pollen extracts against the Gram-positive and Gram-negative bacteria and fungi. All pollen extracts showed medium antiradical activity and reductive ability. The most effective was the freeze-dried extract in both evaluation systems. The evaluation of the protective effects of DNA using a biosensor showed an opposite trending-frozen ˃ dried ˃ freeze-dried pollen. For the evaluation of antiradical activity, the DPPH method was used, and reductive ability was assessed by means of phosphomolybdic complex formation. The comparison of the polyphenols content shows higher values in freeze-dried bee pollen than in the dried and frozen pollen. The highest content of flavonoids was found in the frozen samples and the most carotenoids were present in the dried samples. In our study, the best antibacterial effects of the dried sunflower bee pollen extracts were found against Paenibacillus larvae, Pseudomonas aeruginosa, and Enterococcus raffinosus. The best inhibitory properties of the frozen sunflower bee pollen extracts were found against Escherichia coli, Pseudomonas aeruginosa, and Paenibacillus larvae. Very good inhibitory effects of freeze-dried sunflower bee pollen were found against Paenibacillus larvae, Brochotrix thermosphacta, and Enterococcus raffinosus. The best antifungal activity of the sunflower bee pollen was found in the frozen bee pollen extracts against Aspergillus ochraceus and freeze-dried bee pollen extracts against Aspergillus niger.

Effect of drying on the bioactive compounds, antioxidant, antibacterial and antityrosinase activities of pomegranate peel.

PubMed

Mphahlele, Rebogile R; Fawole, Olaniyi A; Makunga, Nokwanda P; Opara, Umezuruike L

2016-05-26

The use of pomegranate peel is highly associated with its rich phenolic concentration. Series of drying methods are recommended since bioactive compounds are highly sensitive to thermal degradation. The study was conducted to evaluate the effects of drying on the bioactive compounds, antioxidant as well as antibacterial and antityrosinase activities of pomegranate peel. Dried pomegranate peels with the initial moisture content of 70.30 % wet basis were prepared by freeze and oven drying at 40, 50 and 60 °C. Difference in CIE-LAB, chroma (C*) and hue angle (h°) were determined using colorimeter. Individual polyphenol retention was determined using LC-MS and LC-MS(E) while total phenolics concentration (TPC), total flavonoid concentration (TFC), total tannins concentration (TTC) and vitamin C concentration were measured using colorimetric methods. The antioxidant activity was measured by radical scavenging activity (RSA) and ferric reducing antioxidant power (FRAP). Furthermore, the antibacterial activity of methanolic peel extracts were tested on Gram negative (Escherichia coli and Klebsiella pneumonia) and Gram positive bacteria (Staphylococcus aureus and Bacillus subtilis) using the in vitro microdilution assays. Tyrosinase enzyme inhibition was investigated against monophenolase (tyrosine) and diphenolase (DOPA), with arbutin as positive controls. Oven drying at 60 °C resulted in high punicalin concentration (888.04 ± 141.03 mg CE/kg dried matter) along with poor red coloration (high hue angle). Freeze dried peel contained higher catechin concentration (674.51 mg/kg drying matter) + catechin and -epicatechin (70.56 mg/kg drying matter) compared to oven dried peel. Furthermore, freeze dried peel had the highest total phenolic, tannin and flavonoid concentrations compared to oven dried peel over the temperature range studied. High concentration of vitamin C (31.19 μg AAE/g dried matter) was observed in the oven dried (40 °C) pomegranate peel. Drying at 50 °C showed the highest inhibitory activity with the MIC values of 0.10 mg/ml against Gram positive (Staphylococcus aureus and Bacillus subtili. Likewise, the extracts dried at 50 °C showed potent inhibitory activity concentration (22.95 mg/ml) against monophenolase. Principal component analysis showed that the peel colour characteristics and bioactive compounds isolated the investigated drying method. The freeze and oven dried peel extracts exhibited a significant antibacterial and antioxidant activities. The freeze drying method had higher total phenolic, tannin and flavonoid concentration therefore can be explored as a feasible method for processing pomegranate peel to ensure retention of the maximum amount of their naturally occurring bioactive compounds. Not relevant for this study.

Annealing to optimize the primary drying rate, reduce freezing-induced drying rate heterogeneity, and determine T(g)' in pharmaceutical lyophilization.

PubMed

Searles, J A; Carpenter, J F; Randolph, T W

2001-07-01

In a companion paper we show that the freezing of samples in vials by shelf-ramp freezing results in significant primary drying rate heterogeneity because of a dependence of the ice crystal size on the nucleation temperature during freezing.1 The purpose of this study was to test the hypothesis that post-freezing annealing, in which the product is held at a predetermined temperature for a specified duration, can reduce freezing-induced heterogeneity in sublimation rates. In addition, we test the impact of annealing on primary drying rates. Finally, we use the kinetics of relaxations during annealing to provide a simple measurement of T(g)', the glass transition temperature of the maximally freeze-concentrated amorphous phase, under conditions and time scales most appropriate for industrial lyophilization cycles. Aqueous solutions of hydroxyethyl starch (HES), sucrose, and HES:sucrose were either frozen by placement on a shelf while the temperature was reduced ("shelf-ramp frozen") or by immersion into liquid nitrogen. Samples were then annealed for various durations over a range of temperatures and partially lyophilized to determine the primary drying rate. The morphology of fully dried liquid nitrogen-frozen samples was examined using scanning electron microscopy. Annealing reduced primary drying rate heterogeneity for shelf-ramp frozen samples, and resulted in up to 3.5-fold increases in the primary drying rate. These effects were due to increased ice crystal sizes, simplified amorphous structures, and larger and more numerous holes on the cake surface of annealed samples. Annealed HES samples dissolved slightly faster than their unannealed counterparts. Annealing below T(g)' did not result in increased drying rates. We present a simple new annealing-lyophilization method of T(g)' determination that exploits this phenomenon. It can be carried out with a balance and a freeze-dryer, and has the additional advantage that a large number of candidate formulations can be evaluated simultaneously.

A Method of Lyophilizing Vaccines Containing Aluminum Salts into a Dry Powder Without Causing Particle Aggregation or Decreasing the Immunogenicity Following Reconstitution

PubMed Central

Li, Xinran; Thakkar, Sachin G.; Ruwona, Tinashe B.; Williams, Robert O.; Cui, Zhengrong

2015-01-01

Many currently licensed and commercially available human vaccines contain aluminum salts as vaccine adjuvants. A major limitation with these vaccines is that they must not be exposed to freezing temperatures during transport or storage such that the liquid vaccine freezes, because freezing causes irreversible coagulation that damages the vaccines (e.g., loss of efficacy). Therefore, vaccines that contain aluminum salts as adjuvants are formulated as liquid suspensions and are required to be kept in cold chain (2–8°C) during transport and storage. Formulating vaccines adjuvanted with aluminum salts into dry powder that can be readily reconstituted before injection may address the limitation. Spray freeze-drying of vaccines with low concentrations of aluminum salts and high concentrations of trehalose alone, or a mixture of sugars and amino acids, as excipients can convert vaccines containing aluminum salts into dry powder, but fails to preserve the particle size and/or immunogenicity of the vaccines. In the present study, using ovalbumin as a model antigen adsorbed onto aluminum hydroxide or aluminum phosphate, a commercially available tetanus toxoid vaccine adjuvanted with potassium alum, a human hepatitis B vaccine adjuvanted with aluminum hydroxide, and a human papillomavirus vaccine adjuvanted with aluminum hydroxyphosphate sulfate, it was shown that vaccines containing a relatively high concentration of aluminum salts (i.e., up to ~1%, w/v, of aluminum hydroxide) can be converted into a dry powder by thin-film freezing followed by removal of the frozen solvent by lyophilization while using low levels of trehalose (i.e., as low as 2% w/v) as an excipient. Importantly, the thin-film freeze-drying process did not cause particle aggregation, nor decreased the immunogenicity of the vaccines. Moreover, repeated freezing-and-thawing of the dry vaccine powder did not cause aggregation. Thin-film freeze-drying is a viable platform technology to produce dry powders of vaccines that contain aluminum salts. PMID:25735896

Production of freeze-dried yeast culture for the brewing of traditional sorghum beer, tchapalo.

PubMed

N'Guessan, Florent K; Coulibaly, Hermann W; Alloue-Boraud, Mireille W A; Cot, Marlène; Djè, Koffi Marcellin

2016-01-01

Freeze-drying is a well-known dehydration method widely used to preserve microorganisms. In order to produce freeze-dried yeast starter culture for the brewing purpose of African sorghum beer, we tested protective agents (sucrose, glucose, glycerol) in combination with support materials (millet, maize, sorghum, and cassava flours) at 1:1 ratio (v/v). The yeast strains Saccharomyces cerevisiae F 12-7 and Candida tropicalis C 0-7 previously isolated from sorghum beer were used in a mixed culture at a ratio of 2:1 (C. tropicalis/S. cerevisiae). After the freeze-drying, the residual water contents were between 0.78 -2.27%, 0.55 -4.09%, and 0.40-2.61%, respectively, with sucrose, glucose and glycerol. The dried yeasts viabilities were between 4.0% and 10.6%. Among the protective agents used, sucrose was found to be the best protectant giving cell viabilities of 8.4-10.6%. Considering the support materials, millet flour was the best support after drying. When the freeze-dried yeast powders were stored at 4°C and room temperature (25-28°C) for up to 3 months, the survival rates were the highest with cassava flour as the support material.

Effect of cryoprotectants on the porosity and stability of insulin-loaded PLGA nanoparticles after freeze-drying

PubMed Central

Fonte, Pedro; Soares, Sandra; Costa, Ana; Andrade, José Carlos; Seabra, Vítor; Reis, Salette; Sarmento, Bruno

2012-01-01

PLGA nanoparticles are useful to protect and deliver proteins in a localized or targeted manner, with a long-term systemic delivery pattern intended to last for a period of time, depending on polymer bioerosion and biodegradability. However, the principal concern regarding these carriers is the hydrolytic instability of polymer in aqueous suspension. Freeze-drying is a commonly used method to stabilize nanoparticles, and cryoprotectants may be also used, to even increase its physical stability. The aim of the present work was to analyze the influence of cryoprotectants on nanoparticle stability and porosity after freeze-drying, which may influence protein release and stability. It was verified that freeze-drying significantly increased the number of pores on PLGA-NP surface, being more evident when cryoprotectants are added. The presence of pores is important in a lyophilizate to facilitate its reconstitution in water, although this may have consequences to protein release and stability. The release profile of insulin encapsulated into PLGA-NP showed an initial burst in the first 2 h and a sustained release up to 48 h. After nanoparticles freeze-drying the insulin release increased about 18% in the first 2 h due to the formation of pores, maintaining a sustained release during time. After freeze-drying with cryoprotectants, the amount of insulin released was higher for trehalose and lower for sucrose, glucose, fructose and sorbitol comparatively to freeze-dried PLGA-NP with no cryoprotectant added. Besides the porosity, the ability of cryoprotectants to be adsorbed on the nanoparticles surface may also play an important role on insulin release and stability. PMID:23507897

Short communication: Effects of vacuum freeze-drying on inactivation of Cronobacter sakazakii ATCC29544 in liquid media with different initial inoculum levels.

PubMed

Jiao, Rui; Gao, Jina; Zhang, Xiyan; Zhang, Maofeng; Chen, Jiren; Wu, Qingping; Zhang, Jumei; Ye, Yingwang

2017-03-01

Vacuum freeze-drying is an important food-processing technology for valid retention of nutrients and bioactive compounds. Cronobacter sakazakii has been reported to be associated with severe infections in neonates through consumption of contaminated powdered infant formula. In this study, effects of vacuum freeze-drying treatment for 12, 24, and 36 h on inactivation of C. sakazakii with different initial inoculum levels in sterile water, tryptic soy broth (TSB), skim milk, and whole milk were determined. Results indicated that the lethality rate of C. sakazakii in each sample increased with the extension of vacuum freeze-drying time. With initial inoculum levels of 10 2 and 10 3 cfu/mL, the survival of C. sakazakii in different liquid media was significantly affected by vacuum freeze-drying for 12, 24, and 36 h. In addition, the lethality rates of C. sakazakii in whole milk, skim milk, and TSB was significantly reduced compared with those in sterile water. Furthermore, whole milk showed the strongest protective role for C. sakazakii cells, followed by skim milk and TSB medium. Using the scanning electron microscope, the intracellular damage and obvious distortion of C. sakazakii cells were observed after vacuum freeze-drying for 24 and 36 h compared with the untreated sample, and the injured cells increased with the extension of vacuum-drying time. We concluded that inactivation of vacuum freeze-drying on C. sakazakii cells is related to the food matrix, and a combination with other methods for inactivating C. sakazakii is required for ensuring microbial safety of powdered infant formula. Copyright © 2017 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

Effects of protectant and rehydration conditions on the survival rate and malolactic fermentation efficiency of freeze-dried Lactobacillus plantarum JH287.

PubMed

Lee, Sae-Byuk; Kim, Dong-Hwan; Park, Heui-Dong

2016-09-01

In this study, Lactobacillus plantarum JH287 was used as a malolactic fermentation starter in Campbell Early wine production. L. plantarum JH287 was first lyophilized, and the malolactic fermentation potential of freeze-dried L. plantarum JH287 was investigated. Different protective media and rehydration conditions were tested to improve the survival rate of freeze-dried L. plantarum JH287. Optimal protective medium contained 10 % sorbitol and 10 % skim milk. The optimal rehydration condition was a 1-h rehydration time conducted in the same protective media, and the combination of these two methods produced a survival rate of 86.37 %. In addition, a 77.71 % survival rate was achieved using freeze-dried samples that were stored at 4 °C for 2 months. Freeze-dried L. plantarum JH287 and Saccharomyces cerevisiae Fermivin were used to inoculate the Campbell Early grape must to decrease its malic acid content. Using this mixed-fermentation method, wine showed a decrease in malic acid content after 9 days of fermentation. GC-MS analysis detected 15 volatile ester compounds in the wine. A sensory evaluation showed that the taste and aroma of mix-fermented wine were better than those of the control that had not been inoculated with L. plantarum JH287.

Effect of freezing, hot tumble drying and washing with eucalyptus oil on house dust mites in soft toys.

PubMed

Chang, Chin-Fu; Wu, Francis Fu-Sheng; Chen, Chi-Ying; Crane, Julian; Siebers, Rob

2011-09-01

Soft toys are a major source of house dust mites (HDM) and HDM allergens, and sleeping with soft toys is a significant risk factor for HDM sensitization. We studied three techniques to eliminate HDM from soft toys, namely freezing, hot tumble drying and washing with eucalyptus oil. Thirty-six toys (12 in each treatment group) were enumerated for live HDM by the heat escape method before and after freezing overnight, hot tumble drying for 1 h and washing in 0.2% to 0.4% eucalyptus oil. Freezing, hot tumble drying and washing with eucalyptus oil resulted in significant reductions in live HDM, an average reduction of 95.1%, 89.1% and 95.1%, respectively. Additionally, washing with eucalyptus oil resulted in a significant reduction in HDM allergens as well from a geometric mean of 9.12 μg/g to 0.37 μg/g (p = 0.033). These three HDM elimination techniques give parents of infants effective and acceptable methods of limiting HDM exposure. © 2011 John Wiley & Sons A/S.

Improvement of fish freshness determination method by the application of amorphous freeze-dried enzymes.

PubMed

Srirangsan, Paveena; Hamada-Sato, Naoko; Kawai, Kiyoshi; Watanabe, Manabu; Suzuki, Toru

2010-12-08

Alkaline phosphatase (ALP), nucleoside phosphorylase (NP), and xanthine oxidase (XOD) were used in a colorimetric method for evaluation of fish freshness based on the Ki value. Two enzyme mixtures, NP-XOD and ALP-NP-XOD, were prepared with a color developing agent, and stabilities of the enzymes were improved by freeze-drying with glass-forming additives, i.e., sucrose and sucrose-gelatin. As a result, a linear relationship was obtained between the Ki values determined by the developed colorimetric method and a conventional high-performance liquid chromatography with a high correlation coefficient of 0.997. All enzyme samples containing the additive(s) were amorphous, and higher enzymes activities were maintained compared to those freeze-dried without an additive. Sucrose-gelatin/enzyme mixtures showed higher glass transition temperature; consequently, the enzymes were better stabilized than the sucrose/enzyme formulations. Using the sucrose-gelatin/enzyme mixture, Ki values of fish meat could be accurately determined even after 6-month storage of the dried enzymes at 40 °C.

On the use of tert-butanol/water cosolvent systems in production and freeze-drying of poly-ε-caprolactone nanoparticles.

PubMed

Zelenková, Tereza; Barresi, Antonello A; Fissore, Davide

2015-01-01

This work deals with the use of a water/tert-butyl alcohol (TBA) system in the manufacturing process of poly-ε-caprolactone (PCL) nanoparticles, namely in the synthesis stage, using the solvent displacement method in a confined impinging jet mixer (CIJM), and in the following freeze-drying stage. The experimental investigation evidenced that the nanoparticles size is significantly reduced with respect to the case where acetone is the solvent. Besides, the solvent evaporation step is not required before freeze-drying as TBA is fully compatible with the freeze-drying process. The effect of initial polymer concentration, flow rate, water to TBA flow rate ratio, and quench volumetric ratio on the mean nanoparticles size was investigated, and a simple equation was proposed to relate the mean nanoparticles size to these operating parameters. Then, freeze-drying of the nanoparticles suspensions was studied. Lyoprotectants (sucrose and mannitol) and steric stabilizers (Cremophor EL and Poloxamer 388) have to be used to avoid nanoparticles aggregation, thus preserving particle size distribution and mean nanoparticles size. Their effect, as well as that of the heating shelf temperature, has been investigated by means of statistical techniques, with the goal to identify which of these factors, or combination of factors, plays the key role in the nanoparticles size preservation at the end of the freeze-drying process. © 2014 Wiley Periodicals, Inc. and the American Pharmacists Association.

Improving survival and storage stability of bacteria recalcitrant to freeze-drying: a coordinated study by European culture collections.

PubMed

Peiren, Jindrich; Buyse, Joke; De Vos, Paul; Lang, Elke; Clermont, Dominique; Hamon, Sylviane; Bégaud, Evelyne; Bizet, Chantal; Pascual, Javier; Ruvira, María A; Macián, M Carmen; Arahal, David R

2015-04-01

The objective of this study is to improve the viability after freeze-drying and during storage of delicate or recalcitrant strains safeguarded at biological resource centers. To achieve this objective, a joint experimental strategy was established among the different involved partner collections of the EMbaRC project ( www.embarc.eu ). Five bacterial strains considered as recalcitrant to freeze-drying were subjected to a standardized freeze-drying protocol and to seven agreed protocol variants. Viability of these strains was determined before and after freeze-drying (within 1 week, after 6 and 12 months, and after accelerated storage) for each of the protocols. Furthermore, strains were exchanged between partners to perform experiments with different freeze-dryer-dependent parameters. Of all tested variables, choice of the lyoprotectant had the biggest impact on viability after freeze-drying and during storage. For nearly all tested strains, skim milk as lyoprotectant resulted in lowest viability after freeze-drying and storage. On the other hand, best freeze-drying and storage conditions were strain and device dependent. For Aeromonas salmonicida CECT 894(T), best survival was obtained when horse serum supplemented with trehalose was used as lyoprotectant, while Aliivibrio fischeri LMG 4414(T) should be freeze-dried in skim milk supplemented with marine broth in a 1:1 ratio. Freeze-drying Campylobacter fetus CIP 53.96(T) using skim milk supplemented with trehalose as lyoprotectant resulted in best recovery. Xanthomonas fragariae DSM 3587(T) expressed high viability after freeze-drying and storage for all tested lyoprotectants and could not be considered as recalcitrant. In contrary, Flavobacterium columnare LMG 10406(T) did not survive the freeze-drying process under all tested conditions.

Influence of drying method on the surface energy of cellulose nanofibrils determined by inverse gas chromatography

Treesearch

Yucheng Peng; Douglas J. Gardner; Yousoo Han; Zhiyong Cai; Mandla A. Tshabalala

2013-01-01

Research and development of the renewable nanomaterial cellulose nanofibrils (CNFs) has received considerable attention. The effect of drying on the surface energy of CNFs was investigated. Samples of nanofibrillated cellulose (NFC) and cellulose nanocrystals (CNC) were each subjected to four separate drying methods: air-drying, freeze-drying, spray-drying, and...

Developments in the formulation and delivery of spray dried vaccines.

PubMed

Kanojia, Gaurav; Have, Rimko Ten; Soema, Peter C; Frijlink, Henderik; Amorij, Jean-Pierre; Kersten, Gideon

2017-10-03

Spray drying is a promising method for the stabilization of vaccines, which are usually formulated as liquids. Usually, vaccine stability is improved by spray drying in the presence of a range of excipients. Unlike freeze drying, there is no freezing step involved, thus the damage related to this step is avoided. The edge of spray drying resides in its ability for particles to be engineered to desired requirements, which can be used in various vaccine delivery methods and routes. Although several spray dried vaccines have shown encouraging preclinical results, the number of vaccines that have been tested in clinical trials is limited, indicating a relatively new area of vaccine stabilization and delivery. This article reviews the current status of spray dried vaccine formulations and delivery methods. In particular it discusses the impact of process stresses on vaccine integrity, the application of excipients in spray drying of vaccines, process and formulation optimization strategies based on Design of Experiment approaches as well as opportunities for future application of spray dried vaccine powders for vaccine delivery.

Encapsulation of black carrot juice using spray and freeze drying.

PubMed

Murali, S; Kar, Abhijit; Mohapatra, Debabandya; Kalia, Pritam

2015-12-01

Black carrot juice extracted using pectinase enzyme was encapsulated in three different carrier materials (maltodextrin 20DE, gum arabic and tapioca starch) using spray drying at four inlet temperatures (150, 175, 200 and 225 ℃) and freeze drying at a constant temperature of - 53 ℃ and vacuum of 0.22-0.11 mbar with the constant feed mixture. The products were analyzed for total anthocyanin content, antioxidant activity, water solubility index, encapsulation efficiency and total colour change. For both the drying methods followed in this study, maltodextrin 20DE as the carrier material has proven to be better in retaining maximum anthocyanin and antioxidant activity compared to gum arabic and tapioca starch. The best spray dried product, was obtained at 150 ℃. The most acceptable was the freeze dried product with maximum anthocyanin content, antioxidant activity, water solubility index, encapsulation efficiency and colour change. © The Author(s) 2014.

Drying-induced physico-chemical changes in cranberry products.

PubMed

Michalska, Anna; Wojdyło, Aneta; Honke, Joanna; Ciska, Ewa; Andlauer, Wilfried

2018-02-01

Sugar-free cranberry juice (XAD) and juice with 15% of maltodextrin were dried by freeze-, vacuum and spray drying methods. Total phenolics (589-6435mg/kg dry matter) including 5 flavonols, 3 phenolic acids, 2 procyanidins and 5 anthocyanins were stronger affected by juice formulation than by drying methods. Spray drying of juice, regardless of its formulation, was competitive to freeze drying in terms of polyphenols' retention. Increase in temperature up to 100°C during vacuum drying of XAD extracts resulted in degradation of polyphenolics (down to 4%), except chlorogenic acid. Its content increased with rise in temperature and accelerated hydroxymethylfurfural formation. The stronger the impact of drying, the more chlorogenic acid is present in cranberry products. In all powders analysed, formation of furoylmethyl amino acids was noted. Antioxidant capacity of cranberry products was influenced by juice formulation and was linked to content of polyphenols. Copyright © 2017 Elsevier Ltd. All rights reserved.

Quantification and characterisation of fatty acid methyl esters in microalgae: Comparison of pretreatment and purification methods.

PubMed

Lage, Sandra; Gentili, Francesco G

2018-06-01

A systematic qualitative and quantitative analysis of fatty acid methyl esters (FAMEs) is crucial for microalgae species selection for biodiesel production. The aim of this study is to identify the best method to assess microalgae FAMEs composition and content. A single-step method, was tested with and without purification steps-that is, separation of lipid classes by thin-layer chromatography (TLC) or solid-phase extraction (SPE). The efficiency of a direct transesterification method was also evaluated. Additionally, the yield of the FAMEs and the profiles of the microalgae samples with different pretreatments (boiled in isopropanol, freezing, oven-dried and freeze-dried) were compared. The application of a purification step after lipid extraction proved to be essential for an accurate FAMEs characterisation. The purification methods, which included TLC and SPE, provided superior results compared to not purifying the samples. Freeze-dried microalgae produced the lowest FAMEs yield. However, FAMEs profiles were generally equivalent among the pretreatments. Copyright © 2018 Elsevier Ltd. All rights reserved.

Computational analysis of fluid dynamics in pharmaceutical freeze-drying.

PubMed

Alexeenko, Alina A; Ganguly, Arnab; Nail, Steven L

2009-09-01

Analysis of water vapor flows encountered in pharmaceutical freeze-drying systems, laboratory-scale and industrial, is presented based on the computational fluid dynamics (CFD) techniques. The flows under continuum gas conditions are analyzed using the solution of the Navier-Stokes equations whereas the rarefied flow solutions are obtained by the direct simulation Monte Carlo (DSMC) method for the Boltzmann equation. Examples of application of CFD techniques to laboratory-scale and industrial scale freeze-drying processes are discussed with an emphasis on the utility of CFD for improvement of design and experimental characterization of pharmaceutical freeze-drying hardware and processes. The current article presents a two-dimensional simulation of a laboratory scale dryer with an emphasis on the importance of drying conditions and hardware design on process control and a three-dimensional simulation of an industrial dryer containing a comparison of the obtained results with analytical viscous flow solutions. It was found that the presence of clean in place (CIP)/sterilize in place (SIP) piping in the duct lead to significant changes in the flow field characteristics. The simulation results for vapor flow rates in an industrial freeze-dryer have been compared to tunable diode laser absorption spectroscopy (TDLAS) and gravimetric measurements.

Hydroxypropyl-ß-cyclodextrin as a membrane protectant during freeze-drying of hydrogenated and non-hydrogenated liposomes and molecule-in-cyclodextrin-in- liposomes: Application to trans-anethole.

PubMed

Gharib, Riham; Greige-Gerges, Hélène; Fourmentin, Sophie; Charcosset, Catherine

2018-11-30

The effect of hydrogenation of phospholipids on the characteristics of freeze-dried liposomes was investigated using hydroxypropyl-ß-cyclodextrin (HP-ß-CD) as membrane protectant. The ethanol-injection method was applied to prepare liposomes using hydrogenated (Phospholopion-90H and 80H) and non-hydrogenated phospholipids (Lipoid-S100) in combination with cholesterol. Various liposomal formulations were tested: conventional liposomes (CL) and HP-ß-CD-loaded liposomes (CDL). Liposome suspensions were concentrated by ultracentrifugation; the pellets were reconstituted in water or CD solution and the dispersions were characterized for their size, polydispersity index and zeta potential. Results demonstrated that HP-ß-CD protected only the hydrogenated batches (CL and CDL) during freeze-drying. Moreover, the presence of HP-ß-CD in the aqueous phase of CDL protected them during freeze-drying. Freeze-dried CL and CDL made of phospholipon-90H loading anethole were demonstrated to be physically stable upon reconstitution in HP-ß-CD solutions, and are able to retain anethole after 6 months of storage at 4 °C thereby making them valuable for food applications. Copyright © 2017 Elsevier Ltd. All rights reserved.

Resin impregnation of cellulose nanofibril films facilitated by water swelling

Treesearch

Yan Qing; Ronald Sabo; Zhiyong Cai; Yiqiang Wu

2013-01-01

Flexible composite films were produced by impregnating aqueous phenol formaldehyde (PF) resin into water-swollen cellulose nanofibril (CNF) films. CNF films were prepared using a pressurized filtration method in combination with freeze drying. The freeze-dried films were swollen with water then impregnated with PF resin by soaking in aqueous resin solutions of varying...

Evaluation of spin freezing versus conventional freezing as part of a continuous pharmaceutical freeze-drying concept for unit doses.

PubMed

De Meyer, L; Van Bockstal, P-J; Corver, J; Vervaet, C; Remon, J P; De Beer, T

2015-12-30

Spin-freezing as alternative freezing approach was evaluated as part of an innovative continuous pharmaceutical freeze-drying concept for unit doses. The aim of this paper was to compare the sublimation rate of spin-frozen vials versus traditionally frozen vials in a batch freeze-dryer, and its impact on total drying time. Five different formulations, each having a different dry cake resistance, were tested. After freezing, the traditionally frozen vials were placed on the shelves while the spin-frozen vials were placed in aluminum vial holders providing radial energy supply during drying. Different primary drying conditions and chamber pressures were evaluated. After 2h of primary drying, the amount of sublimed ice was determined in each vial. Each formulation was monitored in-line using NIR spectroscopy during drying to determine the sublimation endpoint and the influence of drying conditions upon total drying time. For all tested formulations and applied freeze-drying conditions, there was a significant higher sublimation rate in the spin-frozen vials. This can be explained by the larger product surface and the lower importance of product resistance because of the much thinner product layers in the spin frozen vials. The in-line NIR measurements allowed evaluating the influence of applied drying conditions on the drying trajectories. Copyright © 2015 Elsevier B.V. All rights reserved.

Aseptic Freeze-Dried versus Sterile Wet-Packaged Human Cadaveric Acellular Dermal Matrix in Immediate Tissue Expander Breast Reconstruction: A Propensity Score Analysis.

PubMed

Hanson, Summer E; Meaike, Jesse D; Selber, Jesse C; Liu, Jun; Li, Liang; Hassid, Victor J; Baumann, Donald P; Butler, Charles E; Garvey, Patrick B

2018-05-01

Although multiple acellular dermal matrix sources exist, it is unclear how its processing impacts complication rates. The authors compared complications between two preparations of human cadaveric acellular dermal matrix (freeze dried and ready-to-use) in immediate tissue expander breast reconstruction to analyze the effect of processing on complications. The authors retrospectively reviewed all alloplastic breast reconstructions with freeze-dried or ready-to-use human acellular dermal matrices between 2006 and 2016. The primary outcome measure was surgical-site occurrence defined as seroma, skin dehiscence, surgical-site infection, or reconstruction failure. The two groups were compared before and after propensity score matching. The authors included 988 reconstructions (freeze-dried, 53.8 percent; ready-to-use, 46.2 percent). Analysis of 384 propensity score-matched pairs demonstrated a slightly higher rate of surgical-site occurrence (21.4 percent versus 16.7 percent; p = 0.10) and surgical-site infection (9.6 percent versus 7.8 percent; p = 0.13) in the freeze-dried group than in the ready-to-use group, but the difference was not significant. However, failure was significantly higher for the freeze-dried versus ready-to-use group (7.8 percent versus 4.4 percent; p = 0.050). This is the largest study comparing the outcomes of alloplastic breast reconstruction using human acellular dermal matrix materials prepared by different methods. The authors demonstrated higher early complications with aseptic, freeze-dried matrix than with sterile ready-to-use matrix; reconstructive failure was the only outcome to achieve statistical significance. The authors conclude that acellular dermal matrix preparation has an independent impact on patient outcomes in their comparison of one company's product. Therapeutic, III.

[Freeze drying process optimization of ginger juice-adjuvant for Chinese materia medica processing and stability of freeze-dried ginger juice powder].

PubMed

Yang, Chun-Yu; Guo, Feng-Qian; Zang, Chen; Cao, Hui; Zhang, Bao-Xian

2018-02-01

Ginger juice， a commonly used adjuvant for Chinese materia medica， is applied in processing of multiple Chinese herbal decoction pieces. Because of the raw materials and preparation process of ginger juice， it is difficult to be preserved for a long time， and the dosage of ginger juice in the processing can not be determined base on its content of main compositions. Ginger juice from different sources is hard to achieve consistent effect during the processing of traditional Chinese herbal decoction pieces. Based on the previous studies， the freeze drying of ginger juice under different shelf temperatures and vacuum degrees were studied， and the optimized freeze drying condition of ginger juice was determined. The content determination method for 6-gingerol， 8-gingerol， 10-gingerol and 6-shagaol in ginger juice and redissolved ginger juice was established. The content changes of 6-gingerol， 8-gingerol， 10-gingerol， 6-gingerol， 6-shagaol， volatile oil and total phenol were studied through the drying process and 30 days preservation period. The results showed that the freeze drying time of ginger juice was shortened after process optimization; the compositions basically remained unchanged after freeze drying， and there was no significant changes in the total phenol content and gingerol content， but the volatile oil content was significantly decreased( P <0.05). Within 30 days， the contents of gingerol， total phenol， and volatile oil were on the decline as a whole. This study has preliminarily proved the feasibility of freeze-drying process of ginger juice as an adjuvant for Chinese medicine processing. Copyright© by the Chinese Pharmaceutical Association.

The Importance of Measuring Mercury in Wood

NASA Astrophysics Data System (ADS)

Yang, Y.; Yanai, R. D.; Driscoll, C. T.; Montesdeoca, M.

2014-12-01

Forests are important receptors of Hg deposition, and biological Hg hotspots occur mainly in forested regions, but few efforts have been made to determine the Hg content of trees. Mercury concentrations in stem tissue are lower than the foliage and bark, so low that they have often been below detection limits, especially in hardwood species. However, because wood is the largest component of forest biomass, it can be a larger Hg pool than the foliage, and thus quantifying concentrations in wood is important to Hg budgets in forests. The objective of our study was to determine the methods necessary to detect Hg in bole wood of four tree species, including two hardwoods and two conifers. We also evaluated the effect of air-drying and oven-drying samples on Hg recovery, compared to freeze-drying samples prior to analysis, which is the standard procedure. Many archived wood samples that were air-dried or oven-dried could be appropriate for Hg analysis if these methods could be validated; few are freeze-dried. We analyzed samples for total Hg using thermal decomposition, catalytic conversion, amalgamation, and atomic absorption spectrophotometry (Method 7473, USEPA 1998). The result of the method detection limit study was 1.27 ng g-1, based on apple leaf standards (NIST 1515, 44 ± 4 ng/g). Concentrations in the hardwood species were 1.48 ± 0.23 ng g-1 for sugar maple and 1.75 ± 0.14 ng g-1 for American beech. Concentrations were higher in red spruce and balsam fir. Samples that were analyzed fresh, freeze-dried, or oven-dried at 65 ˚C were in close agreement, after correcting for moisture content. However, Hg concentrations were 34 to 45% too high in the air-dry samples, presumably reflecting absorption from the atmosphere, and they were 44 to 66% too low in the samples oven-dried at 103 ˚C, presumably due to volatilization. We recommend that samples be freeze-dried or oven-dried at 65 ˚C for analysis of Hg in wood; archived samples that have been oven-dried at higher temperatures or stored exposed to the air may not be suitable for Hg analysis.

A GIS analysis of the relationship between sinkholes, dry-well complaints and groundwater pumping for frost-freeze protection of winter strawberry production in Florida.

PubMed

Aurit, Mark D; Peterson, Robert O; Blanford, Justine I

2013-01-01

Florida is riddled with sinkholes due to its karst topography. Sometimes these sinkholes can cause extensive damage to infrastructure and homes. It has been suggested that agricultural practices, such as sprinkler irrigation methods used to protect crops, can increase the development of sinkholes, particularly when temperatures drop below freezing, causing groundwater levels to drop quickly during groundwater pumping. In the strawberry growing region, Dover/Plant City, Florida, the effects have caused water shortages resulting in dry-wells and ground subsidence through the development of sinkholes that can be costly to maintain and repair. In this study, we look at how frost-freeze events have affected West Central Florida over the past 25 years with detailed comparisons made between two cold-years (with severe frost-freeze events) and a warm year (no frost-freeze events). We analyzed the spatial and temporal correlation between strawberry farming freeze protection practices and the development of sinkholes/dry well complaints, and assessed the economic impact of such events from a water management perspective by evaluating the cost of repairing and drilling new wells and how these compared with using alternative crop-protection methods. We found that the spatial distribution of sinkholes was non-random during both frost-freeze events. A strong correlation between sinkhole occurrence and water extraction and minimum temperatures was found. Furthermore as temperatures fall below 41°F and water levels decrease by more than 20 ft, the number of sinkholes increase greatly (N >10). At this time alternative protection methods such as freeze-cloth are cost prohibitive in comparison to repairing dry wells. In conclusion, the findings from this study are applicable in other agricultural areas and can be used to develop comprehensive water management plans in areas where the abstraction of large quantities of water occur.

A GIS Analysis of the Relationship between Sinkholes, Dry-Well Complaints and Groundwater Pumping for Frost-Freeze Protection of Winter Strawberry Production in Florida

PubMed Central

Aurit, Mark D.; Peterson, Robert O.; Blanford, Justine I.

2013-01-01

Florida is riddled with sinkholes due to its karst topography. Sometimes these sinkholes can cause extensive damage to infrastructure and homes. It has been suggested that agricultural practices, such as sprinkler irrigation methods used to protect crops, can increase the development of sinkholes, particularly when temperatures drop below freezing, causing groundwater levels to drop quickly during groundwater pumping. In the strawberry growing region, Dover/Plant City, Florida, the effects have caused water shortages resulting in dry- wells and ground subsidence through the development of sinkholes that can be costly to maintain and repair. In this study, we look at how frost-freeze events have affected West Central Florida over the past 25 years with detailed comparisons made between two cold-years (with severe frost-freeze events) and a warm year (no frost-freeze events). We analyzed the spatial and temporal correlation between strawberry farming freeze protection practices and the development of sinkholes/dry well complaints, and assessed the economic impact of such events from a water management perspective by evaluating the cost of repairing and drilling new wells and how these compared with using alternative crop-protection methods. We found that the spatial distribution of sinkholes was non-random during both frost-freeze events. A strong correlation between sinkhole occurrence and water extraction and minimum temperatures was found. Furthermore as temperatures fall below 41°F and water levels decrease by more than 20 ft, the number of sinkholes increase greatly (N >10). At this time alternative protection methods such as freeze-cloth are cost prohibitive in comparison to repairing dry wells. In conclusion, the findings from this study are applicable in other agricultural areas and can be used to develop comprehensive water management plans in areas where the abstraction of large quantities of water occur. PMID:23326518

The effect of drying and size reduction pretreatments on recovery of inorganic crop nutrients from inedible wheat residues

NASA Technical Reports Server (NTRS)

Strayer, R. F.; Alazraki, M. P.; Judkins, J.

2003-01-01

Inorganic nutrients can be easily recovered from ALS crop residue solid wastes by aqueous leaching. However, oven drying and milling pretreatment of these residues has been frequently required to accommodate crop scientists and facility storage limitations. As part of a research study that will compare three different bioreactor technologies for processing these wastes, we realized that different drying and size-reduction pretreatments had been utilized for each technology. This paper compares the effects of residue pretreatment on recovery of nutrients by leaching. Pretreatments included three drying methods [fresh, oven-dried (70 degrees C overnight), and freeze-dried] and two size reduction methods [chopped (2 cm length) and milled (2 mm diameter)]. Determination of mass balances (dry weight and ash content of solids) before and after leaching indicated solubilization was least for fresh residues (23% dry weight loss and 50% for ash loss), and most for freeze-dried residues (41-47% dry weight loss and nearly 100% for ash loss). Mineral recovery of major elements (NO3, PO4, K, Ca, and Mg) in leachates was poorest for fresh residues. P and K recovery in leachates were best for oven-dried residues and Ca, Mg, and N recovery best for freeze-dried residues. The differences in recovery for N, P, and K in leachates were minimal between chopping and milling and slightly better for Ca and Mg from milled residues.

Solid Lipid Nanoparticle assemblies (SLNas) for an anti-TB inhalation treatment-A Design of Experiments approach to investigate the influence of pre-freezing conditions on the powder respirability.

PubMed

Maretti, Eleonora; Rustichelli, Cecilia; Romagnoli, Marcello; Balducci, Anna Giulia; Buttini, Francesca; Sacchetti, Francesca; Leo, Eliana; Iannuccelli, Valentina

2016-09-10

For direct intramacrophagic antitubercular therapy, pulmonary administration through Dry Powder Inhaler (DPI) devices is a reasonable option. For the achievement of efficacious aerosolisation, rifampicin-loaded Solid Lipid Nanoparticle assemblies (SLNas) were developed using the melt emulsifying technique followed by freeze-drying. Indeed, this drying method can cause freezing or drying stresses compromising powder respirability. It is the aim of this research to offer novel information regarding pre-freezing variables. These included type and concentration of cryoprotectants, pre-freezing temperature, and nanoparticle concentration in the suspension. In particular, the effects of such variables were observed at two main levels. First of all, on SLNas characteristics - i.e., size, polydispersity index, zeta-potential, circularity, density, and drug loading. Secondly, on powder respirability, taking into account aerodynamic diameter, emitted dose, and respirable fraction. Considering the complexity of the factors involved in a successful respirable powder, a Design of Experiments (DoE) approach was adopted as a statistical tool for evaluating the effect of pre-freezing conditions. Interestingly, the most favourable impact on powder respirability was exerted by quick-freezing combined with a certain grade of sample dilution before the pre-freezing step without the use of cryoprotectants. In such conditions, a very high SLNas respirable fraction (>50%) was achieved, along with acceptable yields in the final dry powder as well as a reduction of powder mass to be introduced into DPI capsules with benefits in terms of administered drug dose feasibility. Copyright © 2016 Elsevier B.V. All rights reserved.

Freeze-drying process design by manometric temperature measurement: design of a smart freeze-dryer.

PubMed

Tang, Xiaolin Charlie; Nail, Steven L; Pikal, Michael J

2005-04-01

To develop a procedure based on manometric temperature measurement (MTM) and an expert system for good practices in freeze drying that will allow development of an optimized freeze-drying process during a single laboratory freeze-drying experiment. Freeze drying was performed with a FTS Dura-Stop/Dura-Top freeze dryer with the manometric temperature measurement software installed. Five percent solutions of glycine, sucrose, or mannitol with 2 ml to 4 ml fill in 5 ml vials were used, with all vials loaded on one shelf. Details of freezing, optimization of chamber pressure, target product temperature, and some aspects of secondary drying are determined by the expert system algorithms. MTM measurements were used to select the optimum shelf temperature, to determine drying end points, and to evaluate residual moisture content in real-time. MTM measurements were made at 1 hour or half-hour intervals during primary drying and secondary drying, with a data collection frequency of 4 points per second. The improved MTM equations were fit to pressure-time data generated by the MTM procedure using Microcal Origin software to obtain product temperature and dry layer resistance. Using heat and mass transfer theory, the MTM results were used to evaluate mass and heat transfer rates and to estimate the shelf temperature required to maintain the target product temperature. MTM product dry layer resistance is accurate until about two-thirds of total primary drying time is over, and the MTM product temperature is normally accurate almost to the end of primary drying provided that effective thermal shielding is used in the freeze-drying process. The primary drying times can be accurately estimated from mass transfer rates calculated very early in the run, and we find the target product temperature can be achieved and maintained with only a few adjustments of shelf temperature. The freeze-dryer overload conditions can be estimated by calculation of heat/mass flow at the target product temperature. It was found that the MTM results serve as an excellent indicator of the end point of primary drying. Further, we find that the rate of water desorption during secondary drying may be accurately measured by a variation of the basic MTM procedure. Thus, both the end point of secondary drying and real-time residual moisture may be obtained during secondary drying. Manometric temperature measurement and the expert system for good practices in freeze drying does allow development of an optimized freeze-drying process during a single laboratory freeze-drying experiment.

Naproxen Microparticulate Systems Prepared Using In Situ Crystallisation and Freeze-Drying Techniques.

PubMed

Solaiman, Amanda; Tatari, Adam Keenan; Elkordy, Amal Ali

2017-07-01

Poor drug solubility and dissolution rate remain to be one of the major problems facing pharmaceutical scientists, with approximately 40% of drugs in the industry categorised as practically insoluble or poorly water soluble. This in turn can lead to serious delivery challenges and poor bioavailability. The aim of this research was to investigate the effects of the surfactants, poloxamer 407 (P407) and caprol® PGE 860 (CAP), at various concentrations (0.1, 0.5, 1 and 3% w/v) on the enhancement of the dissolution properties of poorly water-soluble drug, naproxen, using in situ micronisation by solvent change method and freeze-drying. The extent at which freeze-drying influences the dissolution rate of naproxen microcrystals is investigated in this study by comparison with desiccant-drying. All formulations were evaluated and characterised using particle size analysis and morphology, in vitro dissolution studies, differential scanning calorimetry (DSC), and Fourier transform infra-red (FT-IR) spectroscopy. An increase in poloxamer 407 concentration in freeze-dried formulations led to enhancement of drug dissolution compared to desiccator-dried formulations, naproxen/caprol® PGE 860 formulations and untreated drug. DSC and FT-IR results show no significant chemical interactions between drug and poloxamer 407, with only very small changes to drug crystallinity. On the other hand, caprol® PGE 860 showed some interactions with drug components, alterations to the crystal lattice of naproxen, and poor dissolution profiles using both drying methods, making it a poor choice of excipient.

Heat and Mass Transfer Model in Freeze-Dried Medium

NASA Astrophysics Data System (ADS)

Alfat, Sayahdin; Purqon, Acep

2017-07-01

There are big problems in agriculture sector every year. One of the major problems is abundance of agricultural product during the peak of harvest season that is not matched by an increase in demand of agricultural product by consumers, this causes a wasted agricultural products. Alternative way was food preservation by freeze dried method. This method was already using heat transfer through conduction and convection to reduce water quality in the food. The main objective of this research was to design a model heat and mass transfer in freeze-dried medium. We had two steps in this research, the first step was design of medium as the heat injection site and the second was simulate heat and mass transfer of the product. During simulation process, we use physical property of some agriculture product. The result will show how temperature and moisture distribution every second. The method of research use finite element method (FEM) and will be illustrated in three dimensional.

Demonstrating Functional Equivalence of Pilot and Production Scale Freeze-Drying of BCG

PubMed Central

ten Have, R.; Reubsaet, K.; van Herpen, P.; Kersten, G.; Amorij, J.-P.

2016-01-01

Process analytical technology (PAT)-tools were used to monitor freeze-drying of Bacille Calmette-Guérin (BCG) at pilot and production scale. Among the evaluated PAT-tools, there is the novel use of the vacuum valve open/close frequency for determining the endpoint of primary drying at production scale. The duration of primary drying, the BCG survival rate, and the residual moisture content (RMC) were evaluated using two different freeze-drying protocols and were found to be independent of the freeze-dryer scale evidencing functional equivalence. The absence of an effect of the freeze-dryer scale on the process underlines the feasibility of the pilot scale freeze-dryer for further BCG freeze-drying process optimization which may be carried out using a medium without BCG. PMID:26981867

Demonstrating Functional Equivalence of Pilot and Production Scale Freeze-Drying of BCG.

PubMed

Ten Have, R; Reubsaet, K; van Herpen, P; Kersten, G; Amorij, J-P

2016-01-01

Process analytical technology (PAT)-tools were used to monitor freeze-drying of Bacille Calmette-Guérin (BCG) at pilot and production scale. Among the evaluated PAT-tools, there is the novel use of the vacuum valve open/close frequency for determining the endpoint of primary drying at production scale. The duration of primary drying, the BCG survival rate, and the residual moisture content (RMC) were evaluated using two different freeze-drying protocols and were found to be independent of the freeze-dryer scale evidencing functional equivalence. The absence of an effect of the freeze-dryer scale on the process underlines the feasibility of the pilot scale freeze-dryer for further BCG freeze-drying process optimization which may be carried out using a medium without BCG.

Effect of dehydration on raspberries: polyphenol and anthocyanin retention, antioxidant capacity, and antiadipogenic activity.

PubMed

Mejia-Meza, E I; Yáñez, J A; Remsberg, C M; Takemoto, J K; Davies, N M; Rasco, B; Clary, C

2010-01-01

Fresh and dried raspberries prepared by freeze drying (FD), microwave-vacuum (MIVAC), hot-air drying (HAD), and a combination of hot-air drying and microwave-vacuum (HAD/MIVAC) drying methods were evaluated for polyphenol retention, total polyphenol and anthocyanin contents, total antioxidant capacity, and antiadipogenic activity (the inhibition of fat cell development). Ellagic acid and quercetin were present in the largest concentrations in fresh and dehydrated raspberries. Dehydration led to a loss of polyphenols and anthocyanins and antioxidant capacity. Polyphenols (aglycone form) were retained in the greatest amount: 20% (freeze dried) to 30% (HAD/MIVAC) (fresh = 100%). A total of 30% of polyphenols (glycoside form) were retained in raspberries dried by the HAD/MIVAC methods with 5% of retention observed for raspberries dried by FD, HAD, or MIVAC. FD and MIVAC resulted in higher retention of anthocyanins (aglycone form) than other drying methods. It was also observed that antioxidant activity was reduced by dehydration. Adipogenesis was inhibited by polyphenolic glycosides (30%) and aglycones (30% to 40%) in fresh and HAD/MIVAC raspberries. Extracts from dried raspberries by HAD/MIVAC methods were relatively more effective at inhibiting adipogenesis compared to HAD and FD dried raspberries.

Simulation of the process kinetics and analysis of physicochemical properties in the freeze drying of kale

NASA Astrophysics Data System (ADS)

Dziki, Dariusz; Polak, Renata; Rudy, Stanisław; Krzykowski, Andrzej; Gawlik-Dziki, Urszula; Różyło, Renata; Miś, Antoni; Combrzyński, Maciej

2018-01-01

Investigations were performed to study the freeze-drying process of kale (Brassica oleracea L. var acephala). The process of freeze-drying was performed at temperatures of 20, 40, and 60°C for whole pieces of leaves and for pulped leaves. The kinetics of the freeze-drying of both kale leaves and kale pulp were best described by the Page model. The increasing freeze-drying temperature from 20 to 60°C induced an approximately two-fold decrease in the drying time. Freeze-drying significantly increased the value of the lightness, delta Chroma, and browning index of kale, and had little influence on the hue angle. The highest increase in the lightness and delta Chroma was observed for whole leaves freeze-dried at 20°C. An increase in the drying temperature brought about a slight decrease in the lightness, delta Chroma and the total colour difference. Pulping decreased the lightness and hue angle, and increased browning index. Freeze-drying engendered a slight decrease in the total phenolics content and antioxidant activity, in comparison to fresh leaves. The temperature of the process and pulping had little influence on the total phenolics content and antioxidant activity of dried kale, but significantly decreased the contents of chlorophyll a and chlorophyll b.

Fundamentals of freeze-drying.

PubMed

Nail, Steven L; Jiang, Shan; Chongprasert, Suchart; Knopp, Shawn A

2002-01-01

Given the increasing importance of reducing development time for new pharmaceutical products, formulation and process development scientists must continually look for ways to "work smarter, not harder." Within the product development arena, this means reducing the amount of trial and error empiricism in arriving at a formulation and identification of processing conditions which will result in a quality final dosage form. Characterization of the freezing behavior of the intended formulation is necessary for developing processing conditions which will result in the shortest drying time while maintaining all critical quality attributes of the freeze-dried product. Analysis of frozen systems was discussed in detail, particularly with respect to the glass transition as the physical event underlying collapse during freeze-drying, eutectic mixture formation, and crystallization events upon warming of frozen systems. Experiments to determine how freezing and freeze-drying behavior is affected by changes in the composition of the formulation are often useful in establishing the "robustness" of a formulation. It is not uncommon for seemingly subtle changes in composition of the formulation, such as a change in formulation pH, buffer salt, drug concentration, or an additional excipient, to result in striking differences in freezing and freeze-drying behavior. With regard to selecting a formulation, it is wise to keep the formulation as simple as possible. If a buffer is needed, a minimum concentration should be used. The same principle applies to added salts: If used at all, the concentration should be kept to a minimum. For many proteins a combination of an amorphous excipient, such as a disaccharide, and a crystallizing excipient, such as glycine, will result in a suitable combination of chemical stability and physical stability of the freeze-dried solid. Concepts of heat and mass transfer are valuable in rational design of processing conditions. Heat transfer by conduction--the dominant mechanism of heat transfer in freeze-drying--is inefficient at the pressures used in freeze-drying. Steps should be taken to improve the thermal contact between the product and the shelf of the freeze dryer, such as eliminating metal trays from the drying process. Quantitation of the heat transfer coefficient for the geometry used is a useful way of assessing the impact of changes in the system such as elimination of product trays and changes in the vial. Because heat transfer by conduction through the vapor increases with increasing pressure, the commonly held point of view that "the lower the pressure, the better" is not true with respect to process efficiency. The optimum pressure for a given product is a function of the temperature at which freeze-drying is carried out, and lower pressures are needed at low product temperatures. The controlling resistance to mass transfer is almost always the resistance of the partially dried solids above the submination interface. This resistance can be minimized by avoiding fill volumes of more than about half the volume of the container. The development scientist should also recognize that very high concentrations of solute may not be appropriate for optimum freeze-drying, particularly if the resistance of the dried product layer increases sharply with concentration. Although the last 10 years has seen the publication of a significant body of literature of great value in allowing development scientists and engineers to "work smarter," there is still much work needed in both the science and the technology of freeze-drying. Scientific development is needed for improving analytical methodology for characterization of frozen systems and freeze-dried solids. A better understanding of the relationship between molecular mobility and reactivity is needed to allow accurate prediction of product stability at the intended storage temperature based on accelerated stability at higher temperatures. This requires that the temperature dependence of glass transition-associated mobility, particularly at temperatures below the glass transition, be studied in greater depth. The relevance of the concept of strong and fragile glasses to frozen systems and freeze-dried solids has only begun to be explored. The list of pharmaceutically acceptable protective solutes is very short, and more imagination--and work--is needed in order to develop pharmaceutically acceptable alternative stabilizers. There is a need for technology development in process monitoring, particularly in developing a way to measure the status of the product during freezing and freeze-drying without placing temperature measurement probes in individual vials of product. The current practice of placing thermocouples in vials is uncertain with respect to reliability of the data, inconsistent with elimination of personnel in close proximity to open vials of product in an aseptic environment, and incompatible with technology for automatic material handling in freeze-drying. In addition, a method for controlling the degree of supercooling during freezing would allow better control of freezing rate and would, in many cases, result in more consistent product quality.

Cryoprotectant choice and analyses of freeze-drying drug suspension of nanoparticles with functional stabilisers.

PubMed

Wang, Lulu; Ma, Yingying; Gu, Yu; Liu, Yangyang; Zhao, Juan; Yan, Beibei; Wang, Yancai

2018-04-19

Freeze-drying is an effective way to improve long-term physical stability of nanosuspension in drug delivery applications. Nanosuspension also known as suspension of nanoparticles. In this study, the effect of freeze-drying with different cryoprotectants on the physicochemical characteristics of resveratrol (RSV) nanosuspension and quercetin (QUE) nanosuspension was evaluated. D-α-tocopheryl polyethylene glycol succinate (TPGS) and folate-modified distearoylphosphatidyl ethanolamine-polyethylene glycol (DSPE-PEG-FA) were selected as functional stabilisers formulated nanosuspension which were prepared by anti-solvent precipitation method. RSV nanoparticle size and QUE nanoparticle size were about 210 and 110 nm, respectively. The AFM and TEM results of nanosuspension showed uniform and irregular shape particles. After freeze-drying, the optimal concentration of four cryoprotectants was determined by the particle size of re-dispersed nanoparticles. The dissolution profile of drug nanoparticle significantly showed approximately at a 6-8-fold increase dissolution rate. Moreover, TPGS and DSPE-PEG-FA stabilised RSV nanosuspension and QUE nanosuspension samples showed better effect on long-term physical stability.

Detecting phase separation of freeze-dried binary amorphous systems using pair-wise distribution function and multivariate data analysis.

PubMed

Chieng, Norman; Trnka, Hjalte; Boetker, Johan; Pikal, Michael; Rantanen, Jukka; Grohganz, Holger

2013-09-15

The purpose of this study is to investigate the use of multivariate data analysis for powder X-ray diffraction-pair-wise distribution function (PXRD-PDF) data to detect phase separation in freeze-dried binary amorphous systems. Polymer-polymer and polymer-sugar binary systems at various ratios were freeze-dried. All samples were analyzed by PXRD, transformed to PDF and analyzed by principal component analysis (PCA). These results were validated by differential scanning calorimetry (DSC) through characterization of glass transition of the maximally freeze-concentrate solute (Tg'). Analysis of PXRD-PDF data using PCA provides a more clear 'miscible' or 'phase separated' interpretation through the distribution pattern of samples on a score plot presentation compared to residual plot method. In a phase separated system, samples were found to be evenly distributed around the theoretical PDF profile. For systems that were miscible, a clear deviation of samples away from the theoretical PDF profile was observed. Moreover, PCA analysis allows simultaneous analysis of replicate samples. Comparatively, the phase behavior analysis from PXRD-PDF-PCA method was in agreement with the DSC results. Overall, the combined PXRD-PDF-PCA approach improves the clarity of the PXRD-PDF results and can be used as an alternative explorative data analytical tool in detecting phase separation in freeze-dried binary amorphous systems. Copyright © 2013 Elsevier B.V. All rights reserved.

Pharmaceutical patent applications in freeze-drying.

PubMed

Ekenlebie, Edmond; Einfalt, Tomaž; Karytinos, Arianna Irò; Ingham, Andrew

2016-09-01

Injectable products are often the formulation of choice for new therapeutics; however, formulation in liquids often enhances degradation through hydrolysis. Thus, freeze-drying (lyophilization) is regularly used in pharmaceutical manufacture to reduce water activity. Here we examine its contribution to 'state of the art' and look at its future potential uses. A comprehensive search of patent databases was conducted to characterize the international patent landscape and trends in the use of freeze-drying. A total of 914 disclosures related to freeze-drying, lyophilization or drying of solid systems in pressures and temperatures equivalent to those of freeze-drying were considered over the period of 1992-2014. Current applications of sublimation technology were contrasted across two periods those with patents due to expire (1992-1993) and those currently filed. The number of freeze-drying technology patents has stabilized after initial activity across the biotechnology sector in 2011 and 2012. Alongside an increasing trend for patent submissions, freeze-drying submissions have slowed since 2002 and is indicative of a level of maturity.

Inhibitory effect of burdock leaves on elastase and tyrosinase activity.

PubMed

Horng, Chi-Ting; Wu, Hsing-Chen; Chiang, Ni-Na; Lee, Chiu-Fang; Huang, Yu-Syuan; Wang, Hui-Yun; Yang, Jai-Sing; Chen, Fu-An

2017-10-01

Burdock ( Arctium lappa L.) leaves generate a considerable amount of waste following burdock root harvest in Taiwan. To increase the use of burdock leaves, the present study investigated the optimal methods for producing burdock leaf extract (BLE) with high antioxidant polyphenolic content, including drying methods and solvent extraction concentration. In addition, the elastase and tyrosinase inhibitory activity of BLE was examined. Burdock leaves were dried by four methods: Shadow drying, oven drying, sun drying and freeze-drying. The extract solution was then subjected to total polyphenol content analysis and the method that produced BLE with the highest amount of total antioxidant components was taken forward for further analysis. The 1,1-diphenyl-2-pycrylhydrazyl scavenging, antielastase and antityrosinase activity of the BLE were measured to enable the evaluation of the antioxidant and skin aging-associated enzyme inhibitory activities of BLE. The results indicated that the total polyphenolic content following extraction with ethanol (EtOH) was highest using the freeze-drying method, followed by the oven drying, shadow drying and sun drying methods. BLE yielded a higher polyphenol content and stronger antioxidant activity as the ratio of the aqueous content of the extraction solvent used increased. BLE possesses marked tyrosinase and elastase inhibitory activities, with its antielastase activity notably stronger compared with its antityrosinase activity. These results indicate that the concentration of the extraction solvent was associated with the antioxidant and skin aging-associated enzyme inhibitory activity of BLE. The reactive oxygen species scavenging theory of skin aging may explain the tyrosinase and elastase inhibitory activity of BLE. In conclusion, the optimal method for obtaining BLE with a high antioxidant polyphenolic content was freeze-drying followed by 30-50% EtOH extraction. In addition, the antielastase and antityrosinase activities of the BLE produced may be aid in the development of skincare products with antiwrinkle and skin-evening properties.

Inhibitory effect of burdock leaves on elastase and tyrosinase activity

PubMed Central

Horng, Chi-Ting; Wu, Hsing-Chen; Chiang, Ni-Na; Lee, Chiu-Fang; Huang, Yu-Syuan; Wang, Hui-Yun; Yang, Jai-Sing; Chen, Fu-An

2017-01-01

Burdock (Arctium lappa L.) leaves generate a considerable amount of waste following burdock root harvest in Taiwan. To increase the use of burdock leaves, the present study investigated the optimal methods for producing burdock leaf extract (BLE) with high antioxidant polyphenolic content, including drying methods and solvent extraction concentration. In addition, the elastase and tyrosinase inhibitory activity of BLE was examined. Burdock leaves were dried by four methods: Shadow drying, oven drying, sun drying and freeze-drying. The extract solution was then subjected to total polyphenol content analysis and the method that produced BLE with the highest amount of total antioxidant components was taken forward for further analysis. The 1,1-diphenyl-2-pycrylhydrazyl scavenging, antielastase and antityrosinase activity of the BLE were measured to enable the evaluation of the antioxidant and skin aging-associated enzyme inhibitory activities of BLE. The results indicated that the total polyphenolic content following extraction with ethanol (EtOH) was highest using the freeze-drying method, followed by the oven drying, shadow drying and sun drying methods. BLE yielded a higher polyphenol content and stronger antioxidant activity as the ratio of the aqueous content of the extraction solvent used increased. BLE possesses marked tyrosinase and elastase inhibitory activities, with its antielastase activity notably stronger compared with its antityrosinase activity. These results indicate that the concentration of the extraction solvent was associated with the antioxidant and skin aging-associated enzyme inhibitory activity of BLE. The reactive oxygen species scavenging theory of skin aging may explain the tyrosinase and elastase inhibitory activity of BLE. In conclusion, the optimal method for obtaining BLE with a high antioxidant polyphenolic content was freeze-drying followed by 30–50% EtOH extraction. In addition, the antielastase and antityrosinase activities of the BLE produced may be aid in the development of skincare products with antiwrinkle and skin-evening properties. PMID:28912875

Freeze-drying in novel container system: Characterization of heat and mass transfer in glass syringes.

PubMed

Patel, Sajal M; Pikal, Michael J

2010-07-01

This study is aimed at characterizing and understanding different modes of heat and mass transfer in glass syringes to develop a robust freeze-drying process. Two different holder systems were used to freeze-dry in syringes: an aluminum (Al) block and a plexiglass holder. The syringe heat transfer coefficient was characterized by a sublimation test using pure water. Mannitol and sucrose (5% w/v) were also freeze-dried, as model systems, in both the assemblies. Dry layer resistance was determined from manometric temperature measurement (MTM) and product temperature was measured using thermocouples, and was also determined from MTM. Further, freeze-drying process was also designed using Smart freeze-dryer to assess its application for freeze-drying in novel container systems. Heat and mass transfer in syringes were compared against the traditional container system (i.e., glass tubing vial). In the Al block, the heat transfer was via three modes: contact conduction, gas conduction, and radiation with gas conduction being the dominant mode of heat transfer. In the plexiglass holder, the heat transfer was mostly via radiation; convection was not involved. Also, MTM/Smart freeze-drying did work reasonably well for freeze-drying in syringes. When compared to tubing vials, product temperature decreases and hence drying time increases in syringes. (c) 2010 Wiley-Liss, Inc. and the American Pharmacists Association

[Analysis of dynamic changes of flavonoids and alkaloids during different drying process of Morus alba leaves].

PubMed

Bai, Yong-liang; Duan, Jin-ao; Su, Shu-lan; Qian, Ye-fei; Qian, Da-wei; Ouyang, Zhen

2014-07-01

To find out dynamic changes of flavonoids and alkaloids in Morus alba leaves by analyzing influence of different drying method and drying degrees, in order to provide evidence for quality evaluation of Morus alba leaves. Different drying methods, programmed temperature methods and constant temperature methods were adopted to dry Morus alba leaves samples respectively. Contents of flavonoids and alkaloids were analyzed by HPLC-PDA and LC-TQ/MS respectively. It's shown obviously that the content of flavonoids were influenced heavily by different drying methods. Methods that suitable for flavonoids were freezing-dried > shade-dried > dried > sun-dried > microwave-dried > infrared-dried; Methods that suitable for alkaloids were freezing-dried > shade-dried > dried > sun-dried > infrared-dried > microwave-dried. The 55 -65 degrees C group was shown to be the lowest in both flavonoids and DNJ while the 85 - 95 degrees C group was shown to be the best for DNJ. For fagomine, the 45 degrees C group was shown to be the lowest concentrations while the 95 - 105 degrees C group was shown to be the highest. Samples with different moisture were shown to be different in content of flavonoids and alkaloids. And samples with 10% moisture contain highest flavonoids while those with 30% - 50% moisture contain lowest flavonoids. Content of DNJ and fagomine raised as moisture decreasing. In addition, the 55 - 65 degrees C group was better than the 95 -105 degrees C one in alkaloids content. The results provide optimal drying methods and condition for drying Morus alba leaves, and foundations for uncovering biochemical transform of Morus alba leaves.

Developments in the formulation and delivery of spray dried vaccines

PubMed Central

Kanojia, Gaurav; Have, Rimko ten; Soema, Peter C.; Frijlink, Henderik; Amorij, Jean-Pierre; Kersten, Gideon

2017-01-01

ABSTRACT Spray drying is a promising method for the stabilization of vaccines, which are usually formulated as liquids. Usually, vaccine stability is improved by spray drying in the presence of a range of excipients. Unlike freeze drying, there is no freezing step involved, thus the damage related to this step is avoided. The edge of spray drying resides in its ability for particles to be engineered to desired requirements, which can be used in various vaccine delivery methods and routes. Although several spray dried vaccines have shown encouraging preclinical results, the number of vaccines that have been tested in clinical trials is limited, indicating a relatively new area of vaccine stabilization and delivery. This article reviews the current status of spray dried vaccine formulations and delivery methods. In particular it discusses the impact of process stresses on vaccine integrity, the application of excipients in spray drying of vaccines, process and formulation optimization strategies based on Design of Experiment approaches as well as opportunities for future application of spray dried vaccine powders for vaccine delivery. PMID:28925794

Freeze drying vs microwave drying-methods for synthesis of sinteractive thoria powders

NASA Astrophysics Data System (ADS)

Annie, D.; Chandramouli, V.; Anthonysamy, S.; Ghosh, Chanchal; Divakar, R.

2017-02-01

Thoria powders were synthesized by oxalate precipitation from an aqueous solution of the nitrate. The filtered precipitates were freeze dried or microwave dried before being calcined at 1073 K. The thoria powders obtained were characterized for crystallite size, specific surface area, bulk density, particle size distribution and residual carbon. Microstructure of the product was studied using scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Sinterability of the synthesized powders was studied by measuring the density of the sintered compacts. Powders that can be consolidated and sintered to densities ∼96% theoretical density (TD) at 1773 K were obtained.

Changes in non-volatile taste components of button mushroom (Agaricus bisporus) during different stages of freeze drying and freeze drying combined with microwave vacuum drying.

PubMed

Pei, Fei; Shi, Ying; Gao, Xingyang; Wu, Fangning; Mariga, Alfred Mugambi; Yang, Wenjian; Zhao, Liyan; An, Xinxin; Xin, Zhihong; Yang, Fangmei; Hu, Qiuhui

2014-12-15

Button mushroom slices were dehydrated using freeze drying (FD) or FD combined with microwave vacuum drying (FMVD), and the non-volatile component profiles were studied. The results showed that the level of non-volatile components in button mushroom firstly increased during sublimation of FD/FMVD process and then fell during desorption in FD process and MVD in FMVD process. Compared to FD products, the contents of soluble sugars and polyols in FMVD products were relatively low, whereas the contents of total free amino acids were significantly higher, close to the level of fresh mushroom. However, there was no significant difference in the contents of 5'-nucleotides and organic acids between FD and FMVD products. The equivalent umami concentration (EUC) values for FD and FMVD products did not differ from fresh, indicating that both drying methods could effectively preserve MSG (monosodium glutamate)-like components in button mushroom. Copyright © 2014 Elsevier Ltd. All rights reserved.

Influence of entanglements on glass transition temperature of polystyrene

NASA Astrophysics Data System (ADS)

Ougizawa, Toshiaki; Kinugasa, Yoshinori

2013-03-01

Chain entanglement is essential behavior of polymeric molecules and it seems to affect many physical properties such as not only viscosity of melt state but also glass transition temperature (Tg). But we have not attained the quantitative estimation because the entanglement density is considered as an intrinsic value of the polymer at melt state depending on the chemical structure. Freeze-drying method is known as one of the few ways to make different entanglement density sample from dilute solution. In this study, the influence of entanglements on Tg of polystyrene obtained by the freeze-dried method was estimated quantitatively. The freeze-dried samples showed Tg depression with decreasing the concentration of precursor solution due to the lower entanglement density and their depressed Tg would be saturated when the almost no intermolecular entanglement was formed. The molecular weight dependence of the maximum value of Tg depression was discussed.

Survival differences among freeze-dried genetically engineered and wild-type bacteria.

PubMed Central

Israeli, E; Shaffer, B T; Hoyt, J A; Lighthart, B; Ganio, L M

1993-01-01

Because the death mechanisms of freeze-dried and air-dried bacteria are thought to be similar, freeze-drying was used to investigate the survival differences between potentially airborne genetically engineered microorganisms and their wild types. To this end, engineered strains of Escherichia coli and Pseudomonas syringae were freeze-dried and exposed to air, visible light, or both. The death rates of all engineered strains were significantly higher than those of their parental strains. Light and air exposure were found to increase the death rates of all strains. Application of death rate models to freeze-dried engineered bacteria to be released into the environment is discussed. PMID:8434925

Care during freeze-drying of bovine pericardium tissue to be used as a biomaterial: a comparative study.

PubMed

Polak, Roberta; Pitombo, Ronaldo N M

2011-10-01

Bovine pericardium (BP) tissue is widely used in the manufacture of bioprosthetics. The effects of freeze-drying on the BP tissue have been studied by some researchers in order to decrease their cytotoxicity due to preservation in formaldehyde solution, and to increase the lifetime of the product in storage. This study was undertaken in order to study the effect of freeze-drying in the structure of BP. To perform this study BP samples were freeze-dried in two different types of freeze-dryers available in our laboratory: a laboratory freeze-dryer, in which it was not possible to control parameters and a pilot freeze-dryer, wherein all parameters during freezing and drying were controlled. After freeze-drying processes, samples were analyzed by SEM, Raman spectroscopy, tensile strength, water uptake tests and TEM. In summary, it has been demonstrated that damages occur in collagen fibers by the loss of bulk water of collagen structure implicating in a drastic decreasing of BP mechanical properties due to its structural alterations. Moreover, it was proven that the collagen fibrils suffered breakage at some points, which can be attributed to the uncontrolled parameters during drying. Copyright © 2011 Elsevier Inc. All rights reserved.

Effect of freeze-drying on viability and in vitro probiotic properties of a mixture of lactic acid bacteria and yeasts isolated from kefir.

PubMed

Bolla, Patricia A; Serradell, María de los Angeles; de Urraza, Patricio J; De Antoni, Graciela L

2011-02-01

The effect of freeze-drying on viability and probiotic properties of a microbial mixture containing selected bacterial and yeast strains isolated from kefir grains (Lactobacillus kefir, Lactobacillus plantarum, Lactococcus lactis, Saccharomyces cerevisiae and Kluyveromyces marxianus) was studied. The microorganisms were selected according to their potentially probiotic properties in vitro already reported. Two types of formulations were performed, a microbial mixture (MM) suspended in milk and a milk product fermented with MM (FMM). To test the effect of storage on viability of microorganisms, MM and FMM were freeze-dried and maintained at 4°C for six months. After 180 days of storage at 4°C, freeze-dried MM showed better survival rates for each strain than freeze-dried FMM. The addition of sugars (trehalose or sucrose) did not improve the survival rates of any of the microorganisms after freeze-drying. Freeze-drying did not affect the capacity of MM to inhibit growth of Shigella sonnei in vitro, since the co-incubation of this pathogen with freeze-dried MM produced a decrease of 2 log in Shigella viability. The safety of freeze-dried MM was tested in mice and non-translocation of microorganisms to liver or spleen was observed in BALB/c mice feed ad libitum during 7 or 20 days. To our knowledge, this is the first report about the effect of freeze-drying on viability, in vitro probiotic properties and microbial translocation of a mixture containing different strains of both bacteria and yeasts isolated from kefir.

Drying techniques for the visualisation of agarose-based chromatography media by scanning electron microscopy.

PubMed

Nweke, Mauryn C; Turmaine, Mark; McCartney, R Graham; Bracewell, Daniel G

2017-03-01

The drying of chromatography resins prior to scanning electron microscopy is critical to image resolution and hence understanding of the bead structure at sub-micron level. Achieving suitable drying conditions is especially important with agarose-based chromatography resins, as over-drying may cause artefact formation, bead damage and alterations to ultrastructural properties; and under-drying does not provide sufficient resolution for visualization under SEM. This paper compares and contrasts the effects of two drying techniques, critical point drying and freeze drying, on the morphology of two agarose based resins (MabSelect™/d w ≈85 µm and Capto™ Adhere/d w ≈75 µm) and provides a complete method for both. The results show that critical point drying provides better drying and subsequently clearer ultrastructural visualization of both resins under SEM. Under this protocol both the polymer fibers (thickness ≈20 nm) and the pore sizes (diameter ≈100 nm) are clearly visible. Freeze drying is shown to cause bead damage to both resins, but to different extents. MabSelect resin encounters extensive bead fragmentation, whilst Capto Adhere resin undergoes partial bead disintegration, corresponding with the greater extent of agarose crosslinking and strength of this resin. While freeze drying appears to be the less favorable option for ultrastructural visualization of chromatography resin, it should be noted that the extent of fracturing caused by the freeze drying process may provide some insight into the mechanical properties of agarose-based chromatography media. © 2017 The Authors. Biotechnology Journal published by WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Model for heat and mass transfer in freeze-drying of pellets.

PubMed

Trelea, Ioan Cristian; Passot, Stéphanie; Marin, Michèle; Fonseca, Fernanda

2009-07-01

Lyophilizing frozen pellets, and especially spray freeze-drying, have been receiving growing interest. To design efficient and safe freeze-drying cycles, local temperature and moisture content in the product bed have to be known, but both are difficult to measure in the industry. Mathematical modeling of heat and mass transfer helps to determine local freeze-drying conditions and predict effects of operation policy, and equipment and recipe changes on drying time and product quality. Representative pellets situated at different positions in the product slab were considered. One-dimensional transfer in the slab and radial transfer in the pellets were assumed. Coupled heat and vapor transfer equations between the temperature-controlled shelf, the product bulk, the sublimation front inside the pellets, and the chamber were established and solved numerically. The model was validated based on bulk temperature measurement performed at two different locations in the product slab and on partial vapor pressure measurement in the freeze-drying chamber. Fair agreement between measured and calculated values was found. In contrast, a previously developed model for compact product layer was found inadequate in describing freeze-drying of pellets. The developed model represents a good starting basis for studying freeze-drying of pellets. It has to be further improved and validated for a variety of product types and freeze-drying conditions (shelf temperature, total chamber pressure, pellet size, slab thickness, etc.). It could be used to develop freeze-drying cycles based on product quality criteria such as local moisture content and glass transition temperature.

Extraction condition optimization and effects of drying methods on physicochemical properties and antioxidant activities of polysaccharides from comfrey (Symphytum officinale L.) root.

PubMed

Shang, Hongmei; Zhou, Haizhu; Duan, Mengying; Li, Ran; Wu, Hongxin; Lou, Yujie

2018-06-01

This study was designed to investigate the extraction conditions of polysaccharides from comfrey (Symphytum officinale L.) root (CRPs) using response surface methodology (RSM). The effects of three variables including liquid-solid ratio, extraction time and extraction temperature on the extraction yield of CRPs were taken into consideration. Moreover, the effects of drying methods including hot air drying (HD), vacuum drying (VD) and freeze drying (FD) on the physicochemical properties and antioxidant activities of CRPs were evaluated. The optimal conditions to extract the polysaccharides were as follows: liquid-solid ratio (15mL/g), extraction time (74min), and extraction temperature (95°C), allowed a maximum polysaccharides yield of 22.87%. Different drying methods had significant effects on the physicochemical properties of CRPs such as the chemical composition (contents of total polysaccharides and uronic acid), relative viscosity, solubility and molecular weight. CRPs drying with FD method showed stronger reducing power and radical scavenging capacities against DPPH and ABTS radicals compared with CRPs drying with HD and VD methods. Therefore, freeze drying served as a good method for keeping the antioxidant activities of polysaccharides from comfrey root. Copyright © 2018 Elsevier B.V. All rights reserved.

Effects of buffer composition and processing conditions on aggregation of bovine IgG during freeze-drying.

PubMed

Sarciaux, J M; Mansour, S; Hageman, M J; Nail, S L

1999-12-01

The objective of this study was to identify critical formulation and processing variables affecting aggregation of bovine IgG during freeze-drying when no lyoprotective solute is used. Parameters examined were phosphate buffer concentration and counterion (Na versus K phosphate), added salts, cooling rate, IgG concentration, residual moisture level, and presence of a surfactant. No soluble aggregates were detected in any formulation after either freezing/thawing or freeze-drying. No insoluble aggregates were detected in any formulation after freezing, but insoluble aggregate levels were always detectable after freeze-drying. The data are consistent with a mechanism of aggregate formation involving denaturation of IgG at the ice/freeze-concentrate interface which is reversible upon freeze-thawing, but becomes irreversible after freeze-drying and reconstitution. Rapid cooling (by quenching in liquid nitrogen) results in more and larger aggregates than slow cooling on the shelf of the freeze-dryer. This observation is consistent with surface area measurements and environmental electron microscopic data showing a higher surface area of freeze-dried solids after fast cooling. Annealing of rapidly cooled solutions results in significantly less aggregation in reconstituted freeze-dried solids than in nonannealed controls, with a corresponding decrease in specific surface area of the freeze-dried, annealed system. Increasing the concentration of IgG significantly improves the stability of IgG against freeze-drying-induced aggregation, which may be explained by a smaller percentage of the protein residing at the ice/freeze-concentrate interface as IgG concentration is increased. A sodium phosphate buffer system consistently results in more turbid reconstituted solids than a potassium phosphate buffer system at the same concentration, but this effect is not attributable to a pH shift during freezing. Added salts such as NaCl or KCl contribute markedly to insoluble aggregate formation. Both sodium and potassium chloride contribute more to turbidity of the reconstituted solid than either sodium or potassium phosphate buffers at similar ionic strength, with sodium chloride resulting in a substantially higher level of aggregates than potassium chloride. At a given cooling rate, the specific surface area of dried solids is approximately a factor of 2 higher for the formulation containing sodium chloride than the formulation containing potassium chloride. Turbidity is also influenced by the extent of secondary drying, which underscores the importance of minimizing secondary drying of this system. Including a surfactant such as polysorbate 80, either in the formulation or in the water used for reconstitution, decreased, but did not eliminate, insoluble aggregates. There was no correlation between pharmaceutically acceptability of the freeze-dried cake and insoluble aggregate levels in the reconstituted product.

In-line multipoint near-infrared spectroscopy for moisture content quantification during freeze-drying.

PubMed

Kauppinen, Ari; Toiviainen, Maunu; Korhonen, Ossi; Aaltonen, Jaakko; Järvinen, Kristiina; Paaso, Janne; Juuti, Mikko; Ketolainen, Jarkko

2013-02-19

During the past decade, near-infrared (NIR) spectroscopy has been applied for in-line moisture content quantification during a freeze-drying process. However, NIR has been used as a single-vial technique and thus is not representative of the entire batch. This has been considered as one of the main barriers for NIR spectroscopy becoming widely used in process analytical technology (PAT) for freeze-drying. Clearly it would be essential to monitor samples that reliably represent the whole batch. The present study evaluated multipoint NIR spectroscopy for in-line moisture content quantification during a freeze-drying process. Aqueous sucrose solutions were used as model formulations. NIR data was calibrated to predict the moisture content using partial least-squares (PLS) regression with Karl Fischer titration being used as a reference method. PLS calibrations resulted in root-mean-square error of prediction (RMSEP) values lower than 0.13%. Three noncontact, diffuse reflectance NIR probe heads were positioned on the freeze-dryer shelf to measure the moisture content in a noninvasive manner, through the side of the glass vials. The results showed that the detection of unequal sublimation rates within a freeze-dryer shelf was possible with the multipoint NIR system in use. Furthermore, in-line moisture content quantification was reliable especially toward the end of the process. These findings indicate that the use of multipoint NIR spectroscopy can achieve representative quantification of moisture content and hence a drying end point determination to a desired residual moisture level.

Freeze-drying of tert-butyl alcohol/water cosolvent systems: effects of formulation and process variables on residual solvents.

PubMed

Wittaya-Areekul, S; Nail, S L

1998-04-01

The objective of this study was to identify significant formulation and processing variables affecting levels of tert-butyl alcohol (TBA) and isopropyl alcohol (IPA) in freeze-dried solids prepared from TBA/water cosolvent systems. The variables examined were the physical state of the solute (crystalline vs amorphous), initial TBA concentration, freezing rate, cake thickness, and the temperature and duration of secondary drying. Sucrose and glycine were used as models for noncrystallizing and crystallizing solutes, respectively. The TBA concentration above which eutectic crystallization takes place was determined by differential scanning calorimetry. Model formulations were subjected to extremes of freezing rate by either dipping in liquid nitrogen or by slowly freezing on the shelf of a freeze-dryer. Dynamics of solvent loss during secondary drying was determined by withdrawing samples as a function of time at different shelf temperatures using a thief system. On the basis of these studies, the most important determinant of residual TBA level is the physical state of the solute. Freeze-dried glycine contained very low levels of residual TBA (0.01-0.03%) regardless of freezing rate or initial TBA concentration. For freeze-dried sucrose, residual TBA levels were approximately 2 orders of magnitude higher and were significantly affected by initial TBA concentration and freezing rate. For the sucrose/TBA/water system, relatively low residual TBA levels were obtained when the initial TBA level was above the threshold concentration for eutectic crystallization of TBA, whereas samples freeze-dried from solutions containing TBA concentrations below this threshold contained significantly higher levels of TBA. Residual IPA levels increased continuously with initial concentration of TBA in the sucrose/TBA/water system. Formulations of sucrose/TBA/water which were frozen rapidly contained residual TBA levels which were approximately twice those measured in the same formulation after slow freezing and drying under the same conditions. For the sucrose/TBA/water system, the temperature and time of secondary drying had only minimal influence on residual TBA in the freeze-dried solid. At low initial TBA concentrations (2%), residual TBA increases with increased cake thickness, perhaps because of the influence of depth of fill on effective freezing rate.

[Preparation of freeze-dried powder of recombinate hirudin-2 nanoparticle for nasal delivery and permeability through nasal membrane in vitro].

PubMed

Chen, Ming-Xia; Zhang, Jian-Bao; Yu, Ji-Ping; Ye, Jing; Wei, Bao-Hong; Zhang, Yu-Jie

2013-06-01

To optimize the freeze-dried powder preparation technology of recombinate hirudin-2 (rHV2) nanoparticle which has bio-adhesive characteristic for nasal delivery, also to investigate its stability and permeability through nasal membrane in vitro. Taking the appearance, rediffusion of nanoparticle and rHV2 encapsulation efficiency as the evaluation indexes. Cryoprotector, the preparative technique and the effect of illumination and high temperature factors on its stability for rHV2 freeze-dried powder were investigated. Using Fraze diffusion cell technique, the permeability of rHV2 across rabbit nasal mucous membrane in chitosan solution, chitosan nanoparticle, and nanoparticle frozen-dried powder were compared with that in normal saline solution. The optimized preparation of rHV2 nanoparticle freeze-dried powder was as follows: 5% trehalose and glucose (1:1) was used as cryoprotector, nanoparticle solution was freezed for 24 h in vacuum frozen-dryer after being pre-freezed for 24 h. The content of rHV2 in the freeze-dried powder was 1.1 ug/mg. Illumination had little effect on the appearance, rediffusion and encapsulation efficiency of the rHV2 freeze-dried powder. High temperature could obviously influence the appearance of nanoparticle freeze-dried powder. The permeability coefficient (P) of nanoparticle was 5 times more than that in chictonson solution. It was indicated that chitosan nanoparticle has effect on increasing the permeability of rHV2. The freeze-dried powder of chitosan nanoparticle can be a good nasal preparation of rHV2.

Reduced pressure ice fog technique for controlled ice nucleation during freeze-drying.

PubMed

Patel, Sajal M; Bhugra, Chandan; Pikal, Michael J

2009-01-01

A method to achieve controlled ice nucleation during the freeze-drying process using an ice fog technique was demonstrated in an earlier report. However, the time required for nucleation was about 5 min, even though only one shelf was used, which resulted in Ostwald ripening (annealing) in some of the vials that nucleated earlier than the others. As a result, the ice structure was not optimally uniform in all the vials. The objective of the present study is to introduce a simple variation of the ice fog method whereby a reduced pressure in the chamber is utilized to allow more rapid and uniform freezing which is also potentially easier to scale up. Experiments were conducted on a lab scale freeze dryer with sucrose as model compound at different concentration, product load, and fill volume. Product resistance during primary drying was measured using manometric temperature measurement. Specific surface area of the freeze-dried cake was also determined. No difference was observed either in average product resistance or specific surface area for the different experimental conditions studied, indicating that with use of the reduced pressure ice fog technique, the solutions nucleated at very nearly the same temperature (-10 degrees C). The striking feature of the "Reduced Pressure Ice Fog Technique" is the rapid ice nucleation (less than a minute) under conditions where the earlier procedure required about 5 min; hence, effects of variable Ostwald ripening were not an issue.

Preservation of flavor in freeze dried green beans

NASA Technical Reports Server (NTRS)

Huber, C. S.; Heidelbaugh, N. D.; Davis, D.

1973-01-01

Before freeze drying, green beans are heated to point at which their cell structure is altered. Beans freeze dried with altered cell structure have improved rehydration properties and retain color, flavor, and texture.

Isolation, characterization of wheat gluten and its regeneration properties.

PubMed

Kaushik, Ravinder; Kumar, Naveen; Sihag, Manvesh Kumar; Ray, Aradhita

2015-09-01

In order to assess the effectiveness of different drying methods on physicochemical and reconstitution properties of wheat gluten, four wheat cultivars were selected and milled. Gluten was extracted and its wet and dry gluten content and water holding capacity were estimated. The washed starch and other flour constituents were dried. Isolated gluten was dried using three treatments viz. oven drying, vacuum drying and freeze drying. Dried gluten of four wheat cultivars were characterized for its water and oil absorption properties and thermal properties. The dried gluten and washed and dried flour constituents were then reconstituted and this flour was checked for flour quality (SDS volume, texture analysis and falling number). Only reconstituted flour using freeze dried gluten showed no significant difference to control flour in SDS volume and dough strength. In Falling number all reconstituted flour samples showed significant difference to control flour.

Folic acid content in thermostabilized and freeze-dried space shuttle foods

NASA Technical Reports Server (NTRS)

Lane, H. W.; Nillen, J. L.; Kloeris, V. L.

1995-01-01

This study was designed to determine whether freeze-dried and thermostabilized foods on a space shuttle contain adequate folate and to investigate any effects of freeze-drying on folacin. Frozen vegetables were analyzed after three states of processing: thawed; cooked; and rehydrated. Thermostabilized items were analyzed as supplied with no further processing. Measurable folate decreased in some freeze-dried vegetables and increased in others. Folacin content of thermostabilized food items was comparable with published values. We concluded that although the folacin content of some freeze-dried foods was low, adequate folate is available from the shuttle menu to meet RDA guidelines.

Solidification of liposomes by freeze-drying: the importance of incorporating gelatin as interior support on enhanced physical stability.

PubMed

Guan, Peipei; Lu, Yi; Qi, Jianping; Niu, Mengmeng; Lian, Ruyue; Wu, Wei

2015-01-30

The main purpose of this study was to investigate the effect of gelatin as interior support on the physical stability of freeze-dried liposomes. Anticancer agent paclitaxel (PTX) was selected as a model drug. Freeze-dried liposomes containing interior gelatin support (GLs) were prepared by thin-film dispersion/freeze-drying method. Several properties of the GLs, including entrapment efficiency, particle size and gelation temperature, were extensively characterized. Encapsulation efficiency of conventional liposomes (CLs) and liposomes containing lyoprotectants as interior support dropped to lower than 20% after reconstitution, while GLs still maintained an entrapment efficiency of over 84%. Scanning electron microscopy revealed well preserved liposomal structure of GLs after reconstitution. Meanwhile, the particle size and entrapment efficiency of GLs were also well preserved after reconstitution. In contrary, deformation of CLs and recrystallization of PTX were observed, as well as significant changes in particle size and entrapment efficiency. Taken together, interior gelatin support obviously enhanced the physical stability of liposomes against the lyophilization stress. Copyright © 2014 Elsevier B.V. All rights reserved.

Freeze-Drying of Plant Tissue Containing HBV Surface Antigen for the Oral Vaccine against Hepatitis B

PubMed Central

Milczarek, Magdalena; Pajtasz-Piasecka, Elżbieta; Wietrzyk, Joanna

2014-01-01

The aim of this study was to develop a freeze-drying protocol facilitating successful processing of plant material containing the small surface antigen of hepatitis B virus (S-HBsAg) while preserving its VLP structure and immunogenicity. Freeze-drying of the antigen in lettuce leaf tissue, without any isolation or purification step, was investigated. Each process step was consecutively evaluated and the best parameters were applied. Several drying profiles and excipients were tested. The profile of 20°C for 20 h for primary and 22°C for 2 h for secondary drying as well as sucrose expressed efficient stabilisation of S-HBsAg during freeze-drying. Freezing rate and postprocess residual moisture were also analysed as important factors affecting S-HBsAg preservation. The process was reproducible and provided a product with VLP content up to 200 µg/g DW. Assays for VLPs and total antigen together with animal immunisation trials confirmed preservation of antigenicity and immunogenicity of S-HBsAg in freeze-dried powder. Long-term stability tests revealed that the stored freeze-dried product was stable at 4°C for one year, but degraded at elevated temperatures. As a result, a basis for an efficient freeze-drying process has been established and a suitable semiproduct for oral plant-derived vaccine against HBV was obtained. PMID:25371900

Effect of mixing time, freeze-drying and baking on phenolics, anthocyanins and antioxidant capacity of raspberry juice during processing of muffins.

PubMed

Rosales-Soto, Maria U; Powers, Joseph R; Alldredge, J Richard

2012-05-01

Consumption of baked products constitutes an important part of a daily breakfast considering that people are continually grabbing meals on the go. Among baked products, muffins rank third in breakfast products and attract a broad range of consumers. Incorporation of red raspberry juice into muffins can add value to the product while preserving health benefits to the consumer. The purpose of this study was to evaluate the effect of mixing time, freeze-drying and baking on the phenolic and anthocyanin contents and antioxidant capacity of raspberry juice during the preparation of muffins. Freeze-drying of raspberry batters reduced their phenolic content and antioxidant capacity regardless of mixing time. Non-freeze-dried raspberry batter mixed for 5 min had the highest phenolic content (0.88 mg gallic acid equivalent g(-1) dry matter (DM)). Non-freeze-dried raspberry muffins had the highest antioxidant capacity (0.041 µmol Trolox equivalent g(-1) DM). Freeze-dried raspberry batters mixed for 5 and 10 min had the highest anthocyanin content (0.065 mg cyanidin-3-glucoside g(-1) DM). Baking reduced the anthocyanin content of both non-freeze-dried and freeze-dried raspberry muffins. Despite the reduction in valuable compounds, muffin is a vehicle for the delivery of these compounds. Copyright © 2012 Society of Chemical Industry.

Inulin rich carbohydrates extraction from Jerusalem artichoke (Helianthus tuberosus L.) tubers and application of different drying methods.

PubMed

Rubel, Irene A; Iraporda, Carolina; Novosad, Rocio; Cabrera, Fernanda A; Genovese, Diego B; Manrique, Guillermo D

2018-01-01

In this study the operational extraction variables to obtain higher yields of inulin from Jerusalem artichoke tubers (JAT), as well as the optimal conditions to obtain a stable and dispersible powdered product by either spray or freeze drying, were studied. With this purpose, the powder yield, moisture content, water activity and flowability or products obtained by different experimental conditions were analyzed. Inulin rich carbohydrates (IRC) extraction was performed from lyophilized and ground tubers employing distilled hot water as solvent. It was proved that the solid:solvent ratio (S:S) was the critical variable in the extraction process, followed by temperature. Thus, the IRC extraction was optimal without ultrasound assistance, at 76°C, employing a S:S of 1:16, during 90min. In addition, the powder obtained by freeze-drying of the IRC extract showed advantages respect to powders obtained by spray-drying regarding the yield and considering that maltodextrin was not necessary as encapsulation agent. In another hand, spray drying process provided IRC powered materials with appropriate flow properties, and taking into account cost and time of production, this method should be considered as an alternative of freeze-drying. Copyright © 2017 Elsevier Ltd. All rights reserved.

Implementation of a process analytical technology system in a freeze-drying process using Raman spectroscopy for in-line process monitoring.

PubMed

De Beer, T R M; Allesø, M; Goethals, F; Coppens, A; Heyden, Y Vander; De Diego, H Lopez; Rantanen, J; Verpoort, F; Vervaet, C; Remon, J P; Baeyens, W R G

2007-11-01

The aim of the present study was to propose a strategy for the implementation of a Process Analytical Technology system in freeze-drying processes. Mannitol solutions, some of them supplied with NaCl, were used as models to freeze-dry. Noninvasive and in-line Raman measurements were continuously performed during lyophilization of the solutions to monitor real time the mannitol solid state, the end points of the different process steps (freezing, primary drying, secondary drying), and physical phenomena occurring during the process. At-line near-infrared (NIR) and X-ray powder diffractometry (XRPD) measurements were done to confirm the Raman conclusions and to find out additional information. The collected spectra during the processes were analyzed using principal component analysis and multivariate curve resolution. A two-level full factorial design was used to study the significant influence of process (freezing rate) and formulation variables (concentration of mannitol, concentration of NaCl, volume of freeze-dried sample) upon freeze-drying. Raman spectroscopy was able to monitor (i) the mannitol solid state (amorphous, alpha, beta, delta, and hemihydrate), (ii) several process step end points (end of mannitol crystallization during freezing, primary drying), and (iii) physical phenomena occurring during freeze-drying (onset of ice nucleation, onset of mannitol crystallization during the freezing step, onset of ice sublimation). NIR proved to be a more sensitive tool to monitor sublimation than Raman spectroscopy, while XRPD helped to unravel the mannitol hemihydrate in the samples. The experimental design results showed that several process and formulation variables significantly influence different aspects of lyophilization and that both are interrelated. Raman spectroscopy (in-line) and NIR spectroscopy and XRPD (at-line) not only allowed the real-time monitoring of mannitol freeze-drying processes but also helped (in combination with experimental design) us to understand the process.

Optimization of pectin extraction and antioxidant activities from Jerusalem artichoke

NASA Astrophysics Data System (ADS)

Liu, Shengyi; Shi, Xuejie; Xu, Lanlan; Yi, Yuetao

2016-03-01

Jerusalem artichoke is an economic crop widely planted in saline-alkaline soil. The use of Jerusalem artichoke is of great significance. In this study, the response surface method was employed to optimize the effects of processing variables (extraction temperature, pH, extraction time, and liquid-to-solid ratio) on the yield of Jerusalem artichoke pectin. Under the optimal extraction conditions: pH 1.52, 63.62 min, 100°C and a liquid-to-solid ratio of 44.4 mL/g, the maximum pectin yield was predicted to be 18.76%. Experiments were conducted under these optimal conditions and a pectin yield of 18.52±0.90% was obtained, which validated the model prediction. The effects of diff erent drying methods (freeze drying, spray drying and vacuum drying) on the properties of Jerusalem artichoke pectin were evaluated and they were compared with apple pectin. FTIR spectral analysis showed no major structural diff erences in Jerusalem artichoke pectin samples produced by various drying treatments. The antioxidant activities of pectin dried by diff erent methods were investigated using in vitro hydroxyl and DPPH radical scavenging systems. The results revealed that the activities of spray dried pectin (SDP) and apple pectin (AP) were stronger than those of vacuum oven dried pectin (ODP) and vacuum freeze dried pectin (FDP). Therefore compared with the other two drying methods, the spray drying method was the best.

Protective effect of sugars on storage stability of microwave freeze-dried and freeze-dried Lactobacillus paracasei F19.

PubMed

Ambros, S; Hofer, F; Kulozik, U

2018-05-31

Microwave freeze drying in comparison to conventional freeze drying allows for intensification of the preservation process of lactic acid bacteria without imposing additional processing stress. Viability as a function of storage time of microwave freeze-dried Lactobacillus paracasei ssp. paracasei F19 was investigated in comparison to conventionally lyophilized bacteria of the same strain. Further, the impact of the protectants, sorbitol, trehalose and maltodextrin, on shelf life was analyzed. The highest inactivation rates of 0.035 and 0.045 d -1 , respectively, were found for cultures without protectants. Thus, all additives were found to exhibit a protective effect during storage with inactivation rates between 0.015 and 0.040 d -1 . Although trehalose and maltodextrin samples were in the glassy state during storage, in contrast to samples containing sorbitol as protectant, the best protective effect could be found for sorbitol with the lowest inactivation rate of 0.015 d -1 . Due to its low molecular weight, it might protect cells owing to better adsorption to the cytoplasma membrane. Sorbitol additionally shows antioxidative properties. Storage behavior of microwave freeze-dried cultures follows the typical behavior of a product dried by conventional lyophilization. No significant influence of the drying technique on storage behavior was detected. General findings concerning storage behavior in freeze drying are likely to be applicable in microwave freeze drying with only slight adjustments. This article is protected by copyright. All rights reserved. This article is protected by copyright. All rights reserved.

Depositing nanoparticles on a silicon substrate using a freeze drying technique.

PubMed

Sigehuzi, Tomoo

2017-08-28

For the microscopic observation of nanoparticles, an adequate sample preparation is an essential part of this task. Much research has been performed for usable preparation methods that will yield aggregate-free samples. A freeze drying technique, which only requires a -80  ° C freezer and a freeze dryer, is shown to provide an on-substrate dispersion of mostly isolated nanoparticles. The particle density could be made sufficiently high for efficient observations using atomic force microscopy. Since this sandwich method is purely physical, it could be applied to deposit various nanoparticles independent of their surface chemical properties. Suspension film thickness, or the dimensionality of the suspension film, was shown to be crucial for the isolation of the particles. Silica nanoparticles were dispersed on a silicon substrate using this method and the sample properties were examined using atomic force microscopy.

Collagen/hydroxyapatite composite materials with desired ceramic properties.

PubMed

Andronescu, Ecaterina; Voicu, Georgeta; Ficai, Maria; Mohora, Ioana Anita; Trusca, Roxana; Ficai, Anton

2011-01-01

Our purpose was to obtain and characterize some collagen/hydroxyapatite (COLL/HA) hybrid composite materials with desired ceramic properties. The ceramic properties of these materials were achieved by combining two drying methods: controlled air drying at 30°C followed by freeze-drying. Through the function of the air drying times, the materials morphology varies from porous materials (when the materials are freeze-dried) up to dense materials (when the materials are air-dried), while the combined drying allows us to obtain an intermediary morphology. The composite materials intended to be used as bone grafts and in a drug delivery system were characterized by XRD, FTIR, SEM, and also by determining the ceramic properties by using the Arthur method. The ceramic properties of these COLL/HA composite materials vary in large range, for instance the density of the materials varies from 0.06 up to 1.5 g/cm(3) while the porosity varies from 96.5% down to 27.5%.

Effect of moisture content on the invertase activity of freeze-dried S. cerevisiae.

PubMed

Pitombo, R N; Spring, C; Passos, R F; Tonato, M; Vitolo, M

1994-08-01

The invertase activity of intact Saccharomyces cerevisiae submitted to freezing-thawing was affected by pH, the chemical nature of the buffer, and the freezing cooling rate (CR), leading in some cases to a complete invertase inactivation (acetate buffer, pH 4.0, CR = 0.5 degree C/min). Once established under adequate freezing conditions the invertase activity remained unchanged after freeze-drying. Nevertheless, in some cases the cell-growing capability after freeze-drying diminished around 70%, mainly if the frozen cell suspension was attained through freezing carried out at CR = 0.5 degree C/min. Water sorption isotherms of freeze-dried samples (freeze-dryer Edwards L-4KR; 30 degrees C and 0.1 mB) were determined at 10 and 25 degrees C. The monolayer moisture content (MMC) at each temperature (12.7 and 3.71 for 10 and 25 degrees C, respectively) was calculated from isotherms by applying BET and GAB models. Freeze-dried yeast with water activity (Aw) between 0 and 0.33 (about the MMC value) maintained at 25 degrees C for 235 days and at 89 degrees C for 15 min retained at least 85% of its original invertase activity (IA), whereas samples with Aw > MMC lost at least 60% of its IA. X ray diffraction showed that the freeze-dried cake before and after storage presented an amorphous structure.

References on Compression of Freeze-Dried Foods

DTIC Science & Technology

1978-08-01

ready-to-eat, freeze-dried scrambled egg . Swift and Co., Contract No. DA 19- 129-AMC-121. 67-49-FD (FD-54). January 1967 (AD 650637). In the design...significantly poorer in organoleptic properties than from grades A and B eggs. Freeze- dried scrambled egg packed in cans kept better in storage than when...scrambled, cooked, freeze-dried whole egg product was developed which possessed the appearance, aroma, flavor and texture similar to pan- fried scrambled

Design of freeze-drying processes for pharmaceuticals: practical advice.

PubMed

Tang, Xiaolin; Pikal, Michael J

2004-02-01

Design of freeze-drying processes is often approached with a "trial and error" experimental plan or, worse yet, the protocol used in the first laboratory run is adopted without further attempts at optimization. Consequently, commercial freeze-drying processes are often neither robust nor efficient. It is our thesis that design of an "optimized" freeze-drying process is not particularly difficult for most products, as long as some simple rules based on well-accepted scientific principles are followed. It is the purpose of this review to discuss the scientific foundations of the freeze-drying process design and then to consolidate these principles into a set of guidelines for rational process design and optimization. General advice is given concerning common stability issues with proteins, but unusual and difficult stability issues are beyond the scope of this review. Control of ice nucleation and crystallization during the freezing step is discussed, and the impact of freezing on the rest of the process and final product quality is reviewed. Representative freezing protocols are presented. The significance of the collapse temperature and the thermal transition, denoted Tg', are discussed, and procedures for the selection of the "target product temperature" for primary drying are presented. Furthermore, guidelines are given for selection of the optimal shelf temperature and chamber pressure settings required to achieve the target product temperature without thermal and/or mass transfer overload of the freeze dryer. Finally, guidelines and "rules" for optimization of secondary drying and representative secondary drying protocols are presented.

Optimum Parameters for Freeze-Drying Decellularized Arterial Scaffolds

PubMed Central

Sheridan, William S.; Duffy, Garry P.

2013-01-01

Decellularized arterial scaffolds have achieved success in advancing toward clinical use as vascular grafts. However, concerns remain regarding long-term preservation and sterilization of these scaffolds. Freeze drying offers a means of overcoming these concerns. In this study, we investigated the effects of various freeze-drying protocols on decellularized porcine carotid arteries and consequently, determined the optimum parameters to fabricate a stable, preserved scaffold with unaltered mechanical properties. Freeze drying by constant slow cooling to two final temperatures ((Tf), −10°C and −40°C) versus instant freezing was investigated by histological examination and mechanical testing. Slow cooling to Tf= −10°C produced a stiffer and less distensible response than the non freeze-dried scaffolds and resulted in disruption to the collagen fibers. The mechanical response of Tf= −40°C scaffolds demonstrated disruption to the elastin network, which was confirmed with histology. Snap freezing scaffolds in liquid nitrogen and freeze drying to Tf= −40°C with a precooled shelf at −60°C produced scaffolds with unaltered mechanical properties and a histology resembling non-freeze-dried scaffolds. The results of this study demonstrate the importance of optimizing the nucleation and ice crystal growth/size to ensure homogenous drying, preventing extracellular matrix disruption and subsequent inferior mechanical properties. This new manufacturing protocol creates the means for the preservation and sterilization of decellularized arterial scaffolds while simultaneously maintaining the mechanical properties of the tissue. PMID:23614758

Solubility enhancement of BCS Class II drug by solid phospholipid dispersions: Spray drying versus freeze-drying.

PubMed

Fong, Sophia Yui Kau; Ibisogly, Asiye; Bauer-Brandl, Annette

2015-12-30

The poor aqueous solubility of BCS Class II drugs represents a major challenge for oral dosage form development. Using celecoxib (CXB) as model drug, the current study adopted a novel solid phospholipid nanoparticle (SPLN) approach and compared the effect of two commonly used industrial manufacturing methods, spray- and freeze-drying, on the solubility and dissolution enhancement of CXB. CXB was formulated with Phospholipoid E80 (PL) and trehalose at different CXB:PL:trehalose ratios, of which 1:10:16 was the optimal formulation. Spherical amorphous SPLNs with average diameters <1μm were produced by spray-drying; while amorphous 'matrix'-like structures of solid PL dispersion with larger particle sizes were prepared by freeze-drying. Formulations from both methods significantly enhanced the dissolution rates, apparent solubility, and molecularly dissolved concentration of CXB in phosphate buffer (PBS, pH 6.5) and in biorelevant fasted state simulated intestinal fluid (FaSSIF, pH 6.5) (p<0.05). While similar dissolution rates were found, the spray-dried SPLNs had a larger enhancement in apparent solubility (29- to 132-fold) as well as molecular solubility (18-fold) of CXB at equilibrium (p<0.05). The strong capability of the spray-dried SPLNs to attain 'true' supersaturation state makes them a promising approach for bioavailability enhancement of poorly soluble drugs. Copyright © 2015 Elsevier B.V. All rights reserved.

Freezing and drying effects on potential plant contributions to phosphorus in runoff.

PubMed

Roberson, Tiffany; Bundy, Larry G; Andraski, Todd W

2007-01-01

Phosphorus (P) in runoff from landscapes can promote eutrophication of natural waters. Soluble P released from plant material can contribute significant amounts of P to runoff particularly after plant freezing or drying. This study was conducted to evaluate P losses from alfalfa or grass after freezing or drying as potential contributors to runoff P. Alfalfa (Medicago sativa L.) and grass (principally, Agropyron repens L.) plant samples were subjected to freezing and drying treatments to determine P release. Simulated rainfall runoff and natural runoff from established alfalfa fields and a grass waterway were collected to study P contributions from plant tissue to runoff. The effects of freezing and drying on P released from plant tissue were simulated by a herbicide treatment in selected experiments. Soluble reactive P (SP) extracted from alfalfa and grass samples was markedly increased by freezing or drying. In general, SP extracted from plant samples increased in the order fresh < frozen < frozen/thawed < dried, and averaged 1, 8, 14, and 26% of total P in alfalfa, respectively. Soluble reactive P extracted from alfalfa after freezing or drying increased with increasing soil test P (r(2) = 0.64 to 0.68), suggesting that excessive soil P levels increased the risk of plant P contributions to runoff losses. In simulated rainfall studies, paraquat (1,1'-dimethyl-4, 4''-bipyridinium ion) treatment of alfalfa increased P losses in runoff, and results suggested that this treatment simulated the effects of drying on plant P loss. In contrast to the simulated rainfall results, natural runoff studies over 2 yr did not show higher runoff P losses that could be attributed to P from alfalfa. Actual P losses likely depend on the timing and extent of plant freezing and drying and of precipitation events after freezing.

Development of a compact freeze vacuum drying for jelly fish (Schypomedusae)

NASA Astrophysics Data System (ADS)

Alhamid, M. Idrus; Yulianto, M.; Nasruddin

2012-06-01

A new design of a freeze vacuum drying with internal cooling and heater from condenser's heat loss was built and tested. The dryer was used to dry jelly fish (schypomedusae), to study the effect of drying parameters such as the temperature within the drying chamber on mass losses (evaporation) during the freezing stage and the moisture ratio at the end of the drying process. The midili thin layer mathematical drying model was used to estimate and predict the moisture ratio curve based on different drying chamber temperatures. This experiment shows that decreasing the drying chamber temperature with constant pressure results in less mass loss during the freezing stage Drying time was reduced with an increase in drying temperature. Decreasing the drying chamber temperature results in lower pressure saturation of the material has no effect of drying chamber pressure on mass transfer.

Methods to increase the rate of mass transfer during osmotic dehydration of foods.

PubMed

Chwastek, Anna

2014-01-01

Traditional methods of food preservation such as freezing, freeze drying (lyophilization), vacuum drying, convection drying are often supplemented by new technologies that enable obtaining of high quality products. Osmotic dehydration is more and more often used during processing of fruits and vegetables. This method allows maintaining good organoleptic and functional properties in the finished product. Obtaining the desired degree of dehydration or saturation of the material with an osmoactive substance often requires  elongation of time or use of high temperatures. In recent years much attention was devoted to techniques aimed at increasing the mass transfer between the dehydrated material and the hypertonic solution. The work reviews the literature focused on methods of streamlining the process of osmotic dehydration which include the use of: ultrasound, high hydrostatic pressure, vacuum osmotic dehydration and pulsed electric field.

Development of freeze-dried miyeokguk, Korean seaweed soup, as space food sterilized by irradiation

NASA Astrophysics Data System (ADS)

Song, Beom-Seok; Park, Jin-Gyu; Kim, Jae-Hun; Choi, Jong-Il; Ahn, Dong-Hyun; Hao, Chen; Lee, Ju-Woon

2012-08-01

The purpose of this study was to evaluate microbial populations, Hunter's color values (L*, a*, b*) and the sensory quality of freeze-dried miyeokguk, Korean seaweed soup, in order to use it as space food. Microorganisms were not detected in non-irradiated freeze-dried miyeokguk within the detection limit of 1.00 log CFU/g. However, the microbial population in rehydrated miyeokguk was 7.01 log CFU/g after incubation at 35 °C for 48 h, indicating that freeze-dried miyeokguk was not sterilized by heat treatment during the preparation process. Bacteria in the freeze-dried miyeokguk were tentatively identified as Bacillus cereus, B. subtilis, Enterobacter hormaechei, and Ancinetobacter genomosp. using the 16S rDNA sequencing. In samples that were gamma-irradiated above 10 kGy, it was confirmed that all microorganisms were inactivated. Hunter's color values of the samples irradiated at doses less than 10 kGy were not significantly altered from their baseline appearance (p>0.05). Sensory evaluation showed that preference scores in all sensory properties decreased when freeze-dried miyeokguk was irradiated at doses greater than 10 kGy. Therefore, the results of this study suggest that gamma irradiation at 10 kGy is sufficient to sterilize freeze-dried miyeokguk without significant deterioration in the sensory quality, and thus, the freeze-dried and irradiated miyeokguk at 10 kGy fulfills the microbiological requirements as space food.

An environmentally friendly method for the fabrication of reduced graphene oxide foam with a super oil absorption capacity.

PubMed

He, Yongqiang; Liu, Yue; Wu, Tao; Ma, Junkui; Wang, Xingrui; Gong, Qiaojuan; Kong, Weina; Xing, Fubao; Liu, Yu; Gao, Jianping

2013-09-15

Three kinds of graphene oxide (GO) foams were fabricated using different freezing methods (unidirectional freezing drying (UDF), non-directional freezing drying, and air freezing drying), and the corresponding reduced graphene oxide (RGO) foams were prepared by their thermal reduction of those GO foams. These RGO foams were characterized by Fourier transform infrared spectroscopy, thermal gravimetric analysis, X-ray diffraction, X-ray photoelectron spectroscopy, and scanning electron microscopy. The absorption process and the factors that influence the absorption capacity were investigated. The RGO foams are hydrophobic and showed extremely high absorbing abilities for organic liquids. The absorption capacity of the RGO foams made by UDF was higher than 100 g g(-1) for all the oils tested (gasoline, diesel oil, pump oil, lubricating oil and olive oil) and had the highest value of about 122 g g(-1) for olive oil. The oil absorption capacity of the GO foams was lower than that of the RGO foams, but for olive oil, the absorption capacity was still high than 70 g g(-1), which is higher than that of most oil absorbents. Copyright © 2013 Elsevier B.V. All rights reserved.

Effect of drying methods (microwave vacuum, freeze, hot air and sun drying) on physical, chemical and nutritional attributes of five pepper (Capsicum annuum var. annuum) cultivars.

PubMed

Maurya, Vaibhav Kumar; Gothandam, Kodiveri Muthukaliannan; Ranjan, Vijay; Shakya, Amita; Pareek, Sunil

2018-07-01

A randomized block design experiment was performed to investigate the influence of drying on the physical, chemical and nutritional quality attributes of five prominent cultivars of India under sun drying (SD) (mean temperature 35.5 °C, average daily radiation 5.26 kW h m -2 and mean relative humidity 73.66% RH), hot air drying (HD) at 65 °C, microwave vacuum drying (MVD) (800 W, 5 kPa) and freeze drying (FD) (-50 °C, 5 kPa). Water activity, pH, total phenolic content (TPC), ascorbic acid (AA), capsaicin, β-carotene, color and Scoville heat unit were studied. TPC, AA, capsaicin content, β-carotene, color and water activity were significantly affected by the drying method. FD was observed to be most efficient in minimizing the loss of color, capsaicin and β-carotene. The hotness of analyzed samples decreased in the order 'Bird's Eye' > 'Sannam S4' > 'CO-4' > 'PLR-1' > 'PKM-1' among the studied cultivars, and FD > MVD > HD > SD among the drying methods. The FD method was observed to be the most efficient drying method for retaining capsaicin content over other drying methods (SD, HD, MVD), whereas MVD was found to be most efficient in minimizing the loss to nutritional attributes for all five pepper cultivars. © 2018 Society of Chemical Industry. © 2018 Society of Chemical Industry.

Effect of hot-boned pork on the keeping quality of fresh pork sausage.

PubMed

Guerrero Legarreta, I; Usborne, W R; Ashton, G C

1987-01-01

The first experiment evaluated the effect of solid carbon dioxide (dry ice) addition to hot-boned meat, in different proportions, upon the keeping quality of fresh pork sausage patties. Dry ice had some negative effects at levels of 20% to 40%, such as hardening and colour fading of samples, although it increased water-holding capacity of the sausage. In the second experiment three proportions of hot-boned meat and chilled meat were evaluated as a means to extend the retail storage time of fresh pork sausage links. Hot-boned pork was treated by three methods: freezing the meat before grinding, salting and freezing, and salting plus dry ice addition. The results favoured the use of 50% hot-boned meat and 50% chilled meat, for which the lowest hardness and oxidation values were obtained. Microbial counts and hue values showed no significant variation among the three treatments. Salting and freezing hot-boned meat before grinding was the method which produced the best overall quality. Copyright © 1987. Published by Elsevier Ltd.

Proximate composition, total phenolic content, and antioxidant activity of seagrape (Caulerpa lentillifera).

PubMed

Nguyen, Van Tang; Ueng, Jinn-Pyng; Tsai, Guo-Jane

2011-09-01

The proximate composition of seagrape (Caulerpa lentillifera) from culture ponds in Penghu, Taiwan was analyzed. The phenolic content and the antioxidant activities including the 1,1-diphenyl-2-picryl-hydrazil (DPPH) radical scavenging activity, ferric ion-reducing activity, hydrogen peroxide scavenging activity, and ferrous ion chelating (FIC) activity of the ethanolic extracts of dry seagrape samples using 2 drying methods of freeze drying and thermal drying were compared with the ethanolic extract of Oolong tea as a reference. The contents (dry weight basis) of carbohydrate, crude protein, crude lipid, crude fiber, and ash of seagrape obtained from culture ponds in Taiwan were 64.00%, 9.26%, 1.57%, 2.97%, and 22.20%, respectively. The total phenolic content (1.30 mg gallic acid equivalent [GAE]/g dry weight) of the ethanolic extract of thermally dried seagrape was significantly lower (P < 0.05) than that (2.04 mg GAE/g dry weight) of freeze-dried seagrape, and both were significantly lower than that (13.58 mg GAE/g dry weight) of Oolong tea. At the same phenolic content, the antioxidant activities of freeze-dried seagrape were significantly higher (P < 0.05) than those of thermally dried seagrape. Compared with Oolong tea, seagrape, irrespective of drying method used, generally had strong hydrogen peroxide scavenging activity; but it was weak in DPPH radical scavenging activity, ferric ion-reducing activity, and FIC activity. The antioxidant activity of seagrape and Oolong tea was significantly influenced by their phenolic contents. The proximate composition, total phenolic content, and antioxidant activity of seagrape (Caulerpa lentillifera) in Taiwan were determined in this research to indicate nutritionally of this edible seaweed to human health, and compared these results to previous studies. © 2011 Institute of Food Technologists®

Headspace Moisture Mapping and the Information That Can Be Gained about Freeze-Dried Materials and Processes.

PubMed

Cook, Isobel A; Ward, Kevin R

2011-01-01

Regulatory authorities require proof that lyophilization (freeze drying) cycles have been developed logically and demonstrate uniformity. One measure of uniformity can be consistency of residual water content throughout a batch. In primary drying, heat transfer is effected by gaseous convection and conduction as well as the degree of shelf contact and evenness of heat applied; therefore residual water can be affected by container location, degree of container/tray/shelf contact, radiative heating, packing density, product formulation, and the cycle conditions themselves. In this study we have used frequency modulation spectroscopy (FMS) to create a map of headspace moisture (HSM) for 100% of vials within a number of freeze-dried batches. Karl Fischer (KF)/HSM correlations were investigated in parallel with the moisture mapping studies. A clear, linear relationship was observed between HSM and KF values for vials containing freeze-dried sucrose, implying a relatively straightforward interaction between water and the lyophilized cake for this material. Mannitol demonstrated a more complex correlation, with the interaction of different crystalline forms giving important information on the uniformity of the material produced. It was observed that annealing had a significant impact on the importance of heat transfer by conduction for vials in direct and non-direct contact with the shelf. Moisture mapping of all vials within the freeze dryer enabled further information to be obtained on the relationship of the formulation, process conditions, and equipment geometry on the intra-batch variability in HSM level. The ability of FMS to allow 100% inspection could mean that this method could play an important part in process validation and quality assurance. Lyophilization, also known as freeze drying, is a relatively old technique that has been used in its most basic form for thousands of years (e.g., preservation of fish and meat products). In its more advanced form it is used to preserve many medical products; for example, many vaccines are not stable in solution and therefore need to be dried to allow long-term storage. In order to produce a freeze-dried vaccine, a complex understanding of the processes and critical temperatures is required. Once these have been understood, the material is dried to give relatively low moisture content (e.g., 2% w/w.) This low moisture content is critical for the long-term stability of the product, allowing doctors/chemists to store these goods on site for use when required. This research paper provides further information on a technique called frequency modulation spectroscopy (FMS) that has been used to map the moisture variation across samples within a freeze dryer, enabling us to increase our understanding of the role various processing conditions play on the relationship between the product and water. It has demonstrated its potential application for 100% batch monitoring and the validation of a system or assessment of changes made. This method could assist in improving quality assurance and ultimately the final product that reaches the consumer.

Quality of Dried Bacillus NP5 and its Effect on Growth Performance of Tilapia (Oreochromis niloticus).

PubMed

Utami, Diah Ayu Satyari; Widanarni; Suprayudi, M Agus

2015-02-01

The main things that need to be considered in the preparation of probiotics are viability during preparation and storage which are the disadvantages of the use of fresh culture probiotics. Dried probiotic can be applied through the feed, easy to be applied and has a long shelf life but application of dried probiotic in aquaculture is still not widely studied. This study aimed to evaluate the quality of dried Bacillus NP5 as the probiotic through in vitro assays and determine the best dose for the growth performance of tilapia. The treatment of in vitro assays including the production of dried probiotic without using of the coating material and dried by spray drying method (NS); freeze drying method (NF); with using of the coating material and dried by spray drying method (WS); freeze drying method (WF). The treatment which showed the best result at in vitro assays was applied for in vivo assays. The in vivo assays containing 4 treatments and 5 replicates which were control (K) and the administration of dried Bacillus NP5 Rf(R) (10(10) CFU g(-1)) in feed with dose of 0.5% (A), 1% (B) and 2% (C). The fish fed 3 times a day by at satiation for 28 days. Probiotic that encapsulated by maltodextrin and dried by spray drying method that stored in room temperature had the higher percentage product, viability after drying process and storage. The administration of 0.5% dried Bacillus NP5 showed the best growth performance in tilapia.

Method for low temperature preparation of a noble metal alloy

DOEpatents

Even, Jr., William R.

2002-01-01

A method for producing fine, essentially contamination free, noble metal alloys is disclosed. The alloys comprise particles in a size range of 5 to 500 nm. The method comprises 1. A method for preparing a noble metal alloy at low temperature, the method comprising the steps of forming solution of organometallic compounds by dissolving the compounds into a quantity of a compatible solvent medium capable of solvating the organometallic, mixing a portion of each solution to provide a desired molarity ratio of ions in the mixed solution, adding a support material, rapidly quenching droplets of the mixed solution to initiate a solute-solvent phase separation as the solvent freezes, removing said liquid cryogen, collecting and freezing drying the frozen droplets to produce a dry powder, and finally reducing the powder to a metal by flowing dry hydrogen over the powder while warming the powder to a temperature of about 150.degree. C.

Toward intradermal vaccination: preparation of powder formulations by collapse freeze-drying.

PubMed

Etzl, Elsa E; Winter, Gerhard; Engert, Julia

2014-03-01

Intradermal powder immunization is an emerging technique in vaccine delivery. The purpose of this study was to generate powder particles for intradermal injection by freeze-drying and subsequent cryo-milling. Two different freeze-drying protocols were compared, a moderate freeze-drying cycle and an aggressive freeze-drying cycle, which induced a controlled collapse of the sugar matrix. Ovalbumin served as model antigen. The influence of collapse drying and cryo-milling on particle morphology and protein stability was investigated. Cryo-milling generated irregularly shaped particles of size 20-70 µm. The recovery of soluble monomer of ovalbumin was not changed during freeze-drying and after cryo-milling, or after 12 months of storage at 2-8 °C. A slight increase in higher molecular weight aggregates was found in formulations containing the polymer dextran after 12 months of storage at 50 °C. Light obscuration measurements showed an increase in cumulative particle counts after cryo-milling that did not further increase during storage at 2-8 °C for 12 months. The applicability of the cryo-milling process to other therapeutic proteins was shown using recombinant human granulocyte-colony stimulating factor. Collapse freeze-drying and subsequent cryo-milling allows the generation of particles suitable for intradermal powder injection.

Raman microscopy of freeze-dried mouse eyeball-slice in conjunction with the "in vivo cryotechnique".

PubMed

Terada, Nobuo; Ohno, Nobuhiko; Saitoh, Sei; Fujii, Yasuhisa; Ohguro, Hiroshi; Ohno, Shinichi

2007-07-01

The wavelength of Raman-scattered light depends on the molecular composition of the substance. This is the first attempt to acquire Raman spectra of a mouse eyeball removed from a living mouse, in which the eyeball was preserved using the "in vivo cryotechnique" followed by freeze-drying. Eyeballs were cryofixed using a rapid freezing cryotechnique, and then sliced in the cryostat machine. The slices were sandwiched between glass slides, freeze-dried, and analyzed with confocal Raman microscopy. Important areas including various eyeball tissue layers were selected using bright-field microscopy, and then the Raman spectra were obtained at 240 locations. Four typical patterns of Raman spectra were electronically mapped on the specimen images obtained by the bright-field microscopy. Tissue organization was confirmed by embedding the same eyeball slice used for Raman spectra into epoxy resin and the thick sections were prepared with the inverted capsule method. Each Raman spectral pattern represents a different histological layer in the eyeball which was mapped by comparing the images of toluidine blue staining and Raman mapping with different colors. In the choroid and pigment cell layer, the Raman spectrum had two peaks, corresponding to melanin. Some of the peaks of the Raman spectra obtained from the blood vessels in sclera and the photoreceptor layer were similar to those obtained from the purified hemoglobin and rhodopsin proteins, respectively. Our experimental protocol can distinguish different tissue components with Raman microscopy; therefore, this method can be very useful for examining the distribution of a biological structures and/or chemical components in rapidly frozen freeze-dried tissue.

49 CFR 1039.10 - Exemption of agricultural commodities except grain, soybeans, and sunflower seeds.

Code of Federal Regulations, 2010 CFR

2010-10-01

... other marine products. 20-11 Fresh meat. 20-15 Fresh dressed poultry. 20-17 Processed poultry. 20-21.... 20-999-76 Freeze-dried poultry. 20-999-77 Freeze-dried meat. 20-999-78 Freeze-dried salad ingredients...

Controlled crystallization of the lipophilic drug fenofibrate during freeze-drying: elucidation of the mechanism by in-line Raman spectroscopy.

PubMed

de Waard, Hans; De Beer, Thomas; Hinrichs, Wouter L J; Vervaet, Chris; Remon, Jean-Paul; Frijlink, Henderik W

2010-12-01

We developed a novel process, "controlled crystallization during freeze-drying" to produce drug nanocrystals of poorly water-soluble drugs. This process involves freeze-drying at a relatively high temperature of a drug and a matrix material from a mixture of tertiary butyl alcohol and water, resulting in drug nanocrystals incorporated in a matrix. The aim of this study was to elucidate the mechanisms that determine the size of the drug crystals. Fenofibrate was used as a model lipophilic drug. To monitor the crystallization during freeze-drying, a Raman probe was placed just above the sample in the freeze-dryer. These in-line Raman spectroscopy measurements clearly revealed when the different components crystallized during freeze-drying. The solvents crystallized only during the freezing step, while the solutes only crystallized after the temperature was increased, but before drying started. Although the solutes crystallized only after the freezing step, both the freezing rate and the shelf temperature were critical parameters that determined the final crystal size. At a higher freezing rate, smaller interstitial spaces containing the freeze-concentrated fraction were formed, resulting in smaller drug crystals (based on dissolution data). On the other hand, when the solutes crystallized at a lower shelf temperature, the degree of supersaturation is higher, resulting in a higher nucleation rate and consequently more and therefore smaller crystals. In conclusion, for the model drug fenofibrate, a high freezing rate and a relatively low crystallization temperature resulted in the smallest crystals and therefore the highest dissolution rate.

Emerging freeze-drying process development and scale-up issues.

PubMed

Patel, Sajal Manubhai; Pikal, Michael J

2011-03-01

Although several guidelines do exist for freeze-drying process development and scale-up, there are still a number of issues that require additional attention. The objective of this review article is to discuss some emerging process development and scale-up issue with emphasis on effect of load condition and freeze-drying in novel container systems such as syringes, Lyoguard trays, ampoules, and 96-well plates. Understanding the heat and mass transfer under different load conditions and for freeze-drying in these novel container systems will help in developing a robust freeze-drying process which is also easier to scale-up. Further research and development needs in these emerging areas have also been addressed. © 2011 American Association of Pharmaceutical Scientists

Quality by design: optimization of a freeze-drying cycle via design space in case of heterogeneous drying behavior and influence of the freezing protocol.

PubMed

Pisano, Roberto; Fissore, Davide; Barresi, Antonello A; Brayard, Philippe; Chouvenc, Pierre; Woinet, Bertrand

2013-02-01

This paper shows how to optimize the primary drying phase, for both product quality and drying time, of a parenteral formulation via design space. A non-steady state model, parameterized with experimentally determined heat and mass transfer coefficients, is used to define the design space when the heat transfer coefficient varies with the position of the vial in the array. The calculations recognize both equipment and product constraints, and also take into account model parameter uncertainty. Examples are given of cycles designed for the same formulation, but varying the freezing conditions and the freeze-dryer scale. These are then compared in terms of drying time. Furthermore, the impact of inter-vial variability on design space, and therefore on the optimized cycle, is addressed. With this regard, a simplified method is presented for the cycle design, which reduces the experimental effort required for the system qualification. The use of mathematical modeling is demonstrated to be very effective not only for cycle development, but also for solving problem of process transfer. This study showed that inter-vial variability remains significant when vials are loaded on plastic trays, and how inter-vial variability can be taken into account during process design.

Production of inhalation phage powders using spray freeze drying and spray drying techniques for treatment of respiratory infections

PubMed Central

Leung, Sharon S.Y.; Parumasivam, Thaigarajan; Gao, Fiona G.; Carrigy, Nicholas B.; Vehring, Reinhard; Finlay, Warren H.; Morales, Sandra; Britton, Warwick J; Kutter, Elizabeth; Chan, Hak-Kim

2016-01-01

Purpose The potential of aerosol phage therapy for treating lung infections has been demonstrated in animal models and clinical studies. This work compared the performance of two dry powder formation techniques, spray freeze drying (SFD) and spray drying (SD), in producing inhalable phage powders. Method A Pseudomonas podoviridae phage, PEV2, was incorporated into multi-component formulation systems consisting of trehalose, mannitol and L-leucine (F1 = 60:20:20 and F2 = 40:40:20). The phage titer loss after the SFD and SD processes and in vitro aerosol performance of the produced powders were assessed. Results A significant titer loss (~ 2 log) was noted for droplet generation using an ultrasonic nozzle employed in the SFD method, but the conventional two-fluid nozzle used in the SD method was less destructive for the phage (~0.75 log loss). The phage were more vulnerable during the evaporative drying process (~0.75 log further loss) compared with the freeze drying step, which caused negligible phage loss. In vitro aerosol performance showed that the SFD powders (~80% phage recovery) provided better phage protection than the SD powders (~20% phage recovery) during the aerosolization process. Despite this, higher total lung doses were obtained for the SD formulations (SD-F1 = 13.1 ± 1.7 × 104 pfu and SD-F2 = 11.0 ± 1.4 × 104 pfu) than from their counterpart SFD formulations (SFD-F1 = 8.3 ± 1.8 × 104 pfu and SFD-F2 = 2.1 ± 0.3 × 104 pfu). Conclusion Overall, the SD method caused less phage reduction during the powder formation process and the resulted powders achieved better aerosol performance for PEV2. PMID:26928668

Effects of sample drying and storage, and choice of extraction solvent and analysis method on the yield of birch leaf hydrolyzable tannins.

PubMed

Salminen, Juha-Pekka

2003-06-01

In this study, I investigated the effects of different methods of sample drying and storage, and the choice of extraction solvent and analysis method on the concentrations of 14 individual hydrolyzable tannins (HTs), and insoluble ellagitannins in birch (Betula pubescens) leaves. Freeze- and vacuum-drying of birch leaves were found to provide more reliable results than air- or oven-drying. Storage of leaves at -20 degrees C for 3 months before freeze-drying did not cause major changes in tannin content, although levels of 1,2,3,4,6-penta-O-galloylglucose and isostrictinin were altered. Storage of dried leaf material at -20 degrees C is preferred because 1 year storage of freeze-dried leaves at 4 degrees C and at room temperature decreased the concentration of the pedunculagin derivative, one of the main ellagitannins of birch. Furthermore, storage at room temperature increased the levels of isostrictinin and 2,3-(S)-HHDP-glucose, indicating possible HT catabolism. Of the extraction solvents tested, aqueous acetone was superior to pure acetone, or aqueous or pure methanol. The addition of 0.1% ascorbic acid into 70% acetone significantly increased the yield of ellagitannins. presumably by preventing their oxidation. By comparing the conventional rhodanine assay and the HPLC-ESI-MS assay for quantification of leaf galloylglucoses, the former tends to underestimate total concentrations of galloylglucoses in birch leaf extract. On the basis of the outcomes of all the method and solvent comparisons, their suitability for qualitative and quantitative analysis of plant HTs is discussed, emphasizing that each plant species, with its presumably unique HT composition, is likely to have a unique combination of ideal conditions for tissue preservation and extraction.

Encapsulation of lactase in Ca(II)-alginate beads: Effect of stabilizers and drying methods.

PubMed

Traffano-Schiffo, Maria Victoria; Castro-Giraldez, Marta; Fito, Pedro J; Santagapita, Patricio R

2017-10-01

The purpose of the present work was to analyze the effect of trehalose, arabic and guar gums on the preservation of β-galactosidase activity in freeze-dried and vacuum dried Ca(II)-alginate beads. Freezing process was also studied as a first step of freeze-drying. Trehalose was critical for β-galactosidase conservation, and guar gum as a second excipient showed the highest conservation effect (close to 95%). Systems with T g values ~40°C which were stables at ambient temperature were obtained, being trehalose the main responsible of the formation of an amorphous matrix. Vacuum dried beads showed smaller size (with Feret's diameter below 1.08±0.09mm), higher circularity (reaching 0.78±0.06) and large cracks in their surface than freeze-dried beads, which were more spongy and voluminous. Ice crystallization of the beads revealed that the crystallization of Ca(II)-alginate system follows the Avrami kinetics of nucleation and growth. Particularly, Ca(II)-alginate showed an Avrami index of 2.03±0.07, which means that crystal growing is bidimensional. Neither the addition of trehalose nor gums affected the dimension of the ice growing or its rate. These results open an opportunity in the development of new lactic products able to be consumed by lactose intolerance people. Copyright © 2017 Elsevier Ltd. All rights reserved.

Novel Budesonide Particles for Dry Powder Inhalation Prepared Using a Microfluidic Reactor Coupled With Ultrasonic Spray Freeze Drying.

PubMed

Saboti, Denis; Maver, Uroš; Chan, Hak-Kim; Planinšek, Odon

2017-07-01

Budesonide (BDS) is a potent active pharmaceutical ingredient, often administered using respiratory devices such as metered dose inhalers, nebulizers, and dry powder inhalers. Inhalable drug particles are conventionally produced by crystallization followed by milling. This approach tends to generate partially amorphous materials that require post-processing to improve the formulations' stability. Other methods involve homogenization or precipitation and often require the use of stabilizers, mostly surfactants. The purpose of this study was therefore to develop a novel method for preparation of fine BDS particles using a microfluidic reactor coupled with ultrasonic spray freeze drying, and hence avoiding the need of additional homogenization or stabilizer use. A T-junction microfluidic reactor was employed to produce particle suspension (using an ethanol-water, methanol-water, and an acetone-water system), which was directly fed into an ultrasonic atomization probe, followed by direct feeding to liquid nitrogen. Freeze drying was the final preparation step. The result was fine crystalline BDS powders which, when blended with lactose and dispersed in an Aerolizer at 100 L/min, generated fine particle fraction in the range 47.6% ± 2.8% to 54.9% ± 1.8%, thus exhibiting a good aerosol performance. Subsequent sample analysis confirmed the suitability of the developed method to produce inhalable drug particles without additional homogenization or stabilizers. The developed method provides a viable solution for particle isolation in microfluidics in general. Copyright © 2017 American Pharmacists Association®. All rights reserved.

Freeze-dried stallion spermatozoa: evaluation of two chelating agents and comparative analysis of three sperm DNA damage assays.

PubMed

Olaciregui, M; Luño, V; Martí, J I; Aramayona, J; Gil, L

2016-11-01

During the freeze-drying procedure, sperm DNA might become damaged by both freezing and drying stresses. Sperm DNA status can be detected using well-established assays; however, most techniques are expensive and involve elaborate protocols and equipment. Indirect assessments can provide alternative strategies. The objective of this study was to compare a simple test of DNA status using Diff-Quik (DQ) with two established procedures: acridine orange test (AOT) and sperm chromatin dispersion (SCD) on freeze-dried (FD) stallion spermatozoa. Ejaculated spermatozoa from three stallions were freeze-dried in basic medium supplemented with two different chelating agents: EGTA or EDTA. After rehydration, the spermatozoa were subjected to DNA damage detection using a SCDt, AOT and DQ stain simultaneously. The results showed that the DNA damage levels in the EGTA group were significantly lower than those in the EDTA group. AOT detected a significantly higher proportion of spermatozoa with fragmented DNA than DQ and SCD. The results of the SCD test and DQ stain exhibited a significant positive correlation for DNA fragmentation (r = 0.528), whereas a negative correlation was observed between SCD, DQ and AOT (r = -0.134 and r = -0.332 respectively). The present study shows that both the SCD test and DQ assay are effective methods for detecting FD stallion sperm DNA fragmentation, whereas using of AOT is questionable. © 2016 Blackwell Verlag GmbH.

State transitions and physicochemical aspects of cryoprotection and stabilization in freeze-drying of Lactobacillus rhamnosus GG (LGG).

PubMed

Pehkonen, K S; Roos, Y H; Miao, S; Ross, R P; Stanton, C

2008-06-01

The frozen and dehydrated state transitions of lactose and trehalose were determined and studied as factors affecting the stability of probiotic bacteria to understand physicochemical aspects of protection against freezing and dehydration of probiotic cultures. Lactobacillus rhamnosus GG was frozen (-22 or -43 degrees C), freeze-dried and stored under controlled water vapour pressure (0%, 11%, 23% and 33% relative vapour pressure) conditions. Lactose, trehalose and their mixture (1 : 1) were used as protective media. These systems were confirmed to exhibit relatively similar state transition and water plasticization behaviour in freeze-concentrated and dehydrated states as determined by differential scanning calorimetry. Ice formation and dehydrated materials were studied using cold-stage microscopy and scanning electron microscopy. Trehalose and lactose-trehalose gave the most effective protection of cell viability as observed from colony forming units after freezing, dehydration and storage. Enhanced cell viability was observed when the freezing temperature was -43 degrees C. State transitions of protective media affect ice formation and cell viability in freeze-drying and storage. Formation of a maximally freeze-concentrated matrix with entrapped microbial cells is essential in freezing prior to freeze-drying. Freeze-drying must retain a solid amorphous state of protectant matrices. Freeze-dried matrices contain cells entrapped in the protective matrices in the freezing process. The retention of viability during storage seems to be controlled by water plasticization of the protectant matrix and possibly interactions of water with the dehydrated cells. Highest cell viability was obtained in glassy protective media. This study shows that physicochemical properties of protective media affect the stability of dehydrated cultures. Trehalose and lactose may be used in combination, which is particularly important for the stabilization of probiotic bacteria in dairy systems.

Infrared Drying as a Quick Preparation Method for Dried Tangerine Peel

PubMed Central

Xu, Mingyue; Zhao, Chengying; Ahmad, Aftab; Zhang, Huijuan; Xiao, Hang

2017-01-01

To establish the most convenient and effective method to dry tangerine peels, different methods (sun drying, hot-air drying, freeze drying, vacuum drying, and medium- and short-wave infrared drying) were exploited. Our results indicated that medium- and short-wave infrared drying was the best method to preserve nutraceutical components; for example, vitamin C was raised to 6.77 mg/g (D.W.) from 3.39 mg/g (sun drying). Moreover, the drying time can be shortened above 96% compared with sun drying. Importantly, the efficiency of DPPH radical scavenging was enhanced from 26.66% to 55.92%. These findings would provide a reliable and time-saving methodology to produce high-quality dried tangerine peels. PMID:29348752

Use of a soft sensor for the fast estimation of dried cake resistance during a freeze-drying cycle.

PubMed

Bosca, Serena; Barresi, Antonello A; Fissore, Davide

2013-07-15

This paper deals with the determination of dried cake resistance in a freeze-drying process using the Smart Soft Sensor, a process analytical technology recently proposed by the authors to monitor the primary drying stage of a freeze-drying process. This sensor uses the measurement of product temperature, a mathematical model of the process, and the Kalman filter algorithm to estimate the residual amount of ice in the vial as a function of time, as well as the coefficient of heat transfer between the shelf and the product and the resistance of the dried cake to vapor flow. It does not require expensive (additional) hardware in a freeze-dryer, provided that thermocouples are available. At first, the effect of the insertion of the thermocouple in a vial on the structure of the product is investigated by means of experimental tests, comparing both sublimation rate and cake structure in vials with and without thermocouple. This is required to assess that the temperature measured by the thermocouple is the same of the product in the non-monitored vials, at least in a non-GMP environment, or when controlled nucleation methods are used. Then, results about cake resistance obtained in an extended experimental campaign with aqueous solutions containing different excipients (sucrose, mannitol and polyvinylpyrrolidone), processed in various operating conditions, are presented, with the goal to point out the accuracy of the proposed methodology. Copyright © 2013 Elsevier B.V. All rights reserved.

Microbial analysis and survey test of gamma-irradiated freeze-dried fruits for patient's food

NASA Astrophysics Data System (ADS)

Park, Jae-Nam; Sung, Nak-Yun; Byun, Eui-Hong; Byun, Eui-Baek; Song, Beom-Seok; Kim, Jae-Hun; Lee, Kyung-A.; Son, Eun-Joo; Lyu, Eun-Soon

2015-06-01

This study examined the microbiological and organoleptic qualities of gamma-irradiated freeze-dried apples, pears, strawberries, pineapples, and grapes, and evaluated the organoleptic acceptability of the sterilized freeze-dried fruits for hospitalized patients. The freeze-dried fruits were gamma-irradiated at 0, 1, 2, 3, 4, 5, 10, 12, and 15 kGy, and their quality was evaluated. Microorganisms were not detected in apples after 1 kGy, in strawberries and pears after 4 kGy, in pineapples after 5 kGy, and in grapes after 12 kGy of gamma irradiation. The overall acceptance score, of the irradiated freeze-dried fruits on a 7-point scale at the sterilization doses was 5.5, 4.2, 4.0, 4.1, and 5.1 points for apples, strawberries, pears, pineapples, and grapes, respectively. The sensory survey of the hospitalized cancer patients (N=102) resulted in scores of 3.8, 3.7, 3.9, 3.9, and 3.7 on a 5-point scale for the gamma-irradiated freeze-dried apples, strawberries, pears, pineapples, and grapes, respectively. The results suggest that freeze-dried fruits can be sterilized with a dose of 5 kGy, except for grapes, which require a dose of 12 kGy, and that the organoleptic quality of the fruits is acceptable to immuno-compromised patients. However, to clarify the microbiological quality and safety of freeze-dried fruits should be verified by plating for both aerobic and anaerobic microorganisms.

Influence of postharvest processing and storage conditions on key antioxidants in pūhā (Sonchus oleraceus L.).

PubMed

Ou, Zong-Quan; Schmierer, David M; Strachan, Clare J; Rades, Thomas; McDowell, Arlene

2014-07-01

To investigate effects of different postharvest drying processes and storage conditions on key antioxidants in Sonchus oleraceus L. leaves. Fresh leaves were oven-dried (60°C), freeze-dried or air-dried (∼25°C) for 6 h, 24 h and 3 days, respectively. Design of experiments (DOE) was applied to study the stability of antioxidants (caftaric, chlorogenic and chicoric acids) in S. oleraceus leaves and leaf extracts stored at different temperatures (4, 25 and 50°C) and relative humidities (15%, 43% and 75%) for 180 days. The concentration of antioxidants was quantified by a HPLC-2,2'-diphenylpicrylhydrazyl post-column derivatisation method. Antioxidant activity was assessed by a cellular antioxidant activity assay. The three antioxidants degraded to unquantifiable levels after oven-drying. More than 90% of the antioxidants were retained by freeze-drying and air-drying. Both leaf and extract samples retained >90% of antioxidants, except those stored at 75% relative humidity. Leaf material had higher antioxidant concentrations and greater cellular antioxidant activity than corresponding extract samples. Freeze-drying and air-drying preserved more antioxidants in S. oleraceus than oven-drying. From DOE analysis, humidity plays an important role in degradation of antioxidants during storage. To preserve antioxidant activity, it is preferable to store S. oleraceus as dried leaf material. © 2014 Royal Pharmaceutical Society.

Determination of Total Solids and Ash in Algal Biomass: Laboratory Analytical Procedure (LAP)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Van Wychen, Stefanie; Laurens, Lieve M. L.

2016-01-13

This procedure describes the methods used to determine the amount of moisture or total solids present in a freeze-dried algal biomass sample, as well as the ash content. A traditional convection oven drying procedure is covered for total solids content, and a dry oxidation method at 575 deg. C is covered for ash content.

Moisture sorption characteristics of freeze-dried human platelets*

PubMed Central

Xu, Meng-jie; Chen, Guang-ming; Fan, Ju-li; Liu, Jin-hui; Xu, Xian-guo; Zhang, Shao-zhi

2011-01-01

Freeze-drying is a promising method for a long-term storage of human platelets. The moisture sorption characteristics of freeze-dried human platelets (FDHPs) were studied in this paper. The moisture sorption isotherms of FDHPs and freeze-dried lyophilization buffer (FDLB) were measured at 4, 25, and 37 °C. The experimental data were fitted to Brunauer-Emmett-Teller (BET) and Guggenheim-Anderson-de Boer (GAB) equations. There were no significant statistical differences (P>0.05) between the sorption characteristics of FDHPs and FDLB at 4 and 25 °C, while FDHPs absorbed more water at 37 °C. The net isosteric heat of sorption was derived. The heat for FDHPs showed an abnormal negative value at low moisture contents when 25 and 37 °C data were used. Dynamic sorption experiments were carried out at 25 °C with environmental water activity controlled at 0.75, 0.85, and 0.90. The moisture diffusion coefficient was fitted to be 8.24×10−12 m2/s when experimental data at initial time were used. These results would be helpful in choosing prehydration and storage condition for FDHPs. PMID:21370506

Suitability of microwave drying for mealworms (Tenebrio molitor) as alternative to freeze drying: Impact on nutritional quality and colour.

PubMed

Lenaerts, S; Van Der Borght, M; Callens, A; Van Campenhout, L

2018-07-15

Freeze drying represents the current practice to stabilize mealworms, even though it is an energy demanding technique. Therefore, it was examined in the present study whether microwave drying could be a proper alternative. To this end, the impact of both drying techniques on the proximate composition, vitamin B 12 content, fatty acid profile, oxidation status and colour parameters of mealworms was investigated. Furthermore, the influence of the application of vacuum during microwave drying was studied. The different drying technologies resulted in small differences in the proximate composition, while the vitamin B 12 content was only reduced by microwave drying. The fat fraction of freeze dried mealworms showed a higher oxidation status than the fat of microwave dried mealworms. Application of a vacuum during the microwave drying process did not appear to offer advantages. This research shows that for mealworms microwave drying can be a proper alternative to freeze drying. Copyright © 2018 Elsevier Ltd. All rights reserved.

Noncontact Infrared-Mediated Heat Transfer During Continuous Freeze-Drying of Unit Doses.

PubMed

Van Bockstal, Pieter-Jan; De Meyer, Laurens; Corver, Jos; Vervaet, Chris; De Beer, Thomas

2017-01-01

Recently, an innovative continuous freeze-drying concept for unit doses was proposed, based on spinning the vials during freezing. An efficient heat transfer during drying is essential to continuously process these spin frozen vials. Therefore, the applicability of noncontact infrared (IR) radiation was examined. The impact of several process and formulation variables on the mass of sublimed ice after 15 min of primary drying (i.e., sublimation rate) and the total drying time was examined. Two experimental designs were performed in which electrical power to the IR heaters, distance between the IR heaters and the spin frozen vial, chamber pressure, product layer thickness, and 5 model formulations were included as factors. A near-infrared spectroscopy method was developed to determine the end point of primary and secondary drying. The sublimation rate was mainly influenced by the electrical power to the IR heaters and the distance between the IR heaters and the vial. The layer thickness had the largest effect on total drying time. The chamber pressure and the 5 model formulations had no significant impact on sublimation rate and total drying time, respectively. This study shows that IR radiation is suitable to provide the energy during the continuous processing of spin frozen vials. Copyright © 2016 American Pharmacists Association®. Published by Elsevier Inc. All rights reserved.

The Structural Properties and Stability of Monoclonal Antibodies at Freezing Conditions

NASA Astrophysics Data System (ADS)

Perevozchikova, Tatiana; Zarraga, Isidro; Scherer, Thomas; Wagner, Norman; Liu, Yun

2013-03-01

Monoclonal Antibodies (MAb) have become a crucial therapeutic agent in a number of anti-cancer treatments. Due to the inherent unstable nature of proteins in an aqueous formulation, a freeze-drying method has been developed to maintain long-term stability of biotherapeutics. The microstructural changes in Mabs during freezing, however, remain not fully described, and it was proposed that the formed morphology of freeze drying samples could affect the final product quality after reconstitution. Furthermore, it is well known that proteins tend to aggregate during the freezing process if a careful processing procedure is not formulated. Small Angle Neutron Scattering (SANS) is a powerful tool to investigate the structural properties and interactions of Mabs during various stages of lyophilization in situ. Here we present the SANS results of freeze-thaw studies on two MAbs at several different freezing temperatures. While the chosen proteins share a significant sequence homology, their freezing properties are found to be strikingly distinctive. We also show the effect of excipients, concentration and quenching speed on the final morphology of the frozen samples. These findings provide critical information for more effective lyophilization schemes for therapeutic proteins, as well as increase our understanding on structural properties of proteins under cryogenic conditions.

Rapid formation of phase-clean 110 K (Bi-2223) powders derived via freeze-drying process

DOEpatents

Balachandran, Uthamalingam

1996-01-01

A process for the preparation of amorphous precursor powders for Pb-doped Bi.sub.2 Sr.sub.2 Ca.sub.2 Cu.sub.3 O.sub.x (2223) includes a freeze-drying process incorporating a splat-freezing step. The process generally includes splat freezing a nitrate solution of Bi, Pb, Sr, Ca, and Cu to form flakes of the solution without any phase separation; grinding the frozen flakes to form a powder; freeze-drying the frozen powder; heating the dried powder to form a dry green precursor powders; denitrating the green-powders; heating the denitrated powders to form phase-clean Bi-2223 powders. The grain boundaries of the 2223 grains appear to be clean, leading to good intergrain contact between 2223 grains.

Rapid formation of phase-clean 110 K (Bi-2223) powders derived via freeze-drying process

DOEpatents

Balachandran, U.

1996-06-04

A process for the preparation of amorphous precursor powders for Pb-doped Bi{sub 2}Sr{sub 2} Ca{sub 2}Cu{sub 3}O{sub x} (2223) includes a freeze-drying process incorporating a splat-freezing step. The process generally includes splat freezing a nitrate solution of Bi, Pb, Sr, Ca, and Cu to form flakes of the solution without any phase separation; grinding the frozen flakes to form a powder; freeze-drying the frozen powder; heating the dried powder to form a dry green precursor powders; denitrating the green-powders; heating the denitrated powders to form phase-clean Bi-2223 powders. The grain boundaries of the 2223 grains appear to be clean, leading to good intergrain contact between 2223 grains. 11 figs.

Extraction optimization and influences of drying methods on antioxidant activities of polysaccharide from cup plant (Silphium perfoliatum L.)

PubMed Central

Li, Ran; Duan, Meng-Ying; Wu, Hong-Xin

2017-01-01

Response surface methodology (RSM) was used to investigate the extraction condition of polysaccharide from cup plant (Silphium perfoliatum L.) (named CPP). Water to raw material ratio (10–30 mL/g), extraction time (40–80 min) and extraction temperature (60–100°C) were set as the 3 independent variables, and their effects on the extraction yield of CPP were measured. In addition, the effects of drying methods including hot air drying (HD), vacuum drying (VD) and freeze drying (FD) on the antioxidant activities of CPP were evaluated. The results showed that the optimal condition to extract CPP was: water to raw material ratio (15 mL/g), extraction time (61 min), and extraction temperature (97°C), a maximum CPP yield of 6.49% was obtained under this condition. CPP drying with FD method showed stronger reducing power (0.943 at 6 mg/mL) and radical scavenging capacities against DPPH radical (75.71% at 1.2 mg/mL) and ABTS radical (98.06 at 1.6 mg/mL) than CPP drying with HD and VD methods. Therefore, freeze drying served as a good method for keeping the antioxidant activities of polysaccharide from cup plant. The polysaccharide from cup plant has potential to use as a natural antioxidant. PMID:28837625

Effect of drying methods on the structure, thermo and functional properties of fenugreek (Trigonella foenum graecum) protein isolate.

PubMed

Feyzi, Samira; Varidi, Mehdi; Zare, Fatemeh; Varidi, Mohammad Javad

2018-03-01

Different drying methods due to protein denaturation could alter the functional properties of proteins, as well as their structure. So, this study focused on the effect of different drying methods on amino acid content, thermo and functional properties, and protein structure of fenugreek protein isolate. Freeze and spray drying methods resulted in comparable protein solubility, dynamic surface and interfacial tensions, foaming and emulsifying properties except for emulsion stability. Vacuum oven drying promoted emulsion stability, surface hydrophobicity and viscosity of fenugreek protein isolate at the expanse of its protein solubility. Vacuum oven process caused a higher level of Maillard reaction followed by the spray drying process, which was confirmed by the lower amount of lysine content and less lightness, also more browning intensity. ΔH of fenugreek protein isolates was higher than soy protein isolate, which confirmed the presence of more ordered structures. Also, the bands which are attributed to the α-helix structures in the FTIR spectrum were in the shorter wave number region for freeze and spray dried fenugreek protein isolates that show more possibility of such structures. This research suggests that any drying method must be conducted in its gentle state in order to sustain native structure of proteins and promote their functionalities. © 2017 Society of Chemical Industry. © 2017 Society of Chemical Industry.

Use of manometric temperature measurements (MTM) to characterize the freeze-drying behavior of amorphous protein formulations.

PubMed

Johnson, Robert E; Oldroyd, Megan E; Ahmed, Saleem S; Gieseler, Henning; Lewis, Lavinia M

2010-06-01

The freeze-drying behavior and cake morphology of a model protein in an amorphous formulation were studied at varying protein concentrations using conservative (-25 degrees C) and aggressive (+25 degrees C) shelf temperatures at constant chamber pressure during primary drying. The two cycles were characterized by manometric temperature measurements (MTM) in a SMART freeze dryer that estimates the sublimation rate (dm/dt), product temperature at the freeze-drying front (T(p-MTM)) and product resistance (R(p)) during a run. The calculated sublimation rates (dm/dt) were 3-4 times faster in the aggressive cycle compared to the conservative cycle. For conservatively dried cakes R(p) increased with both dry layer thickness and protein concentration. For aggressively dried cakes (where freeze-drying occurs at the edge of microcollapse), R(p) also increased with protein concentration but was independent of the dry layer thickness. The sublimation rate was influenced by R(p), dry layer thickness and T(p-MTM) in the conservative cycle, but was governed mainly by T(p-MTM) in the aggressive cycle, where R(p) is independent of the dry layer thickness. The aggressively dried cakes had a more open and porous structure compared to their conservatively dried counterparts. (c) 2009 Wiley-Liss, Inc. and the American Pharmacists Association

Effect of drying methods with the application of vacuum microwaves on the bioactive compounds, color, and antioxidant activity of strawberry fruits.

PubMed

Wojdyło, Aneta; Figiel, Adam; Oszmiański, Jan

2009-02-25

The objective of this study was to evaluate the application of vacuum-microwave drying (240, 360, and 480 W) in the production process of dehydrated strawberry and to compare and contrast the quality of these dehydrated strawberries in terms of their polyphenol compounds, concentration of some heat liable components, and color to that of freeze-dried, convective, and vacuum-dried strawberry. Thus, the effect of vacuum-microwave drying and other drying methods on the antioxidant activity of berries was evaluated. Whole fresh and dried fruits were assessed for phenolics (anthocyanins, flavanols, hydroxycinnamic acids, and flavonols), ascorbic acid, and antioxidant activity (all parameters were calculated on a dry matter basis). Analysis of data shows that ellagic acid and flavanol changes were affected by drying techniques and cultivar. Drying destroyed anthocyanins, flavanols, and ascorbic acid, and there was a significant decrease in antioxidant activity. The most striking result was that conventional and vacuum drying decreased antioxidant activity in both cultivars, whereas contradictory results were found for vacuum-microwave processed strawberry. This study has demonstrated that vacuum-microwave drying, especially at 240 W, can produce high-quality products, with the additional advantage of reduced processing times, compared to other processes such as freeze-drying.

The combinatorial effect of different Equex STM paste concentrations, cryoprotectants and the straw-freezing methods on the post-thaw boar semen quality.

PubMed

Wu, T-W; Cheng, F-P; Chen, I-H; Yang, C-H; Tsai, M-Y; Chang, M-H; Wang, J-H; Wu, J-T

2013-02-01

This study was to evaluate the combinatorial effect (14 treatments, A-N) of different Equex STM paste concentrations, cryoprotectants and the straw-freezing method on the post-thaw boar semen quality. Two ejaculates were collected from each of nine boars (three boars from each of three breeds). Semen was diluted in extenders with different concentrations of Equex STM paste and different cryoprotectants [glycerol or dimethylacetamide (DMA)] before cryopreserving via liquid nitrogen or dry ice. Motility, viability, percentage of spermatozoa with intense acrosomal staining and with normal morphology of post-thaw sperm were evaluated. The qualities of thawed semen were best preserved in treatment H (extender with 0.5% Equex STM paste and 5% glycerol and freezing by dry ice) and were worst in treatment B (extender with 0% Equex STM paste and 5% DMA and freezing by dry ice). Significant difference (p < 0.05) was present in post-thawed sperm motility (63% vs 27%), sperm viability (70% vs 33%) and sperm acrosomal integrity rate (68% vs 29%) between treatments H and B. However, sperm proportion with normal morphology showed no significant difference among treatments (66% vs 66%; p > 0.05). Moreover, statistical analysis suggests that no significant difference was present in semen quality among breed or individual donors (p > 0.05). These findings suggest that Equex STM paste improved the cryosurvival efficiency of boar sperm, and the favourable straw-freezing method changes between glycerol and DMA. © 2012 Blackwell Verlag GmbH.

Freeze-Drying as Sample Preparation for Micellar Electrokinetic Capillary Chromatography – Electrochemical Separations of Neurochemicals in Drosophila Brains

PubMed Central

Berglund, E. Carina; Kuklinski, Nicholas J.; Karagündüz, Ekin; Ucar, Kubra; Hanrieder, Jörg; Ewing, Andrew G.

2013-01-01

Micellar electrokinetic capillary chromatography with electrochemical detection has been used to quantify biogenic amines in freeze-dried Drosophila melanogaster brains. Freeze drying samples offers a way to preserve the biological sample while making dissection of these tiny samples easier and faster. Fly samples were extracted in cold acetone and dried in a rotary evaporator. Extraction and drying times were optimized in order to avoid contamination by red-pigment from the fly eyes and still have intact brain structures. Single freeze-dried fly-brain samples were found to produce representative electropherograms as a single hand-dissected brain sample. Utilizing the faster dissection time that freeze drying affords, the number of brains in a fixed homogenate volume can be increased to concentrate the sample. Thus, concentrated brain samples containing five or fifteen preserved brains were analyzed for their neurotransmitter content, and five analytes; dopamine N-acetyloctopamine, Nacetylserotonin, N-acetyltyramine, N-acetyldopamine were found to correspond well with previously reported values. PMID:23387977

Rehydration of freeze-dried and convective dried boletus edulis mushrooms: effect on some quality parameters.

PubMed

Hernando, I; Sanjuán, N; Pérez-Munuera, I; Mulet, A

2008-10-01

Quality of rehydrated products is a key aspect linked to rehydration conditions. To assess the effect of rehydration temperature on some quality parameters, experiments at 20 and 70 degrees C were performed with convective dried and freeze-dried Boletus edulis mushrooms. Rehydration characteristics (through Peleg's parameter, k(1), and equilibrium moisture, W(e)), texture (Kramer), and microstructure (Cryo-Scanning Electron Microscopy) were evaluated. Freeze-dried samples absorbed water more quickly and attained higher W(e) values than convective dried ones. Convective dehydrated samples rehydrated at 20 degrees C showed significantly lower textural values (11.9 +/- 3.3 N/g) than those rehydrated at 70 degrees C (15.7 +/- 1.2 N/g). For the freeze-dried Boletus edulis, the textural values also exhibited significant differences, being 8.2 +/- 1.3 and 10.5 +/- 2.3 N/g for 20 and 70 degrees C, respectively. Freeze-dried samples showed a porous structure that allows rehydration to take place mainly at the extracellular level. This explains the fact that, regardless of temperature, freeze-dried mushrooms absorbed water more quickly and reached higher W(e) values than convective dried ones. Whatever the dehydration technique used, rehydration at 70 degrees C produced a structural damage that hindered water absorption; consequently lower W(e) values and higher textural values were attained than when rehydrating at 20 degrees C.

Gravimetric measurement of momentary drying rate of spray freeze-dried powders in vials.

PubMed

Gieseler, Henning; Lee, Geoffrey

2009-09-01

The profile of drying rate versus primary drying time for a spray freeze-dried trehalose aqueous solution is much different from that determined for regular freeze-drying. Drying rate declines very rapidly, attributed to rate-limiting heat transfer through the packed bed of frozen microparticles contained in a vial. The inter-particulate spaces appear to be the cause of this rate limitation. Use of either liquid nitrogen or liquid propane as a cryogenic produced strong differences in both SFD particle morphology and drying rate using trehalose, sucrose, or mannitol. The lack of any evident correlation supports the argument that the inter-particulate voids determine drying behavior.

Role of mono- and oligosaccharides from FOS as stabilizing agents during freeze-drying and storage of Lactobacillus delbrueckii subsp. bulgaricus.

PubMed

Romano, Nelson; Schebor, Carolina; Mobili, Pablo; Gómez-Zavaglia, Andrea

2016-12-01

The aim of this work was to assess the role of mono- and oligosaccharides present in fructo-oligosaccharides (FOS) mixtures as protective agents during freeze-drying and storage of Lactobacillus delbrueckii subsp. bulgaricus CIDCA 333. Different FOS mixtures were enzymatically obtained from sucrose and further purified by removing the monosaccharides produced as secondary products. Their glass transition temperatures (T g ) were determined at 11, 22 and 33% relative humidity (RH). Bacterial cultures were freeze-dried in the presence of 20% w/v solutions of the studied FOS. Their protective effect during freeze-drying was assessed by bacterial plate counting, and by determining the lag time from growth kinetics and the uptake of propidium iodide (PI). Plate counting during bacterial storage at 4°C, and 11, 22 and 33% RH for 80days completed this rational analysis of the protective effect of FOS. Purification of FOS led to an increase of T g in all the conditions assayed. Microorganisms freeze-dried in the presence of non-purified FOS were those with the shortest lag times. Bacteria freeze-dried with pure or commercial FOS (92% of total FOS) showed larger lag times (8.9-12.6h). The cultivability of microorganisms freeze-dried with non-purified FOS and with sucrose was not significantly different from that of bacteria before freeze-drying (8.74±0.14logCFU/mL). Pure or commercial FOS were less efficient in protecting bacteria during freeze-drying. All the protectants prevented membrane damage. The cultivability of bacteria freeze-dried with FOS decayed <1logarithmicunit after 80days of storage at 11% RH. When storing at 22 and 33% RH, pure and commercial FOS were those that best protected bacteria, and FOS containing monosaccharides were less efficient. The effect of FOS on bacterial protection is the result of a balance between monosaccharides, sucrose and larger FOS in the mixtures: the smallest sugars are more efficient in protecting lipid membranes, and the larger ones favor the formation of vitreous states. Copyright © 2016 Elsevier Ltd. All rights reserved.

Antioxidant Potential of the Giant Mushroom, Macrocybe gigantea (Agaricomycetes), from India in Different Drying Methods.

PubMed

Gaur, Tanvi; Rao, P B

2016-01-01

Free radicals are responsible for several diseases like cancer, atherosclerosis, gastric ulcers, and several others. Studies have shown that mushrooms possess antioxidant activity and Macrocybe gigantea was recently added to the list of mushrooms under cultivation in India. The methanolic extracts were prepared from lyophilized and oven-dried samples of MA1 and MA2 strains of M. gigantea and their antioxidant properties were studied. MA2 showed comparatively higher total antioxidant activity (111.88 µg/mg) than MA1 (97.00 µg/mg). The scavenging activity on 2,2'-diphenyl picryl hydrazyl free radical (74.41%), ferrous chelating (83.74%), reducing power (0.371), and superoxide anion radical (72.05%) was significantly higher in freeze-dried MA2 than MA1 at 200 µg/mL. Correspondingly, the EC50 values were lower in freeze-dried states (96.03 µg/mL, 95.00 µg/mL, and 68.12 µg/mL in MA2 and 105.12 µg/mL, 109.8 µg/mL, and 74.60 µg/mL in MA1) than in oven-dried states (97.97 µg/mL, 120.2 µg/mL, and 125.33 µg/mL in MA2 and 108.3 µg/mL, 131.2 µg/mL, and 147.5 µg/mL in MA1, respectively). In addition, total phenolic, total flavonoid, and ortho-dihydroxy phenol content was examined and their values were comparatively higher in freeze-dried MA2 (18.00 mg/g of gallic acid equivalents, 1.67 mg/g of quercetin equivalents, and 1.10 mg/g of catechol equivalents, respectively) than in MA1 and oven-dried states in both strains. Further, MA2 showed lower EC50 values in freeze-dried samples than MA1 and oven-dried states in both strains. These results suggested that MA2 contains higher antioxidant potential than MA1 and freeze-drying by lyophilization retains higher antioxidants than heat drying by a hot air oven in both the strains; thus, they can be a good source of nutraceuticals.

Freeze-drying of nanosuspensions, 1: freezing rate versus formulation design as critical factors to preserve the original particle size distribution.

PubMed

Beirowski, Jakob; Inghelbrecht, Sabine; Arien, Albertina; Gieseler, Henning

2011-05-01

It has been recently reported in the literature that using a fast freezing rate during freeze-drying of drug nanosuspensions is beneficial to preserve the original particle size distribution. All freezing rates studied were obtained by utilizing a custom-made apparatus and were then indirectly related to conventional vial freeze-drying. However, a standard freeze-dryer is only capable of achieving moderate freezing rates in the shelf fluid circulation system. Therefore, it was the purpose of the present study to evaluate the possibility to establish a typical freezing protocol applicable to a standard freeze-drying unit in combination with an adequate choice of cryoprotective excipients and steric stabilizers to preserve the original particle size distribution. Six different drug nanosuspensions containing itraconazole as a drug model were studied using freeze-thaw experiments and a full factorial design to reveal major factors for the stabilization of drug nanosuspensions and the corresponding interactions. In contrast to previous reports, the freezing regime showed no significant influence on preserving the original particle size distribution, suggesting that the concentrations of both the steric stabilizer and the cryoprotective agent are optimized. Moreover, it could be pinpointed that the combined effect of steric stabilizer and cryoprotectant clearly contribute to nanoparticle stability. Copyright © 2010 Wiley-Liss, Inc.

Curcuma longa L. leaves: Characterization (bioactive and antinutritional compounds) for use in human food in Brazil.

PubMed

Braga, Monick Cristina; Vieira, Ellen Caroline Silvério; de Oliveira, Tatianne Ferreira

2018-11-01

This study evaluated the physicochemical characterization of Curcuma longa L. leaves with respect to proximate composition, mineral content, the presence of antinutritional factors, content of bioactive compounds and antioxidant capacity, and color measurements of leaves in natura and leaves subjected to microwave drying, oven drying, and freeze-drying methods. The proximate composition showed appreciable levels of protein (39.5 g.100 g -1 ), carbohydrates (44.74 g.100 g -1 ), total fiber (34.47 g.100 g -1 ), soluble fiber (22.65 g.100 g -1 ), insoluble fiber (11.81 g.100 g -1 ), ash (13.81 g.100 g -1 ), and low lipid contents (2.47 g.100 g -1 ). No cyanogenic compounds were detected in both samples. Freeze-drying stood out as the method that led to the greatest reductions of the bioactive compounds (33.12-73.86%, dry basis) and antioxidant capacity when compared to the leaves in natura. Microwave drying was the preservation method that produced dry leaves with higher content of bioactive compounds and antioxidant capacity. Therefore, microwave drying produced dehydrated Curcuma longa L. leaves with the highest bioactive compounds and antioxidant activity. Copyright © 2018 Elsevier Ltd. All rights reserved.

Production and Characterization of Nanosilica from Bagasse Through Biosynthesis Using Lactobacilus bulgaricus.

PubMed

Rahmawati, Nanda Yuli; Harisna, Azza Hanief; Khoirunnisa, Wulida; Yasvinawati, Niarisandi; Sumitro, Sutiman Bambang

2016-06-01

Bagasse has a potential as natural resource of nanosilica. Nanosilica biosynthetic production method is better than chemical or physical methods. The aim of this study is to determine the potential of Lactobacillus bulgaricus in nanosilica synthesis, the effect of the long incubation, and the effect of freeze drying to the nanosilica quality. The method consists of two steps. The first is performing biosynthesize using bagasse and Lactobacillus bulgaricus in dark place with temperature of 37 degress C for the period of 24 hours, 48 hours, and 72 hours. The second is analyzing particles and chemical of nanosilica characterization using Fourier Transformer Infrared Spectroscopy (FTIR), Particle Size Analyzer (PSA), X-ray Diffraction (XRD), some microscopes namely stereo, fluorescence, polarizing, Scanning Electron Microscope (SEM) and Energy Dispersive X-ray (EDX). The results show that nanosilica has spherical shaped, amorphous, and able to fluoresce when exposed by UV. The average size of particles are 104.6 nm in the 24 hours length incubated, 67.3 nm in the 48 hours length incubation, and 30.5 nm in the 72 hours length incubation. Samples using freeze drying have more complex and smaller structure than samples using air drying. The lengths of incubation influence the size and shape of nanosilica. Samples using freeze drying enable change the soil structure, and has beneficiary effect to improve soil fertility, as nanofertilizer. Whereas, the samples using air drying may use for glass or biofilm materials.

Amorphous or Crystalline? A Comparison of Particle Engineering Methods and Selection.

PubMed

Thakkar, Sachin G; Fathe, Kristin; Smyth, Hugh D C

2015-01-01

This review is intended to provide a critical account of the current goals and technologies of particle engineering regarding the production of crystalline and amorphous particles. The technologies discussed here cover traditional crystallization technologies, supercritical fluid technologies, spray drying, controlled solvent crystallization, and sonocrystallization. Also recent advancements in particle engineering including spray freezing into liquid, thin-film freeze-drying, PRINT technology are presented. The paper also examines the merits and limitations of these technologies with respect to their methods of characterization. Additionally a section discussing the utility of creating amorphous and crystalline formulation approaches in regards to bioavailability and utility in formulation is presented.

A comparison study on the behavior of human endometrial stem cell-derived osteoblast cells on PLGA/HA nanocomposite scaffolds fabricated by electrospinning and freeze-drying methods.

PubMed

Namini, Mojdeh Salehi; Bayat, Neda; Tajerian, Roxana; Ebrahimi-Barough, Somayeh; Azami, Mahmoud; Irani, Shiva; Jangjoo, Saranaz; Shirian, Sadegh; Ai, Jafar

2018-03-27

An engineered tissue structure is an artificial scaffold combined with cells and signaling factors. Among various polymers, the polylactide-co-glycolide/hydroxyapatite (PLGA/HA) has attracted much attention due to their optimal properties. The aim of this study was to study the behavior of human endometrial stem cell (hEnSC)-derived osteoblast cells cultured on PLGA/HA nanocomposite scaffolds. hEnSCs were isolated and exposed to osteogenic media for 21 days. Differentiated cells were cultured on PLGA/HA synthetic scaffolds. The PLGA/HA-based nanocomposite scaffolds were fabricated using either electrospinning or freeze-drying methods. Behavior of the cells was evaluated a week after seeding hEnSC-derived osteoblast-like cells on these scaffolds. Osteogenesis was investigated in terms of alkaline phosphatase activity, gene expression, immunocytochemistry (ICC), proliferation, and scanning electron microscopy (SEM). Moreover, scaffold properties, such as pore size and morphology of the cells, onto the scaffolds were evaluated using SEM. Furthermore, biocompatibility of these scaffolds was confirmed by 3-(4,5-dimethylthiazoyl-2-yl)-2,5-diphenyltetrazolium bromide (MTT) assay. The matrix mineralization was proved by alizarin red staining, and the osteogenic media-treated cultures positively expressed osteocalcin and osteopontin markers. Moreover, qRT-PCR results confirmed the positive gene expression of osteopontin and osteonectin in the differentiated osteoblast-like cells. The results of behavior assessment of the cultured cells on electrospinning and freeze-dried scaffolds showed that the behavior of the cultured cells on the freeze-dried PLGA/HA scaffolds was significantly better than the electrospinning PLGA/HA scaffolds. It has been shown that the freeze-dried PLGA/HA nanocomposite scaffolds can appropriately support the attachment and proliferation of the differentiated osteoblast cells and are a suitable candidate for bone tissue engineering.

Infrared Thermography for Monitoring of Freeze-Drying Processes: Instrumental Developments and Preliminary Results

PubMed Central

Emteborg, Håkan; Zeleny, Reinhard; Charoud-Got, Jean; Martos, Gustavo; Lüddeke, Jörg; Schellin, Holger; Teipel, Katharina

2014-01-01

Coupling an infrared (IR) camera to a freeze dryer for on-line monitoring of freeze-drying cycles is described for the first time. Normally, product temperature is measured using a few invasive Pt-100 probes, resulting in poor spatial resolution. To overcome this, an IR camera was placed on a process-scale freeze dryer. Imaging took place every 120 s through a Germanium window comprising 30,000 measurement points obtained contact-free from −40°C to 25°C. Results are presented for an empty system, bulk drying of cheese slurry, and drying of 1 mL human serum in 150 vials. During freezing of the empty system, differences of more than 5°C were measured on the shelf. Adding a tray to the empty system, a difference of more than 8°C was observed. These temperature differences probably cause different ice structures affecting the drying speed during sublimation. A temperature difference of maximum 13°C was observed in bulk mode during sublimation. When drying in vials, differences of more than 10°C were observed. Gradually, the large temperature differences disappeared during secondary drying and products were transformed into uniformly dry cakes. The experimental data show that the IR camera is a highly versatile on-line monitoring tool for different kinds of freeze-drying processes. © 2014 European Union 103:2088–2097, 2014 PMID:24902839

Infrared thermography for monitoring of freeze-drying processes: instrumental developments and preliminary results.

PubMed

Emteborg, Håkan; Zeleny, Reinhard; Charoud-Got, Jean; Martos, Gustavo; Lüddeke, Jörg; Schellin, Holger; Teipel, Katharina

2014-07-01

Coupling an infrared (IR) camera to a freeze dryer for on-line monitoring of freeze-drying cycles is described for the first time. Normally, product temperature is measured using a few invasive Pt-100 probes, resulting in poor spatial resolution. To overcome this, an IR camera was placed on a process-scale freeze dryer. Imaging took place every 120 s through a Germanium window comprising 30,000 measurement points obtained contact-free from -40 °C to 25 °C. Results are presented for an empty system, bulk drying of cheese slurry, and drying of 1 mL human serum in 150 vials. During freezing of the empty system, differences of more than 5 °C were measured on the shelf. Adding a tray to the empty system, a difference of more than 8 °C was observed. These temperature differences probably cause different ice structures affecting the drying speed during sublimation. A temperature difference of maximum 13 °C was observed in bulk mode during sublimation. When drying in vials, differences of more than 10 °C were observed. Gradually, the large temperature differences disappeared during secondary drying and products were transformed into uniformly dry cakes. The experimental data show that the IR camera is a highly versatile on-line monitoring tool for different kinds of freeze-drying processes. © 2014 European Union.

Evaluation of Drying Process on the Composition of Black Pepper Ethanolic Extract by High Performance Liquid Chromatography With Diode Array Detector

PubMed Central

Namjoyan, Foroogh; Hejazi, Hoda; Ramezani, Zahra

2012-01-01

Background Black pepper (Piper nigrum) is one of the well-known spices extensively used worldwide especially in India, and Southeast Asia. The presence of alkaloids in the pepper, namely, piperine and its three stereoisomers, isopiperine, chavicine and isochavicine are well noticed. Objectives The current study evaluated the effect of lyophilization and oven drying on the stability and decomposition of constituents of black pepper ethanolic extract. Materials and Methods In the current study ethanolic extract of black pepper obtained by maceration method was dried using two methods. The effect of freeze and oven drying on the chemical composition of the extract especially piperine and its three isomers were evaluated by HPLC analysis of the ethanolic extract before and after drying processes using diode array detector. The UV Vis spectra of the peaks at piperine retention time before and after each drying methods indicated maximum absorbance at 341.2 nm corresponding to standard piperine. Results The results indicated a decrease in intensity of the chromatogram peaks at approximately all retention times after freeze drying, indicating a few percent loss of piperine and its isomers upon lyophilization. Two impurity peaks were completely removed from the extract. Conclusions In oven dried samples two of the piperine stereoisomers were completely removed from the extract and the intensity of piperine peak was increased. PMID:24624176

Uptake of erythromycin by first-feeding sockeye salmon, Oncorhynchus nerka (Walbaum), fed live or freeze-dried enriched adult Artemia or medicated pellets.

PubMed

Cook, M A; Rust, M B; Massee, K; Majack, T; Peterson, M E

2003-05-01

The potential to use adult Artemia to deliver erythromycin to first-feeding sockeye salmon, Oncorhynchus nerka (Walbaum), was investigated in three trials. In the first trial, first-feeding sockeye were fed live erythromycin enriched adult Artemia or pellets containing equal amounts of erythromycin for 35 days. At the end of the trial, tissue erythromycin concentration of the fish fed the live Artemia was significantly greater (P < 0.05, 25.52 +/- 1.29 microg mL(-1); mean +/- SEM), than the tissue concentration of the fish fed the pellets (0.72 +/- 0.01 microg mL(-1)). In the second trial, first-feeding sockeye were fed either live or freeze-dried bioencapsulated erythromycin (adult Artemia) or pellets containing erythromycin daily for 21 days. Mean daily erythromycin concentration in fish fed the freeze-dried Artemia, live Artemia, or pellets did not differ significantly. In the third trial, apparent erythromycin digestibility was determined. Significantly more (P < 0.05) erythromycin was retained by juvenile sockeye fed freeze-dried bioencapsulated erythromycin (98.3 +/- 1.0%) compared with medicated pellets (89.2 +/- 1.7%). Uptake of bioencapsulated erythromycin from adult Artemia (live or freeze-dried) appears to be greater than uptake from pellets. Freeze-dried and live Artemia were equally effective at delivery suggesting enriched freeze-dried adult Artemia could be produced into a highly palatable, consistent, off-the-shelf product.

Optimization of a protective medium for freeze-dried Pichia membranifaciens and application of this biocontrol agent on citrus fruit.

PubMed

Niu, X; Deng, L; Zhou, Y; Wang, W; Yao, S; Zeng, K

2016-07-01

To optimize a protective medium for freeze-dried Pichia membranifaciens and to evaluate biocontrol efficacies of agents against blue and green mould and anthracnose in citrus fruit. Based on the screening assays of saccharides and antioxidants, response surface methodology was used to optimize sucrose, sodium glutamate and skim milk to improve viability of freeze-dried Pi. membranifaciens. Biocontrol assays were conducted between fresh and freeze-dried Pi. membranifaciens against Penicillium italicum, Penicillium digitatum and Colletotrichum gloeosporioides in citrus fruit. Solving the regression equation indicated that the optimal protective medium was 6·06% (w/v) sucrose combined with 3·40% (w/v) sodium glutamate and 5·43% (w/v) skim milk. Pi. membranifaciens freeze-dried in the optimal protective medium showed 76·80% viability, and retained biocontrol efficacy against Pe. italicum, Pe. digitatum and Co. gloeosporioides in citrus fruit. The optimal protective medium showed more effective protective properties than each of the three protectants used alone. The viability of freeze-dried Pi. membranifaciens finally reached 76·80%. Meanwhile, the biocontrol efficacies showed no significant difference between fresh and freeze-dried yeast against Pe. italicum, Pe. digitatum and Co. gloeosporioides in citrus fruit. The results showed the potential value of Pi. membranifaciens CICC 32259 for commercialization. © 2016 The Society for Applied Microbiology.

Continuous measurement of drying rate of crystalline and amorphous systems during freeze-drying using an in situ microbalance technique.

PubMed

Roth, C; Winter, G; Lee, G

2001-09-01

The use of a novel microbalance (Christ) technique to monitor continuously the weight loss of a vial standing on a shelf of a freeze-dryer has been investigated. The drying rates of the following aqueous solutions were measured during the primary drying phase of a complete freeze-drying cycle: sucrose (75 mg/mL, 2.5-mL fill volume), sucrose and phenylalanine (1:0.2 by weight, 75 mg/mL, 2.5-mL fill volume), and mannitol (75mg/mL, 2.5-mL fill volume). The microbalance yields the cumulative water loss, m(cu) in grams, and the momentary drying rate, Deltam(cu)/Deltat in mg/10 min, of the frozen cake. The momentary drying rate curves were especially useful for examining how Deltam(cu)/Deltat changes with time during primary drying. Initially, Deltam(cu)/Deltat rises to a sharp maximum and then decreases in a fashion depending on shelf temperature, chamber pressure, and the nature of the substance being dried. Different drying behavior was observed for the sucrose and sucrose/phenylalanine systems, which was attributed to the presence of crystalline phenylalanine in the amorphous sucrose. At low shelf-temperature (-24 degrees C) the crystalline mannitol showed lower Deltam(cu)/Deltat than with either sucrose or sucrose/phenylalanine. The balance could also detect differences in Deltam(cu)/Deltat when using different freezing protocols. "Slow" and "moderate" freezing protocols gave similar drying behavior, but "rapid" freezing in liquid nitrogen produced greatly altered drying rate and internal cake morphology. The balance also could be used to detect the endpoint of primary drying. Different endpoint criteria and their influence on final dried cake properties were examined. Copyright 2001 Wiley-Liss, Inc. and the American Pharmaceutical Association

Freeze-Dried Carbon Nanotube Aerogels for High-Frequency Absorber Applications.

PubMed

Anoshkin, Ilya V; Campion, James; Lioubtchenko, Dmitri V; Oberhammer, Joachim

2018-06-13

A novel technique for millimeter wave absorber material embedded in a metal waveguide is proposed. The absorber material is a highly porous carbon nanotube (CNT) aerogel prepared by a freeze-drying technique. CNT aerogel structures are shown to be good absorbers with a low reflection coefficient, less than -12 dB at 95 GHz. The reflection coefficient of the novel absorber is 3-4 times lower than that of commercial absorbers with identical geometry. Samples prepared by freeze-drying at -25 °C demonstrate resonance behavior, while those prepared at liquid nitrogen temperature (-196 °C) exhibit a significant decrease in reflection coefficient, with no resonant behavior. CNT absorbers of identical volume based on wet-phase drying preparation show significantly worse performance than the CNT aerogel absorbers prepared by freeze-drying. Treatment of the freeze-dried CNT aerogel with n- and p-dopants (monoethanolamine and iodine vapors, respectively) shows remarkable improvement in the performance of the waveguide embedded absorbers, reducing the reflection coefficient by 2 dB across the band.

Shrinkage of spray-freeze-dried microparticles of pure protein for ballistic injection by manipulation of freeze-drying cycle.

PubMed

Straller, Georg; Lee, Geoffrey

2017-10-30

Spray-freeze-drying was used to produce shrivelled, partially-collapsed microparticles of pure proteins that may be suitable for use in a ballistic injector. Various modifications of the freeze drying cycle were examined for their effects on collapse of the pure protein microparticles. The use of annealing at a shelf temperature of up to +10°C resulted in no visible particle shrinkage. This was because of the high T g ' of the pure protein. Inclusion of trehalose or sucrose led to particle shrinkage because of the plasticizing effects of the disaccharides on the protein. Only by extending the duration of primary drying from 240 to 2745min at shelf temperatures in the range -12 to -8°C were shrivelled, wrinkled particles of bSA and bCA of reduced porosity obtained. Manipulation of the freeze-drying cycle used for SFD can therefore be used to modify particle morphology and increase particle density. Copyright © 2017 Elsevier B.V. All rights reserved.

Freeze-drying of silica nanoparticles: redispersibility toward nanomedicine applications.

PubMed

Picco, Agustin S; Ferreira, Larissa F; Liberato, Michelle S; Mondo, Gabriela B; Cardoso, Mateus B

2018-01-01

To study freeze-drying of silica nanoparticles (SiO 2 NPs) in order to find suitable conditions to produce lyophilized powders with no aggregation after resuspension and storage. SiO 2 NPs were synthesized using a Stöber-based procedure, and characterized by scanning electron microscopy, dynamic light scattering and nitrogen adsorption/desorption isotherms. SiO 2 NPs hydrodynamic diameters were compared prior and after freeze-drying in the presence/absence of carbohydrate protectants. Glucose was found to be the most suitable protectant against the detrimental effects of lyophilization. The minimum concentration of carbohydrate required to effectively protect SiO 2 NPs from aggregation during freeze-drying is influenced by the nanoparticle's size and texture. Negligible aggregation was observed during storage. Carbohydrates can be used during SiO 2 NPs freeze-drying process to obtain redispersable solids that maintain original sizes without residual aggregation.

Kit for the rapid preparation of .sup.99m Tc red blood cells

DOEpatents

Richards, Powell; Smith, Terry D.

1976-01-01

A method and sample kit for the preparation of .sup.99m Tc-labeled red blood cells in a closed, sterile system. A partially evacuated tube, containing a freeze-dried stannous citrate formulation with heparin as an anticoagulant, allows whole blood to be automatically drawn from the patient. The radioisotope is added at the end of the labeling sequence to minimize operator exposure. Consistent 97% yields in 20 minutes are obtained with small blood samples. Freeze-dried kits have remained stable after five months.

Retention of antioxidant capacity of vacuum microwave dried cranberry.

PubMed

Leusink, Gwen J; Kitts, David D; Yaghmaee, Parastoo; Durance, Tim

2010-04-01

In this study, cranberries were dried by vacuum-microwave drying (VMD), freeze-drying (FD), or hot air-drying (AD), to compare the effects of different drying processes on both physical changes as well as the retention of bioactive components in dried samples. Total porosity (%) and average pore radius of dehydrated cranberries were greater using VMD compared to FD and AD (P < 0.05). Crude methanol cranberry powdered extracts were fractionated by solid phase extraction (SPE) into organic acid-, total phenolics-, anthocyanin-, or proanthocyanidin-enriched extracts, respectively. The chemical composition of the 60% acidified methanol fractions contained cyanidin-3-galactoside, cyanidin-3-arabinoside, peonidin-3-galactoside, and peonidin-3-arabinoside, as assessed by HPLC. Antioxidant activities of cranberry fractions were measured using chemical ORAC and ABTS methods. The 60% acidified methanol fraction had a significantly higher (P < 0.05) antioxidant potential than the other chemical fractions, which was largely attributed to the relatively higher anthocyanin content. In general, vacuum-microwave drying and freeze-drying resulted in similar retention of anthocyanins and antioxidant activity, which were both relatively higher (P < 0.05) than that recovered from cranberries dried by hot air drying.

Heat and mass transfer scale-up issues during freeze-drying, III: control and characterization of dryer differences via operational qualification tests.

PubMed

Rambhatla, S; Tchessalov, S; Pikal, Michael J

2006-04-21

The objective of this research was to estimate differences in heat and mass transfer between freeze dryers due to inherent design characteristics using data obtained from sublimation tests. This study also aimed to provide guidelines for convenient scale-up of the freeze-drying process. Data obtained from sublimation tests performed on laboratory-scale, pilot, and production freeze dryers were used to evaluate various heat and mass transfer parameters: nonuniformity in shelf surface temperatures, resistance of pipe, refrigeration system, and condenser. Emissivity measurements of relevant surfaces such as the chamber wall and the freeze dryer door were taken to evaluate the impact of atypical radiation heat transfer during scale-up. "Hot" and "cold" spots were identified on the shelf surface of different freeze dryers, and the impact of variation in shelf surface temperatures on the primary drying time and the product temperature during primary drying was studied. Calculations performed using emissivity measurements on different freeze dryers suggest that a front vial in the laboratory lyophilizer received 1.8 times more heat than a front vial in a manufacturing freeze dryer operating at a shelf temperature of -25 degrees C and a chamber pressure of 150 mTorr during primary drying. Therefore, front vials in the laboratory are much more atypical than front vials in manufacturing. Steady-state heat and mass transfer equations were used to study a combination of different scale-up issues pertinent during lyophilization cycles commonly used for the freeze-drying of pharmaceuticals.

Influence of the preparation method on the physicochemical properties of indomethacin and methyl-β-cyclodextrin complexes.

PubMed

Rudrangi, Shashi Ravi Suman; Bhomia, Ruchir; Trivedi, Vivek; Vine, George J; Mitchell, John C; Alexander, Bruce David; Wicks, Stephen Richard

2015-02-20

The main objective of this study was to investigate different manufacturing processes claimed to promote inclusion complexation between indomethacin and cyclodextrins in order to enhance the apparent solubility and dissolution properties of indomethacin. Especially, the effectiveness of supercritical carbon dioxide processing for preparing solid drug-cyclodextrin inclusion complexes was investigated and compared to other preparation methods. The complexes were prepared by physical mixing, co-evaporation, freeze drying from aqueous solution, spray drying and supercritical carbon dioxide processing methods. The prepared complexes were then evaluated by scanning electron microscopy, differential scanning calorimetry, X-ray powder diffraction, solubility and dissolution studies. The method of preparation of the inclusion complexes was shown to influence the physicochemical properties of the formed complexes. Indomethacin exists in a highly crystalline solid form. Physical mixing of indomethacin and methyl-β-cyclodextrin appeared not to reduce the degree of crystallinity of the drug. The co-evaporated and freeze dried complexes had a lower degree of crystallinity than the physical mix; however the lowest degree of crystallinity was achieved in complexes prepared by spray drying and supercritical carbon dioxide processing methods. All systems based on methyl-β-cyclodextrin exhibited better dissolution properties than the drug alone. The greatest improvement in drug dissolution properties was obtained from complexes prepared using supercritical carbon dioxide processing, thereafter by spray drying, freeze drying, co-evaporation and finally by physical mixing. Supercritical carbon dioxide processing is well known as an energy efficient alternative to other pharmaceutical processes and may have application for the preparation of solid-state drug-cyclodextrin inclusion complexes. It is an effective and economic method that allows the formation of solid complexes with a high yield, without the use of organic solvents and problems associated with their residues. Copyright © 2015 Elsevier B.V. All rights reserved.

Light assisted drying (LAD) for protein stabilization: optical characterization of samples

NASA Astrophysics Data System (ADS)

Young, Madison A.; McKinnon, Madison E.; Elliott, Gloria D.; Trammell, Susan R.

2018-02-01

Light-Assisted Drying (LAD) is a novel biopreservation technique which allows proteins to be immobilized in a dry, amorphous solid at room temperature. Indicator proteins are used in a variety of diagnostic assays ranging from highthroughput 96-well plates to new microfluidic devices. A challenge in the development of protein-based assays is preserving the structure of the protein during production and storage of the assay, as the structure of the protein is responsible for its functional activity. Freeze-drying or freezing are currently the standard for the preservation of proteins, but these methods are expensive and can be challenging in some environments due to a lack of available infrastructure. An inexpensive, simple processing method that enables supra-zero temperature storage of proteins used in assays is needed. Light-assisted drying offers a relatively inexpensive method for drying samples. Proteins suspended in a trehalose solution are dehydrated using near-infrared laser light. The laser radiation speeds drying and as water is removed the sugar forms a protective matrix. The goal of this study is optically characterize samples processed with LAD. We use polarized light imaging (PLI) to look at crystallization kinetics of samples and determine optimal humidity. PLI shows a 62.5% chance of crystallization during LAD processing and negligible crystallization during low RH storage.

Evaluation of tunable diode laser absorption spectroscopy for in-process water vapor mass flux measurements during freeze drying.

PubMed

Gieseler, Henning; Kessler, William J; Finson, Michael; Davis, Steven J; Mulhall, Phillip A; Bons, Vincent; Debo, David J; Pikal, Michael J

2007-07-01

The goal of this work was to demonstrate the use of Tunable Diode Laser Absorption Spectroscopy (TDLAS) as a noninvasive method to continuously measure the water vapor concentration and the vapor flow velocity in the spool connecting a freeze-dryer chamber and condenser. The instantaneous measurements were used to determine the water vapor mass flow rate (g/s). The mass flow determinations provided a continuous measurement of the total amount of water removed. Full load runs of pure water at different pressure and shelf temperature settings and a 5% (w/w) mannitol product run were performed in both laboratory and pilot scale freeze dryers. The ratio of "gravimetric/TDLAS" measurements of water removed was 1.02 +/- 0.06. A theoretical heat transfer model was used to predict the mass flow rate and the model results were compared to both the gravimetric and TDLAS data. Good agreement was also observed in the "gravimetric/TDLAS" ratio for the 5% mannitol runs dried in both freeze dryers. The endpoints of primary and secondary drying for the product runs were clearly identified. Comparison of the velocity and mass flux profiles between the laboratory and pilot dryers indicated a higher restriction to mass flow for the lab scale freeze dryer. Copyright 2007 Wiley-Liss, Inc.

Freeze drying of orally disintegrating tablets containing taste masked naproxen sodium granules in blisters.

PubMed

Stange, Ulrike; Führling, Christian; Gieseler, Henning

2014-09-15

Abstract Orally disintegrating tablets (ODTs) were freeze dried in blisters using the Lyostar® II SMART™ Freeze Dryer Technology. ODT formulations either without non-water soluble particles (placebo) or containing large fractions (717 mg) of taste-masked naproxen sodium (NaS) granules were freeze dried. The process data revealed differences between ODTs with and without embedded granules in the pressure rise curves as well as in the shelf (inlet) temperature adjustments during freeze-drying. Pressure rise curves of the placebo ODTs from eight hours process time showed no distinct temperature-dominated part, and the last optimization step of the shelf temperature to achieve -24.4 °C might be prone to errors. The final shelf temperature of ODTs containing granules was -23.3 °C. The detection of primary drying endpoints using SMART™ Technology or comparative pressure measurements was reliable for both ODT formulations, whereas the application of thermocouples resulted in premature endpoint indication. Product resistance of ODTs containing granules was generally elevated in comparison to ODTs without granules, but increased only slightly over the course of the drying process. In summary, the developed freeze-drying cycle was found applicable for production of elegant ODTs with incorporated taste masked NaS granules.

The physico-chemical basis for the freeze-drying process.

PubMed

MacKenzie, A P

1976-10-01

To the extent that the final form and quality of a freeze-dried product depends on the way the freeze-drying is conducted, an understanding of the many factors involved is most important. The numerous effects of the design and mode of operation of the freeze-drying equipment on the course of the process need to be known, as do the properties intrinsic to the material to be freeze-dried. Much can be learned and predicted from the study of the "supplemented phase diagram", a series of experimental plots describing the equilibrium and the non-equilibrium phase behavior of the system in question. Such diagrams map and distinguish eutectic and amorphous phase behavior. Further information is available from gravimetric studies allowing the construction of "desorption isotherms", the plots describing the loss of sorbed water accompanying the sublimation of ice, frequently termed "secondary drying". These plots relate the water retained by the product to the "water activity", or relative humidity at different temperatures. Observations in the freeze-drying microscope contribute additional information, in that they reveal the actual course of the process at the microscopic level. These and other laboratory findings facilitate the analysis and comparison of pilot-plant and commercical scale processing experiences. Where scientific and engineering factors appear to interrelate, the nature and extent of the interdependence can often be determined.

Drying characteristics of pumpkin ( Cucurbita moschata) slices in convective and freeze dryer

NASA Astrophysics Data System (ADS)

Caliskan, Gulsah; Dirim, Safiye Nur

2017-06-01

This study was intended to determine the drying and rehydration kinetics of convective and freeze dried pumpkin slices (0.5 × 3.5 × 0.5 cm). A pilot scale tray drier (at 80 ± 2 °C inlet temperature, 1 m s-1 air velocity) and freeze drier (13.33 kPa absolute pressure, condenser temperature of -48 ± 2 °C) were used for the drying experiments. Drying curves were fitted to six well-known thin layer drying models. Nonlinear regression analysis was used to evaluate the parameters of the selected models by using statistical software SPSS 16.0 (SPSS Inc., USA). For the convective and freeze drying processes of pumpkin slices, the highest R2 values, and the lowest RMSE as well as χ2 values were obtained from Page model. The effective moisture diffusivity (Deff) of the convective and freeze dried pumpkin slices were obtained from the Fick's diffusion model, and they were found to be 2.233 × 10-7 and 3.040 × 10-9 m2s-1, respectively. Specific moisture extraction rate, moisture extraction rate, and specific energy consumption values were almost twice in freeze drying process. Depending on the results, moisture contents and water activity values of pumpkin slices were in acceptable limits for safe storage of products. The rehydration behaviour of [at 18 ± 2 and 100 ± 2 °C for 1:25, 1:50, 1:75, 1:100, and 1:125 solid:liquid ratios (w:w)] dried pumpkin slices was determined by Peleg's model with the highest R2. The highest total soluble solid loss of pumpkin slices was observed for the rehydration experiment which performed at 1:25 solid: liquid ratio (w:w). Rehydration ratio of freeze dried slices was found 2-3 times higher than convective dried slices.

Stability of pseudorabies virus during freeze-drying and storage: effect of suspending media.

PubMed Central

Scott, E M; Woodside, W

1976-01-01

The effect of suspending media on the stability of pseudorabies virus upon freeze-drying and subsequent storage was studied. A variety of media was tested, including: sodium glutamate; sucrose; lactose; lactalbumin hydrolysate; peptone; a combination of sucrose, dextran, and glutamate; and various combinations of sucrose, glutamate, and potassium phosphates. Suspending media containing glutamate, either alone or in combination with sucrose and either dextran or phosphates, afforded the greatest degree of protection during the freeze-drying process and upon storage. Some possible functions of these additives in preventing injury to the virus during freezing and drying have been suggested. PMID:182713

Preservation of pathological tissue specimens by freeze-drying for immunohistochemical staining and various molecular biological analyses.

PubMed

Matsuo, S; Sugiyama, T; Okuyama, T; Yoshikawa, K; Honda, K; Takahashi, R; Maeda, S

1999-05-01

Conditions of preserving DNA, RNA and protein in pathological specimens are of great importance as degradation of such macromolecules would critically affect results of molecular biological analysis. The feasibility of freeze-drying as a means of preserving pathological tissue samples for molecular analysis has previously been shown. In the present study, further tests on long-term storage conditions and analyses of freeze-dried samples by polymerase chain reaction (PCR), reverse transcriptase (RT)-PCR, western blotting and immunohistochemistry are reported. Rat chromosomal DNA of freeze-dried samples stored for 4 years showed slight degradation while RNA degradation was more prominently seen at an earlier stage of storage. However, these 4 year DNA and RNA samples were still able to serve as a template for some PCR and RT-PCR analyses, respectively. Overexpression of c-erbB-2 and p53 protein was demonstrated by western blotting and immunohistochemical staining using freeze-dried human breast cancer tissues. Although macromolecules in freeze-dried samples degrade to some extent during the preservation period, they should still be of value for certain molecular biological analyses and morphological examination; hence, providing more convenient and inexpensive ways of pathological tissue storage.

Application of a dye-binding method for the determination of available lysine in skim milk powders.

PubMed

Aalaei, Kataneh; Rayner, Marilyn; Tareke, Eden; Sjöholm, Ingegerd

2016-04-01

A dye-binding method using Acid Orange 12 was investigated regarding its suitability for the quantification of available lysine, as a means of monitoring the Maillard reaction in skim milk powders. The method was evaluated by analyzing a wide range of milk powders produced by three different drying methods and stored under various conditions. A pilot-scale freeze-dryer, spray-dryer and drum-dryer were used to produce skim milk powders and the samples were stored at two temperatures (20 °C and 30 °C) and two relative humidities (33% and 52%) under strictly controlled conditions. Moreover to validate the method, two protein isolates; bovine serum albumin and casein were investigated for their available lysine content. The results demonstrate the suitability of this method for measuring the available lysine in skim milk powders with good precision and high reproducibility. The relative standard deviations obtained from the 125 freeze-dried powders were 1.8%, and those from the 100 drum-dried samples were all 1.9%. The highest variation was found for the spray-dried powders, which showed relative standard deviations between 0.9% and 6.7%. Copyright © 2015 Elsevier Ltd. All rights reserved.

Synthesis and magnetic properties of bacterial cellulose—ferrite (MFe2O4, M  =  Mn, Co, Ni, Cu) nanocomposites prepared by co-precipitation method

NASA Astrophysics Data System (ADS)

Sriplai, Nipaporn; Mongkolthanaruk, Wiyada; Pinitsoontorn, Supree

2017-09-01

The magnetic nanocomposites based on bacterial cellulose (BC) matrix and ferrite (MFe2O4, M  =  Mn, Co, Ni and Cu) nanoparticles (NPs) were fabricated. The never-dried and freeze-dried BC nanofibrils were used as templates and a co-precipitation method was applied for NPs synthesis. The nanocomposites were either freeze-dried or annealed before subjected to characterization. The x-ray diffraction (XRD) and Fourier transform infrared (FTIR) spectroscopy showed that only MnFe2O4 and CoFe2O4 NPs could be successfully incorporated in the BC nanostructures. The results also indicated that the BC template should be freeze-dried prior to the co-precipitation process. The magnetic measurement by a vibrating sample magnetometer (VSM) showed that the strongest ferromagnetic signal was found for BC-CoFe2O4 nanocomposites. The morphological investigation by a scanning electron microscope (SEM) showed the largest volume fraction of NPs in the BC-CoFe2O4 sample which was complimentary to the magnetic property measurement. Annealing resulted in the collapse of the opened nanostructure of the BC composites. Invited talk at 5th Thailand International Nanotechnology Conference (Nano Thailand-2016), 27-29 November 2016, Nakhon Ratchasima, Thailand.

Total phenolics content, anthocyanins, and dietary fiber content of apple pomace powders produced by vacuum-belt drying.

PubMed

Yan, Huitong; Kerr, William L

2013-04-01

Apple pomace is a waste material from apple juice processing, and contains significant amounts of dietary fiber and phytochemicals. Many of these compounds may be degraded post-pressing and during drying operations. Continuous vacuum-belt drying (VBD) was studied as a means of drying and maintaining quality of apple pomace. The color and chemical properties of samples dried by vacuum-belt drying at different temperatures were evaluated including total phenolics content (TPC), monomeric anthocyanins (TMA) and dietary fiber content (TDF). VBD powders were pale golden yellow, and those dried at 80°C did not differ in L*, a* and b* values from freeze-dried powders. VBD pomace had 44.9 to 51.9 g gallic acid equivalents kg(-1) TPC, with greatest retention for pomace dried at 80 and 95°C. TPC for pomace dried at 80 or 95°C was not significantly different from that for freeze-dried pomace. TMA levels (74.0 mg C3G kg(-1), where C3G is cyanidine 3-O-glucoside equivalents) were highest in pomace vacuum dried at 80°C. TDF ranged from 442 to 495 g kg(-1) in vacuum-dried pomace and was not significantly different from TDF of freeze-dried poamce (480 g kg(-1)). In all cases, TPC, TMA and TDF were higher in VBD pomace than in freeze-dried whole apple, while VBD pomace prepared at 80 or 95°C had fiber and phytochemical levels similar to freeze-dried powders. © 2012 Society of Chemical Industry.

Impingement drying for preparing dried apple pomace flour and its fortification in bakery and meat products.

PubMed

Jung, Jooyeoun; Cavender, George; Zhao, Yanyun

2015-09-01

This study aimed to evaluate impingement drying (ID) as a rapid drying method to dry wet apple pomace (WAP) and to investigate the fortification of dried apple pomace flour (APF) or WAP in bakery and meat products. ID at ~110 °C reduced the moisture content of apple pomace from 80 % (wet basis) to 4.5 % within 3 h, compared with 24 h to 2.2 % using 40 °C forced-air drying and ~60 h to 2.3 % using freeze drying. Furthermore, ID enhanced the extractable phenolic compounds, allowing for a 58 % increase in total phenolic content (TPC) compared with wet pomace, a 110 % and 83 % higher than TPC in forced-air dried and freeze dried samples, respectively. The 15-20 % APF-fortified cookies were found to be ~44-59 % softer, ~30 % more chewy, and ~14 % moister than those of the control. WAP-fortified meat products had significantly higher dietary fiber content (0.7-1.8 % vs. 0.1-0.2 % in control) and radical scavenging activity than that of the control. These results suggest that impingement drying is a fast and effective method for preparing dried APF with highly retained bioactive compounds, and apple pomace fortified products maintained or even had improved quality.

Evaluation of a microwave method for dry matter determination in faecal samples from weaned pigs with or without clinical diarrhoea.

PubMed

Pedersen, Ken Steen; Stege, Helle; Nielsen, Jens Peter

2011-07-01

Microwave drying as a procedure for determination of faecal dry matter in weaned pigs was evaluated and clinical relevant cut-off values between faecal consistency scores were determined. Repeatability and reproducibility were evaluated. Overall coefficient of variation was 0.03. The 95% confidence limits for any future faecal subsample examined by any operator in any replica were ± 0.85% faecal dry matter. Robustness in relation to weight of wet faeces was evaluated. The weight categories were 0.5, 1.0, 1.5, 2.0 and 3.0 g. Samples of 0.5 g gave significantly different mean faecal dry matter content compared to weighing of 1.0-3.0 g. Agreement with freeze-drying was evaluated. Lin's concordance correlation coefficient was 0.94. On average the faecal dry matter values was 1.7% (SD=1.99%) higher in freeze dried compared to micro waved samples. Non-parametric ROC analyses were used to determine optimal faecal dry matter cut-off values for clinical faecal consistency scores. The 4 consistency scores were score 1=firm and shaped, score 2=soft and shaped, score 3=loose and score 4=watery. The cut-off values were score 1: faecal dry matter content >19.5%, score 2: faecal dry matter content ≤ 19.5% and >18.0%, score 3: faecal dry matter content ≤ 18.0% and >11.3%, score 4: faecal dry matter content ≤ 11.3%. In conclusion, the microwave procedure has an acceptable repeatability/reproducibility and good agreement with freeze drying can be expected. A minimum of 1.0 g of wet faeces must be used for analyses. Faecal dry matter cut-off values between 4 different clinical consistency scores were determined. © 2011 Elsevier B.V. All rights reserved.

Internal Nano Voids in Yttria-Stabilised Zirconia (YSZ) Powder

PubMed Central

Barad, Chen; Shekel, Gal; Shandalov, Michael; Hayun, Hagay; Kimmel, Giora; Shamir, Dror; Gelbstein, Yaniv

2017-01-01

Porous yttria-stabilised zirconia ceramics have been gaining popularity throughout the years in various fields, such as energy, environment, medicine, etc. Although yttria-stabilised zirconia is a well-studied material, voided yttria-stabilised zirconia powder particles have not been demonstrated yet, and might play an important role in future technology developments. A sol-gel synthesis accompanied by a freeze-drying process is currently being proposed as a method of obtaining sponge-like nano morphology of embedded faceted voids inside yttria-stabilised zirconia particles. The results rely on a freeze-drying stage as an effective and simple method for generating nano-voided yttria-stabilised zirconia particles without the use of template-assisted additives. PMID:29258227

Internal Nano Voids in Yttria-Stabilised Zirconia (YSZ) Powder.

PubMed

Barad, Chen; Shekel, Gal; Shandalov, Michael; Hayun, Hagay; Kimmel, Giora; Shamir, Dror; Gelbstein, Yaniv

2017-12-18

Porous yttria-stabilised zirconia ceramics have been gaining popularity throughout the years in various fields, such as energy, environment, medicine, etc. Although yttria-stabilised zirconia is a well-studied material, voided yttria-stabilised zirconia powder particles have not been demonstrated yet, and might play an important role in future technology developments. A sol-gel synthesis accompanied by a freeze-drying process is currently being proposed as a method of obtaining sponge-like nano morphology of embedded faceted voids inside yttria-stabilised zirconia particles. The results rely on a freeze-drying stage as an effective and simple method for generating nano-voided yttria-stabilised zirconia particles without the use of template-assisted additives.

Effects of different cryoprotectants and freezing methods on post-thaw boar semen quality.

PubMed

Yang, Chung-Hsun; Wu, Ting-Wen; Cheng, Feng-Pang; Wang, Jiann-Hsiung; Wu, Jui-Te

2016-03-01

The current study aimed to investigate the effects of different concentrations of glycerol (0%, 1%, 2%, 3%, and 5%) and dimethylacetamide (DMA: 0%, 1%, 3%, and 5%) on post-sperm quality characteristics following semen freezing in dry ice (D) or liquid nitrogen (N). Semen was collected from Duroc boars and was allocated to 32 treatment groups for cryopreservation. Analysis of post-thaw semen quality and fertility after artificial insemination (AI) was used to examine the combinatorial effects of different treatments. The best scores for post-thaw sperm motility, sperm viability, and sperm acrosomal integrity were observed in semen frozen in: (a) dry ice in the presence of 5% glycerol and no DMA (16D-treatment); (b) dry ice in the presence of 3% glycerol and no DMA (9D-treatment); and (c) liquid nitrogen in the presence of 3% glycerol and 1% DMA (10N-treatment), with no significant difference observed among these three treatments. The farrowing rates after AI with post-thawed semen after 9D- and 10N-treatments were 33% and 50%, respectively. To summarize, the results of the present study indicated that the freezing extender containing 3% glycerol in combination with the straw-freezing method using dry ice produced the best post-thaw quality parameters of boar semen. Combinations of glycerol and DMA did not enhance the cryosurvival of boar spermatozoa. Copyright © 2016 Society for Biology of Reproduction & the Institute of Animal Reproduction and Food Research of Polish Academy of Sciences in Olsztyn. Published by Elsevier Urban & Partner Sp. z o.o. All rights reserved.

Experimental and numerical investigations on freeze-drying of porous media with prebuilt porosity

NASA Astrophysics Data System (ADS)

Wang, Wei; Yang, Jing; Hu, Dapeng; Pan, Yanqiu; Wang, Shihao; Chen, Guohua

2018-05-01

Freeze-drying of initially porous frozen material was investigated aimed at improving the process economics by reducing drying time and raising productivity. Experimental results showed that freeze-drying can be significantly enhanced by the frozen material with prebuilt porosity, and about 31% of drying time can be saved compared with the conventionally solid frozen material under the tested operating conditions. A multiphase transport model was formulated based on the local mass non-equilibrium assumption. Numerical results showed excellent agreements between measured and predicted drying curves. Analyses of saturation and temperature profiles displayed that volumetric sublimation-desorption can occur for the initially porous frozen material.

Assessment of different sample preparation routes for mass spectrometric monitoring and imaging of lipids in bone cells via ToF-SIMS

PubMed Central

Schaepe, Kaija; Kokesch-Himmelreich, Julia; Rohnke, Marcus; Wagner, Alena-Svenja; Schaaf, Thimo; Wenisch, Sabine; Janek, Jürgen

2015-01-01

In ToF-SIMS analysis, the experimental outcome from cell experiments is to a great extent influenced by the sample preparation routine. In order to better judge this critical influence in the case of lipid analysis, a detailed comparison of different sample preparation routines is performed—aiming at an optimized preparation routine for systematic lipid imaging of cell cultures. For this purpose, human mesenchymal stem cells were analyzed: (a) as chemically fixed, (b) freeze-dried, and (c) frozen-hydrated. For chemical fixation, different fixatives, i.e., glutaraldehyde, paraformaldehyde, and a mixture of both, were tested with different postfixative handling procedures like storage in phosphate buffered saline, water or critical point drying. Furthermore, secondary lipid fixation via osmium tetroxide was taken into account and the effect of an ascending alcohol series with and without this secondary lipid fixation was evaluated. Concerning freeze-drying, three different postprocessing possibilities were examined. One can be considered as a pure cryofixation technique while the other two routes were based on chemical fixation. Cryofixation methods known from literature, i.e., freeze-fracturing and simple frozen-hydrated preparation, were also evaluated to complete the comparison of sample preparation techniques. Subsequent data evaluation of SIMS spectra in both, positive and negative, ion mode was performed via principal component analysis by use of peak sets representative for lipids. For freeze-fracturing, these experiments revealed poor reproducibility making this preparation route unsuitable for systematic investigations and statistic data evaluation. Freeze-drying after cryofixation showed improved reproducibility and well preserved lipid contents while the other freeze-drying procedures showed drawbacks in one of these criteria. In comparison, chemical fixation techniques via glutar- and/or paraformaldehyde proved most suitable in terms of reproducibility and preserved lipid contents, while alcohol and osmium treatment led to the extraction of lipids and are therefore not recommended. PMID:25791294

Assessment of different sample preparation routes for mass spectrometric monitoring and imaging of lipids in bone cells via ToF-SIMS.

PubMed

Schaepe, Kaija; Kokesch-Himmelreich, Julia; Rohnke, Marcus; Wagner, Alena-Svenja; Schaaf, Thimo; Wenisch, Sabine; Janek, Jürgen

2015-03-19

In ToF-SIMS analysis, the experimental outcome from cell experiments is to a great extent influenced by the sample preparation routine. In order to better judge this critical influence in the case of lipid analysis, a detailed comparison of different sample preparation routines is performed-aiming at an optimized preparation routine for systematic lipid imaging of cell cultures. For this purpose, human mesenchymal stem cells were analyzed: (a) as chemically fixed, (b) freeze-dried, and (c) frozen-hydrated. For chemical fixation, different fixatives, i.e., glutaraldehyde, paraformaldehyde, and a mixture of both, were tested with different postfixative handling procedures like storage in phosphate buffered saline, water or critical point drying. Furthermore, secondary lipid fixation via osmium tetroxide was taken into account and the effect of an ascending alcohol series with and without this secondary lipid fixation was evaluated. Concerning freeze-drying, three different postprocessing possibilities were examined. One can be considered as a pure cryofixation technique while the other two routes were based on chemical fixation. Cryofixation methods known from literature, i.e., freeze-fracturing and simple frozen-hydrated preparation, were also evaluated to complete the comparison of sample preparation techniques. Subsequent data evaluation of SIMS spectra in both, positive and negative, ion mode was performed via principal component analysis by use of peak sets representative for lipids. For freeze-fracturing, these experiments revealed poor reproducibility making this preparation route unsuitable for systematic investigations and statistic data evaluation. Freeze-drying after cryofixation showed improved reproducibility and well preserved lipid contents while the other freeze-drying procedures showed drawbacks in one of these criteria. In comparison, chemical fixation techniques via glutar- and/or paraformaldehyde proved most suitable in terms of reproducibility and preserved lipid contents, while alcohol and osmium treatment led to the extraction of lipids and are therefore not recommended.

Freeze drying optimization of polymeric nanoparticles for ocular flurbiprofen delivery: effect of protectant agents and critical process parameters on long-term stability.

PubMed

Ramos Yacasi, Gladys Rosario; Calpena Campmany, Ana Cristina; Egea Gras, María Antonia; Espina García, Marta; García López, María Luisa

2017-04-01

The stabilization of flurbiprofen loaded poly-ɛ-caprolactone nanoparticles (FB-PɛCL-NPs) for ocular delivery under accurate freeze-drying (FD) process provides the basis for a large-scale production and its commercial development. Optimization of the FD to improve long-term stability of ocular administration's FB-PɛCL-NPs. FB-PɛCL-NPs were prepared by solvent displacement method with poloxamer 188 (P188) as stabilizer. Freezing and primary drying (PD) were studied and optimized through freeze-thawing test and FD microscopy. Design of experiments was used to accurate secondary drying (SD) conditions and components concentration. Formulations were selected according to desired physicochemical properties. Furthermore, differential scanning calorimetry (DSC) and X-ray diffraction (XRD) were used to study interactions components. Optimized FB-PɛCL-NPs, stabilized with 3.5% (w/w) P188 and protected with 8% (w/w) poly(ethylene glycol), was submitted to precooling at +10 °C for 1 h, freezing at -50 °C for 4 h, PD at +5 °C and 0.140 mbar for 24 h and a SD at +45 °C during 10 h. These conditions showed 188.4 ± 1.3 nm, 0.087 ± 0.014, 85.5 ± 1.4%, 0.61 ± 0.12%, -16.4 ± 0.1 mV and 325 ± 7 mOsm/kg of average size, polydispersity index, entrapment efficiency, residual moisture, surface charge and osmolality, respectively. It performed a long-term stability >12 months. DSC and XRD spectra confirmed adequate chemical interaction between formulation components and showed a semi-crystalline state after FD. An optimal freeze dried ocular formulation was achieved. Evidently, the successful design of this promising colloidal system resulted from rational cooperation between a good formulation and the right conditions in the FD process.

Identification of the compositional changes in Orthosiphon stamineus leaves triggered by different drying techniques using 1 H NMR metabolomics.

PubMed

Pariyani, Raghunath; Ismail, Intan Safinar; Ahmad Azam, Amalina; Abas, Faridah; Shaari, Khozirah

2017-09-01

Java tea is a well-known herbal infusion prepared from the leaves of Orthosiphon stamineus (OS). The biological properties of tea are in direct correlation with the primary and secondary metabolite composition, which in turn largely depends on the choice of drying method. Herein, the impact of three commonly used drying methods, i.e. shade, microwave and freeze drying, on the metabolite composition and antioxidant activity of OS leaves was investigated using proton nuclear magnetic resonance ( 1 H NMR) spectroscopy combined with multivariate classification and regression analysis tools. A total of 31 constituents comprising primary and secondary metabolites belonging to the chemical classes of fatty acids, amino acids, sugars, terpenoids and phenolic compounds were identified. Shade-dried leaves were identified to possess the highest concentrations of bioactive secondary metabolites such as chlorogenic acid, caffeic acid, luteolin, orthosiphol and apigenin, followed by microwave-dried samples. Freeze-dried leaves had higher concentrations of choline, amino acids leucine, alanine and glutamine and sugars such as fructose and α-glucose, but contained the lowest levels of secondary metabolites. Metabolite profiling coupled with multivariate analysis identified shade drying as the best method to prepare OS leaves as Java tea or to include in traditional medicine preparation. © 2017 Society of Chemical Industry. © 2017 Society of Chemical Industry.

Comparative evaluation of two methods of enumerating enterococci in foods: collaborative study.

PubMed

Peterz, M; Steneryd, A C

1993-05-01

Two methods of enumerating enterococci in foods were compared in a collaborative study. Thirteen laboratories tested four blind duplicate samples containing different levels of enterococci and two negative control samples. Freeze-dried mixtures of bacteria were used as simulated food samples. The freeze-dried samples were reconstituted and either spread directly on the surface of Slanetz and Bartley medium (SB) and incubated at 44 degrees C for 48 h or preincubated in tryptone soya agar at 37 degrees C for 2 h before being overlaid by SB and incubated at 37 degrees C for a further 46 h. The numbers CFU of enterococci recovered by the two methods were not significantly different except for one sample where the 37 degrees C method gave a somewhat higher recovery. The 44 degrees C method was less time-consuming and less laborious.

Evaluation of manometric temperature measurement, a process analytical technology tool for freeze-drying: part I, product temperature measurement.

PubMed

Tang, Xiaolin; Nail, Steven L; Pikal, Michael J

2006-02-10

This study examines the factors that may cause systematic errors in the manometric temperature measurement (MTM) procedure used to evaluate product temperature during primary drying. MTM was conducted during primary drying using different vial loads, and the MTM product temperatures were compared with temperatures directly measured by thermocouples. To clarify the impact of freeze-drying load on MTM product temperature, simulation of the MTM vapor pressure rise was performed, and the results were compared with the experimental results. The effect of product temperature heterogeneity in MTM product temperature determination was investigated by comparing the MTM product temperatures with directly measured thermocouple product temperatures in systems differing in temperature heterogeneity. Both the simulated and experimental results showed that at least 50 vials (5 mL) were needed to give sufficiently rapid pressure rise during the MTM data collection period (25 seconds) in the freeze dryer, to allow accurate determination of the product temperature. The product temperature is location dependent, with higher temperature for vials on the edge of the array and lower temperature for the vials in the center of the array. The product temperature heterogeneity is also dependent upon the freeze-drying conditions. In product temperature heterogeneous systems, MTM measures a temperature close to the coldest product temperature, even if only a small fraction of the samples have the coldest product temperature. The MTM method is valid even at very low product temperature (-45 degrees C).

Evaluation of manometric temperature measurement, a process analytical technology tool for freeze-drying: Part I, product temperature measurement.

PubMed

Tang, Xiaolin; Nail, Steven L; Pikal, Michael J

2006-03-01

This study examines the factors that may cause systematic errors in the manometric temperature measurement (MTM) procedure used to evaluate product temperature during primary drying. MTM was conducted during primary drying using different vial loads, and the MTM product temperatures were compared with temperatures directly measured by thermocouples. To clarify the impact of freeze-drying load on MTM product temperatures, simulation of the MTM vapor pressure rise was performed, and the results were compared with the experimental results. The effect of product temperature heterogeneity in MTM product temperature determination was investigated by comparing the MTM product temperatures with directly measured thermocouple product temperatures in systems differing in temperature heterogeneity. Both the simulated and experimental results showed that at least 50 vials (5 mL) were needed to give sufficiently rapid pressure rise during the MTM data collection period (25 seconds) in the freeze dryer, to allow accurate determination of the product temperature. The product temperature is location dependent, with higher temperature for vials on the edge of the array and lower temperature for the vials in the center of the array. The product temperature heterogeneity is also dependent upon the freeze-drying conditions. In product temperature heterogeneous systems, MTM measures a temperature close to the coldest product temperature, even, if only a small fraction of the samples have the coldest product temperature. The MTM method is valid even at very low product temperature (-45°C).

Okara: A Nutritionally Valuable By-product Able to Stabilize Lactobacillus plantarum during Freeze-drying, Spray-drying, and Storage.

PubMed

Quintana, Gabriel; Gerbino, Esteban; Gómez-Zavaglia, Andrea

2017-01-01

Okara is a nutritionally valuable by-product produced in large quantities as result of soymilk elaboration. This work proposes its use as both culture and dehydration medium during freeze-drying, spray-drying, and storage of Lactobacillus plantarum CIDCA 83114. Whole and defatted okara were employed as culture media for L. plantarum CIDCA 83114. The growth kinetics were followed by plate counting and compared with those of bacteria grown in MRS broth (control). No significant differences in plate counting were observed in the three media. The fatty acid composition of bacteria grown in whole and defatted okara showed a noticeable increase in the unsaturated/saturated (U/S) fatty acid ratio, with regard to bacteria grown in MRS. This change was mainly due to the increase in polyunsaturated fatty acids, namely C18:2. For dehydration assays, cultures in the stationary phase were neutralized and freeze-dried (with or without the addition of 250 mM sucrose) or spray-dried. Bacteria were plate counted immediately after freeze-drying or spray-drying and during storage at 4°C for 90 days. Freeze-drying in whole okara conducted to the highest bacterial recovery. Regarding storage, spray-dried bacteria previously grown in whole and defatted okara showed higher plate counts than those grown in MRS. On the contrary, freeze-dried bacteria previously grown in all the three culture media were those with the lowest plate counts. The addition of sucrose to the dehydration media improved their recovery. The higher recovery of microorganisms grown in okara after freeze-drying and spray-drying processes and during storage was ascribed to both the presence of fiber and proteins in the dehydration media, and the increase in U/S fatty acids ratio in bacterial membranes. The obtained results support for the first time the use of okara as an innovative matrix to deliver L. plantarum . Considering that okara is an agro-waste obtained in large quantities, these results represent an innovative strategy to add it value, providing a symbiotic ingredient with promising industrial applications in the development of novel functional foods and feeds.

Okara: A Nutritionally Valuable By-product Able to Stabilize Lactobacillus plantarum during Freeze-drying, Spray-drying, and Storage

PubMed Central

Quintana, Gabriel; Gerbino, Esteban; Gómez-Zavaglia, Andrea

2017-01-01

Okara is a nutritionally valuable by-product produced in large quantities as result of soymilk elaboration. This work proposes its use as both culture and dehydration medium during freeze-drying, spray-drying, and storage of Lactobacillus plantarum CIDCA 83114. Whole and defatted okara were employed as culture media for L. plantarum CIDCA 83114. The growth kinetics were followed by plate counting and compared with those of bacteria grown in MRS broth (control). No significant differences in plate counting were observed in the three media. The fatty acid composition of bacteria grown in whole and defatted okara showed a noticeable increase in the unsaturated/saturated (U/S) fatty acid ratio, with regard to bacteria grown in MRS. This change was mainly due to the increase in polyunsaturated fatty acids, namely C18:2. For dehydration assays, cultures in the stationary phase were neutralized and freeze-dried (with or without the addition of 250 mM sucrose) or spray-dried. Bacteria were plate counted immediately after freeze-drying or spray-drying and during storage at 4°C for 90 days. Freeze-drying in whole okara conducted to the highest bacterial recovery. Regarding storage, spray-dried bacteria previously grown in whole and defatted okara showed higher plate counts than those grown in MRS. On the contrary, freeze-dried bacteria previously grown in all the three culture media were those with the lowest plate counts. The addition of sucrose to the dehydration media improved their recovery. The higher recovery of microorganisms grown in okara after freeze-drying and spray-drying processes and during storage was ascribed to both the presence of fiber and proteins in the dehydration media, and the increase in U/S fatty acids ratio in bacterial membranes. The obtained results support for the first time the use of okara as an innovative matrix to deliver L. plantarum. Considering that okara is an agro-waste obtained in large quantities, these results represent an innovative strategy to add it value, providing a symbiotic ingredient with promising industrial applications in the development of novel functional foods and feeds. PMID:28446905

Drying method has no substantial effect on δ(15)N or δ(13)C values of muscle tissue from teleost fishes.

PubMed

Bessey, Cindy; Vanderklift, Mathew A

2014-02-15

Stable isotope analysis (SIA) is a powerful tool in many fields of research that enables quantitative comparisons among studies, if similar methods have been used. The goal of this study was to determine if three different drying methods commonly used to prepare samples for SIA yielded different δ(15)N and δ(13)C values. Muscle subsamples from 10 individuals each of three teleost species were dried using three methods: (i) oven, (ii) food dehydrator, and (iii) freeze-dryer. All subsamples were analysed for δ(15)N and δ(13)C values, and nitrogen and carbon content, using a continuous flow system consisting of a Delta V Plus mass spectrometer and a Flush 1112 elemental analyser via a Conflo IV universal interface. The δ(13)C values were normalized to constant lipid content using the equations proposed by McConnaughey and McRoy. Although statistically significant, the differences in δ(15)N values between the drying methods were small (mean differences ≤0.21‰). The differences in δ(13)C values between the drying methods were not statistically significant, and normalising the δ(13)C values to constant lipid content reduced the mean differences for all treatments to ≤0.65‰. A statistically significant difference of ~2% in C content existed between tissues dried in a food dehydrator and those dried in a freeze-dryer for two fish species. There was no significant effect of fish size on the differences between methods. No substantial effect of drying method was found on the δ(15)N or δ(13)C values of teleost muscle tissue. Copyright © 2013 John Wiley & Sons, Ltd.

High post-thaw survival of ram sperm after partial freeze-drying.

PubMed

Arav, Amir; Idda, Antonella; Nieddu, Stefano Mario; Natan, Yehudit; Ledda, Sergio

2018-03-14

Recrystallization damages occur when a frozen sample is held at high subzero temperatures and when the warming process is too slow. In this work, ram semen diluted in two different concentrations of sugar solutions (Lyo A consisted of 0.4 M sorbitol and 0.25 M trehalose, and the second, Lyo B composed of 0.26 M sorbitol and 0.165 M trehalose) in egg yolk and Tris medium were compared after freezing 10 μL samples to: (1) - 10, - 25, and - 35 °C and thawing. (2) Freezing to - 10 and - 25 °C, holding for 1 h and then thawing, and (3) freezing to - 10 and - 25 °C and drying for 1 h at these temperatures at a vacuum of 80 mTorr, prior thawing. For drying, we used a new freeze-drying apparatus (Darya, FertileSafe, Israel) having a condensation temperature below - 110 °C and a vacuum pressure of 10-100 mTorr that is reached in less than 10s. Results showed that samples in Lyo B solution frozen at - 25 °C had significantly higher sperm motility in partially freeze-dried samples than frozen samples (46.6 ± 2.8% vs 1.2 ± 2.5%, P < 0.001). Moreover, partially dried samples in Lyo B showed higher motility than Lyo A at - 25 °C (46.6 ± 2.8% vs 35 ± 4%). Cryomicroscopy and low-temperature/low-pressure environmental scanning electronic microscope demonstrated that the amount of the ice crystals present in partially dried samples was lower than in the frozen samples. Holding the sperm at high subzero temperatures is necessary for the primary drying of cells during the freeze-drying process. Rapid freeze-drying can be achieved using this new device, which enables to reduce recrystallization damages.

Effect of Freeze-Drying on the Antioxidant Compounds and Antioxidant Activity of Selected Tropical Fruits

PubMed Central

Shofian, Norshahida Mohamad; Hamid, Azizah Abdul; Osman, Azizah; Saari, Nazamid; Anwar, Farooq; Dek, Mohd Sabri Pak; Hairuddin, Muhammad Redzuan

2011-01-01

The effects of freeze-drying on antioxidant compounds and antioxidant activity of five tropical fruits, namely starfruit (Averrhoa carambola L.), mango (Mangifera indica L.), papaya (Carica papaya L.), muskmelon (Cucumis melo L.), and watermelon Citruluss lanatus (Thunb.) were investigated. Significant (p < 0.05) differences, for the amounts of total phenolic compounds (TPC), were found between the fresh and freeze-dried fruit samples, except muskmelon. There was no significant (p > 0.05) change, however, observed in the ascorbic acid content of the fresh and freeze-dried fruits. Similarly, freeze-drying did not exert any considerable effect on β-carotene concentration of fruits, except for mango and watermelon, where significantly (p < 0.05) higher levels were detected in the fresh samples. The results of DPPH (2,2-diphenyl-1-picrylhydrazyl) radical scavenging and reducing power assays revealed that fresh samples of starfruit and mango had relatively higher antioxidant activity. In case of linoleic acid peroxidation inhibition measurement, a significant (p < 0.05) but random variation was recorded between the fresh and freeze-dried fruits. Overall, in comparison to β-carotene and ascorbic acid, a good correlation was established between the result of TPC and antioxidant assays, indicating that phenolics might have been the dominant compounds contributing towards the antioxidant activity of the fruits tested. PMID:21845104

Effect of freeze-drying on the antioxidant compounds and antioxidant activity of selected tropical fruits.

PubMed

Shofian, Norshahida Mohamad; Hamid, Azizah Abdul; Osman, Azizah; Saari, Nazamid; Anwar, Farooq; Dek, Mohd Sabri Pak; Hairuddin, Muhammad Redzuan

2011-01-01

The effects of freeze-drying on antioxidant compounds and antioxidant activity of five tropical fruits, namely starfruit (Averrhoa carambola L.), mango (Mangifera indica L.), papaya (Carica papaya L.), muskmelon (Cucumis melo L.), and watermelon Citruluss lanatus (Thunb.) were investigated. Significant (p < 0.05) differences, for the amounts of total phenolic compounds (TPC), were found between the fresh and freeze-dried fruit samples, except muskmelon. There was no significant (p > 0.05) change, however, observed in the ascorbic acid content of the fresh and freeze-dried fruits. Similarly, freeze-drying did not exert any considerable effect on β-carotene concentration of fruits, except for mango and watermelon, where significantly (p < 0.05) higher levels were detected in the fresh samples. The results of DPPH (2,2-diphenyl-1-picrylhydrazyl) radical scavenging and reducing power assays revealed that fresh samples of starfruit and mango had relatively higher antioxidant activity. In case of linoleic acid peroxidation inhibition measurement, a significant (p < 0.05) but random variation was recorded between the fresh and freeze-dried fruits. Overall, in comparison to β-carotene and ascorbic acid, a good correlation was established between the result of TPC and antioxidant assays, indicating that phenolics might have been the dominant compounds contributing towards the antioxidant activity of the fruits tested.

In-line and real-time process monitoring of a freeze drying process using Raman and NIR spectroscopy as complementary process analytical technology (PAT) tools.

PubMed

De Beer, T R M; Vercruysse, P; Burggraeve, A; Quinten, T; Ouyang, J; Zhang, X; Vervaet, C; Remon, J P; Baeyens, W R G

2009-09-01

The aim of the present study was to examine the complementary properties of Raman and near infrared (NIR) spectroscopy as PAT tools for the fast, noninvasive, nondestructive and in-line process monitoring of a freeze drying process. Therefore, Raman and NIR probes were built in the freeze dryer chamber, allowing simultaneous process monitoring. A 5% (w/v) mannitol solution was used as model for freeze drying. Raman and NIR spectra were continuously collected during freeze drying (one Raman and NIR spectrum/min) and the spectra were analyzed using principal component analysis (PCA) and multivariate curve resolution (MCR). Raman spectroscopy was able to supply information about (i) the mannitol solid state throughout the entire process, (ii) the endpoint of freezing (endpoint of mannitol crystallization), and (iii) several physical and chemical phenomena occurring during the process (onset of ice nucleation, onset of mannitol crystallization). NIR spectroscopy proved to be a more sensitive tool to monitor the critical aspects during drying: (i) endpoint of ice sublimation and (ii) monitoring the release of hydrate water during storage. Furthermore, via NIR spectroscopy some Raman observations were confirmed: start of ice nucleation, end of mannitol crystallization and solid state characteristics of the end product. When Raman and NIR monitoring were performed on the same vial, the Raman signal was saturated during the freezing step caused by reflected NIR light reaching the Raman detector. Therefore, NIR and Raman measurements were done on a different vial. Also the importance of the position of the probes (Raman probe above the vial and NIR probe at the bottom of the sidewall of the vial) in order to obtain all required critical information is outlined. Combining Raman and NIR spectroscopy for the simultaneous monitoring of freeze drying allows monitoring almost all critical freeze drying process aspects. Both techniques do not only complement each other, they also provided mutual confirmation of specific conclusions.

Quality by design: scale-up of freeze-drying cycles in pharmaceutical industry.

PubMed

Pisano, Roberto; Fissore, Davide; Barresi, Antonello A; Rastelli, Massimo

2013-09-01

This paper shows the application of mathematical modeling to scale-up a cycle developed with lab-scale equipment on two different production units. The above method is based on a simplified model of the process parameterized with experimentally determined heat and mass transfer coefficients. In this study, the overall heat transfer coefficient between product and shelf was determined by using the gravimetric procedure, while the dried product resistance to vapor flow was determined through the pressure rise test technique. Once model parameters were determined, the freeze-drying cycle of a parenteral product was developed via dynamic design space for a lab-scale unit. Then, mathematical modeling was used to scale-up the above cycle in the production equipment. In this way, appropriate values were determined for processing conditions, which allow the replication, in the industrial unit, of the product dynamics observed in the small scale freeze-dryer. This study also showed how inter-vial variability, as well as model parameter uncertainty, can be taken into account during scale-up calculations.

[Preparation of freeze - drying control materials of IgG antibody against Schistosoma japonicum for immunodetection kits].

PubMed

Jin, Huang; Chun-Lian, Tang; Zu-Wu, Tu; Li, Tang; Ke-Hui, Zhang; Qian, Li; Jun, Ye

2018-04-18

To prepare freeze-drying control materials of IgG antibody against Schistosoma japonicum for detection kits. The serum samples of schistosomiasis patients from endemic areas and normal people without history of schistosome infection or contact with infested water in Hubei Province were collected. All the sera were detected by the method approved by China Food and Drug Administration and selected for preparation of quality control samples. Totally twelve positive quality control materials, ten negative quality control materials, and one sensitive and one precision quality control materials were screened. According to the positive serum level, the positive degrees of quality control materials were divided into strong, medium and weak levels. The stability could be valid for one year. The freeze-drying quality control materials of IgG antibody against S. japonicum for detection kits are prepared. They are easy to use and have good stability, and therefore, they may meet the requirement of quality control for the detection of schistosomiasis diagnostics kits.

The performance of five fruit-derived and freeze-dried potentially probiotic Lactobacillus strains in apple, orange and grape juices.

PubMed

Garcia, Estefânia Fernandes; de Oliveira Araújo, Amanda; Luciano, Winnie Alencar; de Albuquerque, Thatyane Mariano Rodrigues; de Oliveira Arcanjo, Narciza Maria; Madruga, Marta Suely; Dos Santos Lima, Marcos; Magnani, Marciane; Saarela, Maria; de Souza, Evandro Leite

2018-03-30

This study assessed the survival of the fruit-derived and freeze-dried L. plantarum 49, L. brevis 59, L. paracasei 108, L. fermentum 111 and L. pentosus 129 strains during frozen storage and when incorporated into apple, orange and grape juice stored under refrigeration. Physicochemical parameters of juices containing the freeze-dried Lactobacillus strains and the survival of the test strains in the fruit juices during in vitro digestion were also evaluated. No decreases in survival rates (log N/log N0) of the freeze-dried cells were observed up to 1 month of storage. The survival rates of the freeze-dried strains L. plantarum 49 and L. paracasei 108 were >0.75 up to 4 months of storage. All freeze-dried strains exhibited survival rates of >0.75 up to 2 weeks of storage in apple juice; only L. plantarum 49 and L. paracasei 108 showed similar survival rates in orange and grape juices up to 2 weeks of storage. The contents of the monitored organic acids or sugars during storage varied depending on the added strain and the type of fruit juice. At the end of the in vitro digestion, L. brevis 59, L. paracasei 108 and L. fermentum 111 showed survival rates of >0.80 in apple juice. Apple juice was as the best substrate to the survival of the tested freeze-dried Lactobacillus strains over time. L. paracasei 108 and L. plantarum 49 as the strains presenting the best performance for incorporation in potentially probiotic fruit juices. This article is protected by copyright. All rights reserved.

Physicochemical characterization of commercial freeze-dried snake antivenoms.

PubMed

Herrera, María; Solano, Daniela; Gómez, Aarón; Villalta, Mauren; Vargas, Mariángela; Sánchez, Andrés; Gutiérrez, José María; León, Guillermo

2017-02-01

Freeze-drying is a process used to improve the stability of pharmaceutical proteins, including snake antivenoms. This additional step confers these with a higher stability in comparison to liquid formulations, especially in tropical regions where high temperatures could affect the activity of immunoglobulins. Currently, the knowledge about freeze-drying process conditions for snake antivenoms is very limited. Some of the scarce scientific works on this subject reported reconstitution times up to 90 min for these preparations, which could imply a delay in the beginning of the antivenom therapy at the clinical setting. Therefore there is a reasonable concern about whether freeze-dried antivenoms exhibit the desired attributes for solid pharmaceutical proteins. In this work, a physicochemical characterization of seven commercial freeze-dried snake antivenoms was performed based on tests recommended by the World Health Organization (WHO). No significant differences were observed between the products regarding macroscopic appearance of the solid cakes, reconstitution times, residual humidity and monomers content. On the other hand, total protein concentration, turbidity and electrophoretic profile were different among samples. Microscopic analysis by scanning electron microscopy showed no collapsed structure and, instead, most of the samples showed a characteristic protein morphology composed of smooth plates and channels. All the parameters tested in this study were according to literature recommendations and evidenced that, in spite of slight variations found for some products, formulation and freeze-drying conditions chosen by manufacturers are adequate to prevent aggregation and generate, in physicochemical terms, freeze-dried antivenoms of acceptable quality. Copyright © 2016 Elsevier Ltd. All rights reserved.

A comparative study of spray-dried and freeze-dried hydrocortisone/polyvinyl pyrrolidone solid dispersions.

PubMed

Dontireddy, Rakesh; Crean, Abina M

2011-10-01

Poor water solubility of new chemical entities (NCEs) is one of the major challenges the pharmaceutical industry currently faces. The purpose of this study was to investigate the feasibility of freeze-drying as an alternative technique to spray-drying to produce solid dispersions of poorly water-soluble drugs. Also investigated was the use of aqueous solvent mixtures in place of pure solvent for the production of solid dispersions. Aqueous solvent systems would reduce the environmental impact of pure organic solvent systems. Spray-dried and freeze-dried hydrocortisone/polyvinyl pyrrolidone solid dispersions exhibited differences in dissolution behavior. Freeze-dried dispersions exhibited faster dissolution rates than the corresponding spray-dried dispersions. Spray-dried systems prepared using both solvent systems (20% v/v and 96% v/v ethanol) displayed similar dissolution performance despite displaying differences in glass transition temperatures (T(g)) and surface areas. All dispersions showed drug/polymer interactions indicated by positive deviations in T(g) from the predicted values calculated using the Couchman-Karasz equation. Fourier transform infrared (FTIR) spectroscopic results confirmed the conversion of crystalline drug to the amorphous in the dispersions. Stability studies were preformed at 40°C and 75% relative humidity to investigate the physical stability of prepared dispersions. Recrystallization was observed after a month and the resultant dispersions were tested for their dissolution performance to compare with the dissolution performance of the dispersions prior to the stability study. The dissolution rate of the freeze-dried dispersions remained higher than both spray-dried dispersions after storage.

Controlled nucleation in freeze-drying: effects on pore size in the dried product layer, mass transfer resistance, and primary drying rate.

PubMed

Konstantinidis, Alex K; Kuu, Wei; Otten, Lori; Nail, Steven L; Sever, Robert R

2011-08-01

A novel and scalable method has been developed to enable control of the ice nucleation step for the freezing process during lyophilization. This method manipulates the chamber pressure of the freeze dryer to simultaneously induce nucleation in all product vials at a desired temperature. The effects of controlled nucleation on the drying rate of various formulations including 5% (w/w) mannitol, 5% (w/w) sucrose, and a mixture of 3% (w/w) mannitol and 2% (w/w) sucrose were studied. For a 5% (w/w) mannitol, uncontrolled ice nucleation occurred randomly at product temperatures between -8.0°C and -15.9°C as the vials were cooled to -40°C. Controlled ice nucleation was achieved at product temperatures between -2.3°C and -3.7°C. The effect of nucleation control on the effective pore radius (r(e) ) of the cake was determined from the product temperature profiles using a pore diffusion model in combination with a nonlinear parameter estimation approach reported earlier. Results show that the value of r(e) for 5% (w/w) mannitol was enlarged from 13 to 27 μm by uniformly inducing nucleation at higher temperatures. Applying the resistance parameters obtained from the pore diffusion model for 5% (w/w) mannitol, optimized cycles were theoretically generated and experimentally tested, resulting in a 41% reduction in primary drying time. Copyright © 2011 Wiley-Liss, Inc.

Calorimetric analysis of cryopreservation and freeze-drying formulations.

PubMed

Sun, Wendell Q

2015-01-01

Differential scanning calorimetry (DSC) is a commonly used thermal analysis technique in cryopreservation and freeze-drying research. It has been used to investigate crystallization, eutectic formation, glass transition, devitrification, recrystallization, melting, polymorphism, molecular relaxation, phase separation, water transport, thermochemistry, and kinetics of complex reactions (e.g., protein denaturation). Such information can be used for the optimization of protective formulations and process protocols. This chapter gives an introduction to beginners who are less familiar with this technique. It covers the instrument and its basic principles, followed by a discussion of the methods as well as examples of specific applications.

Effect of cryoprotective diluent and method of freeze-thawing on survival and acrosomal integrity of ram spermatozoa.

PubMed

Pontbriand, D; Howard, J G; Schiewe, M C; Stuart, L D; Wildt, D E

1989-08-01

A multifactorial study analyzed the effects of freezing method, cryoprotective diluent, semen to diluent ratio, and thawing velocity on post-thaw motility, progressive status, and acrosomal integrity of ram spermatozoa. Although semen to diluent ratio (1:3 vs 1:6, v/v) had no effect (P greater than 0.05), overall post-thaw spermatozoal viability was highly dependent on freezing method and cryoprotectant. Improved results were obtained by freezing semen in 0.5-ml French straws compared to dry ice pelleting. Manually freezing straws 5 cm above liquid nitrogen (LN2) was comparable to cooling straws in an automated, programmable LN2 unit. Of the two cryoprotective diluents tested, BF5F (containing the surfactant component sodium and triethanolamine lauryl sulfate) yielded approximately 50% fewer (P less than 0.05) spermatozoa with loose acrosomal caps compared to TEST. Thawing straws in a water bath at a higher velocity (60 degrees C for 8 sec) had no effect (P greater than 0.05) on spermatozoal motility, progressive status ratings, or acrosomal integrity when compared to a lower rate (37 degrees C for 20 sec). For the TEST group, thawing pellets in a dry, glass culture tube promoted (P less than 0.05) percentage sperm motility at 3 and 6 hr post-thawing, but for BF5F diluted semen this approach decreased the % of spermatozoa with normal apical ridges. The results suggest that the poor fertility rates often experienced using thawed ram semen likely result not only from reduced sperm motility, but also from compromised ultrastructural integrity. This damage is expressed by an increased loosening of the acrosomal cap, a factor which appears insensitive to freezing method but markedly influenced by the cryoprotective properties of the diluents tested.

Filament organization revealed in platinum replicas of freeze-dried cytoskeletons

PubMed Central

1980-01-01

This report presents the appearance of rapidly frozen, freeze-dried cytoskeletons that have been rotary replicated with platinum and viewed in the transmission electron microscope. The resolution of this method is sufficient to visualize individual filaments in the cytoskeleton and to discriminate among actin, microtubules, and intermediate filaments solely by their surface substructure. This identification has been confirmed by specific decoration with antibodies and selective extraction of individual filament types, and correlated with light microscope immunocytochemistry and gel electrophoresis patterns. The freeze-drying preserves a remarkable degree of three-dimensionality in the organization of these cytoskeletons. They look strikingly similar to the meshwork of strands or "microtrabeculae" seen in the cytoplasm of whole cells by high voltage electron microscopy, in that the filaments form a lattice of the same configutation and with the same proportions of open area as the microtrabeculae seen in whole cells. The major differences between these two views of the structural elements of the cytoplasmic matrix can be attributed to the effects of aldehyde fixation and dehydration. Freeze-dried cytoskeletons thus provide an opportunity to study--at high resolution and in the absence of problems caused by chemical fixation--the detailed organization of filaments in different regions of the cytoplasm and at different stages of cell development. In this report the pattern of actin and intermediate filament organization in various regions of fully spread mouse fibroblasts is described. PMID:6893451

Spray-Freeze Drying: a Suitable Method for Aerosol Delivery of Antibodies in the Presence of Trehalose and Cyclodextrins.

PubMed

Pouya, Maryam Amini; Daneshmand, Behnaz; Aghababaie, Shabnam; Faghihi, Homa; Vatanara, Alireza

2018-05-08

We aimed to prepare spray-freeze-dried powder of IgG considering physicochemical stability and aerodynamic aspects. Spray-freeze drying (SFD) exposes proteins to various stresses which should be compensated by suitable stabilizers. The competence of cyclodextrins (CDs), namely beta-cyclodextrin (βCD) and hydroxypropyl βCD (HPβCD), at very low concentrations, was investigated in the presence of separate mannitol- and trehalose-based formulations. Spray-freeze-dried preparations were quantified in terms of monomer recovery and conformation by size exclusion chromatography (SEC-HPLC) and Fourier transform infrared (FTIR) spectroscopy, respectively. Differential scanning calorimetry (DSC) and X-ray diffractometry (XRD) were employed to identify the thermal characteristics of powders. Particle morphology was visualized by scanning electron microscopy (SEM). Aerodynamic behavior of powders was checked through an Anderson cascade impactor (ACI). Although all formulations protected antibody from aggregation during the SFD process (aggregation < 1%), mannitol-containing ones failed upon the storage (19.54% in the worst case). Trehalose-HPβCD incomparably preserved the formulation with fine particle fraction (FPF) of 51.29%. Crystallization of mannitol resulted in IgG destabilization upon storage. Although employed concentration of CDs is too low (less than 50:1 molar ratio to protein), they successfully served as stabilizing agents in SFD with perfect improvement in aerosol functionality. Graphical Abstract ᅟ.

The immunogenicity of thin-film freeze-dried, aluminum salt-adjuvanted vaccine when exposed to different temperatures.

PubMed

Thakkar, Sachin G; Ruwona, Tinashe B; Williams, Robert O; Cui, Zhengrong

2017-04-03

Insoluble aluminum salts such as aluminum oxyhydroxide have been used for decades as adjuvants in human vaccines, and many vaccines contain aluminum salts as adjuvants. Aluminum salt-adjuvanted vaccines must be managed in cold-chain (2-8° C) during transport and storage, as vaccine antigens in general are too fragile to be stable in ambient temperatures, and unintentional slowing freezing causes irreversible aggregation and permanent damage to the vaccines. Previously, we reported that thin-film freeze-drying can be used to convert vaccines adjuvanted with an aluminum salt from liquid suspension into dry powder without causing particle aggregation or decreasing in immunogenicity following reconstitution. In the present study, using ovalbumin (OVA)-adsorbed Alhydrogel® (i.e. aluminum oxyhydroxide, 2% w/v) as a model vaccine, we showed that the immunogenicity of thin-film freeze-dried OVA-adsorbed Alhydrogel® vaccine powder was not significantly changed after it was exposed for an extended period of time in temperatures as high as 40° C or subjected to repeated slow freezing-and-thawing. It is expected that immunization programs can potentially benefit by integrating thin-film freeze-drying into vaccine preparations.

The immunogenicity of thin-film freeze-dried, aluminum salt-adjuvanted vaccine when exposed to different temperatures

PubMed Central

Thakkar, Sachin G.; Ruwona, Tinashe B.; Williams, Robert O.; Cui, Zhengrong

2017-01-01

ABSTRACT Insoluble aluminum salts such as aluminum oxyhydroxide have been used for decades as adjuvants in human vaccines, and many vaccines contain aluminum salts as adjuvants. Aluminum salt-adjuvanted vaccines must be managed in cold-chain (2–8° C) during transport and storage, as vaccine antigens in general are too fragile to be stable in ambient temperatures, and unintentional slowing freezing causes irreversible aggregation and permanent damage to the vaccines. Previously, we reported that thin-film freeze-drying can be used to convert vaccines adjuvanted with an aluminum salt from liquid suspension into dry powder without causing particle aggregation or decreasing in immunogenicity following reconstitution. In the present study, using ovalbumin (OVA)-adsorbed Alhydrogel® (i.e. aluminum oxyhydroxide, 2% w/v) as a model vaccine, we showed that the immunogenicity of thin-film freeze-dried OVA-adsorbed Alhydrogel® vaccine powder was not significantly changed after it was exposed for an extended period of time in temperatures as high as 40° C or subjected to repeated slow freezing-and-thawing. It is expected that immunization programs can potentially benefit by integrating thin-film freeze-drying into vaccine preparations. PMID:28051903

Mannitol/l-Arginine-Based Formulation Systems for Freeze Drying of Protein Pharmaceuticals: Effect of the l-Arginine Counter Ion and Formulation Composition on the Formulation Properties and the Physical State of Mannitol.

PubMed

Stärtzel, Peter; Gieseler, Henning; Gieseler, Margit; Abdul-Fattah, Ahmad M; Adler, Michael; Mahler, Hanns-Christian; Goldbach, Pierre

2016-10-01

Previous studies have shown that protein storage stability in freeze-dried l-arginine-based systems improved in the presence of chloride ions. However, chloride ions reduced the glass transition temperature of the freeze concentrate (Tg') and made freeze drying more challenging. In this study, l-arginine was freeze dried with mannitol to obtain partially crystalline solids that can be freeze dried in a fast process and result in elegant cakes. We characterized the effect of different l-arginine counter ions on physicochemical properties of mannitol compared with mannitol/sucrose systems. Thermal properties of formulations with different compositions were correlated to thermal history during freeze drying and to physicochemical properties (cake appearance, residual moisture, reconstitution time, crystallinity). Partially crystalline solids were obtained even at the highest l-arginine level (mannitol:l-arginine of 2:1) used in this study. All l-arginine-containing formulations yielded elegant cakes. Only cakes containing l-arginine chloride and succinate showed a surface "crust" formed by phase separation. X-ray powder diffraction showed that inhibition of mannitol crystallization was stronger for l-arginine compared with sucrose and varied with the type of l-arginine counter ion. The counter ion affected mannitol polymorphism and higher levels of mannitol hemi-hydrate were obtained at high levels of l-arginine chloride. Copyright © 2016 American Pharmacists Association®. Published by Elsevier Inc. All rights reserved.

Colloid-facilitated mobilization of metals by freeze-thaw cycles.

PubMed

Mohanty, Sanjay K; Saiers, James E; Ryan, Joseph N

2014-01-21

The potential of freeze-thaw cycles to release colloids and colloid-associated contaminants into water is unknown. We examined the effect of freeze-thaw cycles on the mobilization of cesium and strontium in association with colloids in intact cores of a fractured soil, where preferential flow paths are prevalent. Two intact cores were contaminated with cesium and strontium. To mobilize colloids and metal cations sequestered in the soil cores, each core was subjected to 10 intermittent wetting events separated by 66 h pauses. During the first five pauses, the cores were dried at room temperature, and during last five pauses, the cores were subjected to 42 h of freezing followed by 24 h of thawing. In comparison to drying, freeze-thaw cycles created additional preferential flow paths through which colloids, cesium, and strontium were mobilized. The wetting events following freeze-thaw intervals mobilized about twice as many colloids as wetting events following drying at room temperature. Successive wetting events following 66 h of drying mobilized similar amounts of colloids; in contrast, successive wetting events after 66 h of freeze-thaw intervals mobilized greater amounts of colloids than the previous one. Drying and freeze-thaw treatments, respectively, increased and decreased the dissolved cesium and strontium, but both treatments increased the colloidal cesium and strontium. Overall, the freeze-thaw cycles increased the mobilization of metal contaminants primarily in association with colloids through preferential flow paths. These findings suggest that the mobilization of colloid and colloid-associated contaminants could increase when temperature variations occur around the freezing point of water. Thus, climate extremes have the potential to mobilize contaminants that have been sequestered in the vadose zone for decades.

Cold tolerance of Littorinidae from southern Africa: intertidal snails are not constrained to freeze tolerance.

PubMed

Sinclair, Brent J; Marshall, David J; Singh, Sarika; Chown, Steven L

2004-11-01

All intertidal gastropods for which cold tolerance strategies have been assessed have been shown to be freeze tolerant. Thus, freeze tolerance is considered an adaptation to the intertidal environment. We investigated the cold tolerance strategies of three species of subtropical and temperate snails (Gastropoda: Littorinidae) to determine whether this group is phylogenetically constrained to freeze tolerance. We exposed 'dry' acclimated and 'wet' rehydrated snails to low temperatures to determine temperature of crystallisation (Tc), lower lethal temperature and LT(50) and to examine the relationship between ice formation and mortality. Tc was lowest in dry Afrolittorina knysnaensis (-13.6+/-0.4 degrees C), followed by dry Echinolittorina natalensis (-10.9+/-0.2 degrees C) and wet A. knysnaensis (-10.2+/-0.2 degrees C) . The Tc of both A. knysnaensis and E. natalensis increased with rehydration, whereas Tc of dry and wet Afrolittorina africana did not differ (-9.6+/-0.2 and -9.0+/-0.2 degrees C respectively). Wet snails of all species exhibited no or low survival of inoculative freezing, whereas dry individuals of A. knysnaensis could survive subzero temperatures above -8 degrees C when freezing was inoculated with ice . In the absence of external ice, Afrolittorina knysnaensis employs a freeze-avoidance strategy of cold tolerance, the first time this has been reported for an intertidal snail, indicating that there is no family-level phylogenetic constraint to freeze tolerance. Echinolittorina natalensis and A. africana both showed pre-freeze mortality and survival of some internal ice formation, but were not cold hardy in any strict sense.

Characterization of biomasses, concentrates, and permeates of dried powder of Kombucha fermentation of spinach (Amaranthus sp.) and broccoli (Brassica oleracea) with membrane microfiltration and freeze drying techniques for natural sources of folic acid

NASA Astrophysics Data System (ADS)

Nugraha, Tutun; Susilowati, Agustine; Aspiyanto, Lotulung, Puspa Dewi; Maryati, Yati

2017-11-01

Fermentation of spinach (Amaranthus sp) and Broccoli (Brassica oleracea) using Kombucha Culture has been shown to produce biomass that has the potential to become natural sources of folic acid. To produce the materials, following the fermentation, the biomass was filtered using membrane microfiltration (0.15 µm) at a pressure of 40 psia, at room temperature, yielding the concentrate and the permeate fractions. Following this step, freeze drying process was done on the biomass feeds, as well as on the concentrate and permeate fractions. For the freeze drying stage, the samples were frozen, and the condenser was kept at -50°C for 40 hours, while the pressure in the chamber was set at 200 Pa. Freeze drying results showed that the final products, have differences in compositions, as well as differences in the dominat monomers of folates. After water content was driven out, freeze drying increased the concentrations of folic acid in the dried products, and was found to be the highest in the concentrate fractions. Freeze drying has been shown to be capable of protecting the folates from heat and oxidative damages that typicaly occur with other types of drying. The final freeze dried concentrates of fermentation of spinach and broccoli were found to contain folic acid at 2531.88 µg/mL and 1626.94 µg/mL, total solids at 87.23% and 88.65 %, total sugar at 22.66 µg/mL and 25.13 µg/mL, total reducing sugar at 34.46 mg/mL and 15.22 mg/mL, as well as disolved protein concentrations at 0.93 mg/mL and 1.45 mg/mL. Liquid Chromatography Mass Spectometry (LC-MS) identification of the folates in the freeze dried concentrates of fermented spinach and broccoli was done using folic acid and glutamic acid standard solutions as the reference materials. The results showed the presence of folic acid and showed that the dominant monomers of molecules of folates with molecular weights of 441.44 Da. and 441.54 Da. for spinach and broccoli respectively. Moreover, the monomers of glutamic acid were also found at molecular weights of 147.21 Da. and 147.35 Da. for spinach and broccoli respectively. Thus, it has been shown that kombucha fermentation of spinach and broccoli, followed by membrane microfiltration and freeze drying process, could produce dried materials with high concentrations of folates that have the potential to be used as naturally derived sources of folic acid.

Effect of drying methods of microencapsulated Lactobacillus acidophilus and Lactococcus lactis ssp. cremoris on secondary protein structure and glass transition temperature as studied by Fourier transform infrared and differential scanning calorimetry.

PubMed

Dianawati, Dianawati; Mishra, Vijay; Shah, Nagendra P

2013-03-01

Protective mechanisms of casein-based microcapsules containing mannitol on Lactobacillus acidophilus and Lactococcus lactis ssp. cremoris, changes in their secondary protein structures, and glass transition of the microcapsules were studied after spray- or freeze-drying and after 10 wk of storage in aluminum foil pouches containing different desiccants (NaOH, LiCl, or silica gel) at 25°C. An in situ Fourier transform infrared analysis was carried out to recognize any changes in fatty acids (FA) of bacterial cell envelopes, interaction between polar site of cell envelopes and microcapsules, and alteration of their secondary protein structures. Differential scanning calorimetry was used to determine glass transition of microcapsules based on glass transition temperature (T(g)) values. Hierarchical cluster analysis based on functional groups of cell envelopes and secondary protein structures was also carried out to classify the microencapsulated bacteria due to the effects of spray- or freeze-drying and storage for 10 wk. The results showed that drying process did not affect FA and secondary protein structures of bacteria; however, those structures were affected during storage depending upon the type of desiccant used. Interaction between exterior of bacterial cell envelopes and microencapsulant occurred after spray- or freeze-drying; however, these structures were maintained after storage in foil pouch containing sodium hydroxide. Method of drying and type of desiccants influenced the level of similarities of microencapsulated bacteria. Desiccants and method of drying affected glass transition, yet no T(g) ≤25°C was detected. This study demonstrated that the changes in FA and secondary structures of the microencapsulated bacteria still occurred during storage at T(g) above room temperature, indicating that the glassy state did not completely prevent chemical activities. Copyright © 2013 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

Production of Inhalation Phage Powders Using Spray Freeze Drying and Spray Drying Techniques for Treatment of Respiratory Infections.

PubMed

Leung, Sharon S Y; Parumasivam, Thaigarajan; Gao, Fiona G; Carrigy, Nicholas B; Vehring, Reinhard; Finlay, Warren H; Morales, Sandra; Britton, Warwick J; Kutter, Elizabeth; Chan, Hak-Kim

2016-06-01

The potential of aerosol phage therapy for treating lung infections has been demonstrated in animal models and clinical studies. This work compared the performance of two dry powder formation techniques, spray freeze drying (SFD) and spray drying (SD), in producing inhalable phage powders. A Pseudomonas podoviridae phage, PEV2, was incorporated into multi-component formulation systems consisting of trehalose, mannitol and L-leucine (F1 = 60:20:20 and F2 = 40:40:20). The phage titer loss after the SFD and SD processes and in vitro aerosol performance of the produced powders were assessed. A significant titer loss (~2 log) was noted for droplet generation using an ultrasonic nozzle employed in the SFD method, but the conventional two-fluid nozzle used in the SD method was less destructive for the phage (~0.75 log loss). The phage were more vulnerable during the evaporative drying process (~0.75 log further loss) compared with the freeze drying step, which caused negligible phage loss. In vitro aerosol performance showed that the SFD powders (~80% phage recovery) provided better phage protection than the SD powders (~20% phage recovery) during the aerosolization process. Despite this, higher total lung doses were obtained for the SD formulations (SD-F1 = 13.1 ± 1.7 × 10(4) pfu and SD-F2 = 11.0 ± 1.4 × 10(4) pfu) than from their counterpart SFD formulations (SFD-F1 = 8.3 ± 1.8 × 10(4) pfu and SFD-F2 = 2.1 ± 0.3 × 10(4) pfu). Overall, the SD method caused less phage reduction during the powder formation process and the resulted powders achieved better aerosol performance for PEV2.

Freeze Drying of Fruits and Vegetables: A Laboratory Experiment.

ERIC Educational Resources Information Center

Noble, Richard D.

1979-01-01

Describes a laboratory experiment for freeze-drying fruits and vegetables which aims to expose college students to the principles of drying and simultaneous heat and mass transfer. The experimental apparatus, procedure of the experiment, and data analysis are also included. (HM)

Effects of cryoprotectants on the viability and activity of freeze dried recombinant yeasts as novel oral drug delivery systems assessed by an artificial digestive system.

PubMed

Blanquet, Stéphanie; Garrait, Ghislain; Beyssac, Erick; Perrier, Céline; Denis, Sylvain; Hébrard, Géraldine; Alric, Monique

2005-09-01

The aim of this study was to investigate, in a gastric-small intestinal system TIM-1, the effect of cryoprotectants on the survival of freeze-dried Saccharomyces cerevisiae expressing the heterologous P450 73A1 and their ability to convert trans-cinnamic acid into p-coumaric acid. Yeasts were lyophilized in suspensions of trehalose, maltose, lactose, or a milk proteins/trehalose mix. Freeze-dried or native yeasts and trans-cinnamic acid were introduced simultaneously into TIM-1 at the beginning of digestion. Yeast survival rate was evaluated by cell counting in the ileal effluents. P450 73A1 activity was followed by HPLC assay of p-coumaric acid. Freeze-dried yeasts showed high tolerance to digestive conditions. Nevertheless, their survival rate was lower than that of non-dried cells (around 80% whatever the protective agent vs. 96%). The ability of recombinant freeze-dried S. cerevisiae to perform a bioconversion reaction in the digestive tract was shown with all the protectants. The highest trans-cinnamic acid conversion rate (24 vs. 41% for native yeasts) was obtained with the milk proteins/trehalose mix. These results show that freeze-drying might be considered for the pharmaceutical formulation of new drug delivery systems based on orally administered recombinant yeasts and that TIM-1 could be a helpful tool for the pre-screening of oral dosage forms.

Space and Industrial Brine Drying Technologies

NASA Technical Reports Server (NTRS)

Jones, Harry W.; Wisniewski, Richard S.; Flynn, Michael; Shaw, Hali

2014-01-01

This survey describes brine drying technologies that have been developed for use in space and industry. NASA has long considered developing a brine drying system for the International Space Station (ISS). Possible processes include conduction drying in many forms, spray drying, distillation, freezing and freeze drying, membrane filtration, and electrical processes. Commercial processes use similar technologies. Some proposed space systems combine several approaches. The current most promising candidates for use on the ISS use either conduction drying with membrane filtration or spray drying.

Effects of vial packing density on drying rate during freeze-drying of carbohydrates or a model protein measured using a vial-weighing technique.

PubMed

Gieseler, Henning; Lee, Geoffrey

2008-02-01

To determine the effects of vial packing density in a laboratory freeze dryer on drying rate profiles of crystalline and amorphous formulations. The Christ freeze-drying balance measured cumulative water loss, m(t), and instantaneous drying rate, m(t), of water, mannitol, sucrose and sucrose/BSA formulations in commercial vials. Crystalline mannitol shows drying rate behaviour indicative of a largely homogeneous dried-product layer. The drying rate behaviour of amorphous sucrose indicates structural heterogeneity, postulated to come from shrinkage or microcollapse. Trehalose dries more slowly than sucrose. Addition of BSA to either disaccharide decreases primary drying time. Higher vial packing density greatly reduces drying rate because of effects of radiation heat transfer from chamber walls to test vial. Plots of m(t) versus radical t and m(t) versus layer thickness (either ice or dried-product) allow interpretation of changes in internal cake morphology during drying. Vial packing density greatly influences these profiles.

Reversed phase HPLC analysis of stability and microstructural effects on degradation kinetics of β-carotene encapsulated in freeze-dried maltodextrin-emulsion systems.

PubMed

Harnkarnsujarit, Nathdanai; Charoenrein, Sanguansri; Roos, Yrjö H

2012-09-26

Degradation of dispersed lipophilic compounds in hydrophilic solids depends upon matrix stability and lipid physicochemical properties. This study investigated effects of solid microstructure and size of lipid droplets on the stability of dispersed β-carotene in freeze-dried systems. Emulsions of β-carotene in sunflower oil were dispersed in maltodextrin systems (M040/DE6, M100/DE11, and M250/DE25.5) (8% w/w oil) and prefrozen at various freezing conditions prior to freeze-drying to control nucleation and subsequent pore size and structural collapse of freeze-dried solids. The particle size, physical state, and β-carotene contents of freeze-dried emulsions were measured during storage at various water activity (a(w)) using a laser particle size analyzer, differential scanning calorimeter, and high performance liquid chromatography (HPLC), respectively. The results showed that M040 stabilized emulsions in low temperature freezing exhibited lipid crystallization. Collapse of solids in storage at a(w) which plasticized systems to the rubbery state led to flow and increased the size of oil droplets. Degradation of β-carotene analyzed using a reversed-phase C(30) column followed first-order kinetics. Porosity of solids had a major effect on β-carotene stability; however, the highest stability was found in fully plasticized and collapsed solids.

Imaging ion and molecular transport at subcellular resolution by secondary ion mass spectrometry

NASA Astrophysics Data System (ADS)

Chandra, Subhash; Morrison, George H.

1995-05-01

The transport of K+, Na+, and Ca2+ were imaged in individual cells with a Cameca IMS-3f ion microscope. Strict cryogenic frozen freeze-dry sample preparations were employed. Ion redistribution artifacts in conventional chemical preparations are discussed. Cryogenically prepared freeze-fractured freeze-dried cultured cells allowed the three-dimensional ion microscopic imaging of elements. As smaller structures in calcium images can be resolved with the 0.5 [mu]m spatial resolution, correlative techniques are needed to confirm their identity. The potentials of reflected light microscopy, scanning electron microscopy and laser scanning confocal microscopy are discussed for microfeature recognition in freeze-fractured freeze-dried cells. The feasibility of using frozen freeze-dried cells for imaging molecular transport at subcellular resolution was tested. Ion microscopy successfully imaged the transport of the isotopically tagged (13C, 15N) amino acid, -arginine. The labeled amino acid was imaged at mass 28 with a Cs+ primary ion beam as the 28(13C15N)- species. After a 4 h exposure of LLC-PK1 kidney cells to 4 mM labeled arginine, the amino acid was localized throughout the cell with a preferential incorporation into the nucleus and nucleolus. An example is also shown of the ion microscopic imaging of sodium borocaptate, an experimental therapeutic drug for brain tumors, in cryogenically prepared frozen freeze-dried Swiss 3T3 cells.

Assessment of degree of disorder (amorphicity) of lyophilized formulations of growth hormone using isothermal microcalorimetry.

PubMed

Mosharraf, Mitra

2004-05-01

When determining the degree of disorder of a lyophilized cake of a protein, it is important to use an appropriate analytical technique. Differential scanning calorimetry (DSC) and X-ray powder diffraction (XRPD) are the most commonly used thermoanalytical techniques for characterizing freeze-dried protein formulations. Unfortunately, these methods are unable to detect solid-state disorder at levels < 10%. Also, interpretation of DSC results for freeze-dried protein formulations can be difficult, as a result of the more complex thermal events occurring with this technique. For example, proteins can inhibit the thermally induced recrystallization of the lyophilized cake, resulting in potential misinterpretation of DSC degree of disorder results. The aim of this investigation was to study the use of isothermal microcalorimetry (IMC) in the assessment of degree of solid-state disorder (amorphicity) of lyophilized formulations of proteins. For this purpose, two formulations of growth hormone were prepared by lyophilization. These formulations consisted of the same amounts of protein, mannitol, glycine, and phosphate buffer, but differed in the freeze-drying procedure. After lyophilization, the recrystallization of the samples was studied using IMC at 25 degrees C under different relative humidities (58-75%). The effect of available surface area was studied by determining the heat of recrystallization (Q) of the samples before and after disintegration of the cakes. The results showed that, in contrast to DSC, IMC allowed detection of the recrystallization event in the formulations. Although both formulations were completely disordered and indistinguishable according to XRPD method, IMC revealed that formulation B had a different solid-sate structure than formulation A. This difference was the result of differences in the freeze-drying parameters, demonstrating the importance of choosing appropriate analytical methodology.

Recent developments in high efficient freeze-drying of fruits and vegetables assisted by microwave: A review.

PubMed

Fan, Kai; Zhang, Min; Mujumdar, Arun S

2018-01-10

Microwave heating has been applied in the drying of high-value solids as it affords a number of advantages, including shorter drying time and better product quality. Freeze-drying at cryogenic temperature and extremely low pressure provides the advantage of high product quality, but at very high capital and operating costs due partly to very long drying time. Freeze-drying coupled with a microwave heat source speeds up the drying rate and yields good quality products provided the operating unit is designed and operated to achieve the potential for an absence of hot spot developments. This review is a survey of recent developments in the modeling and experimental results on microwave-assisted freeze-drying (MFD) over the past decade. Owing to the high costs involved, so far all applications are limited to small-scale operations for the drying of high-value foods such as fruits and vegetables. In order to promote industrial-scale applications for a broader range of products further research and development efforts are needed to offset the current limitations of the process. The needs and opportunities for future research and developments are outlined.

Effect of controlled ice nucleation on primary drying stage and protein recovery in vials cooled in a modified freeze-dryer.

PubMed

Passot, Stéphanie; Tréléa, Ioan Cristian; Marin, Michèle; Galan, Miquel; Morris, G John; Fonseca, Fernanda

2009-07-01

The freezing step influences lyophilization efficiency and protein stability. The main objective of this work was to investigate the impact on the primary drying stage of an ultrasound controlled ice nucleation technology, compared with usual freezing protocols. Lyophilization cycles involving different freezing protocols (applying a constant shelf cooling rate of 1 degrees C/min or 0.2 degrees C/min, putting vials on a precooled shelf, and controlling nucleation by ultrasounds or by addition of a nucleating agent) were performed in a prototype freeze-dryer. Three protective media including sucrose or maltodextrin and differing by their thermal properties and their ability to preserve a model protein (catalase) were used. The visual aspect of the lyophilized cake, residual water content, and enzymatic activity recovery of catalase were assessed after each lyophilization cycle and after 1 month of storage of the lyophilized product at 4 degrees C and 25 degrees C. The freezing protocols allowing increasing nucleation temperature (precooled shelf and controlled nucleation by using ultrasounds or a nucleating agent) induced a faster sublimation step and higher sublimation rate homogeneity. Whatever the composition of the protective medium, applying the ultrasound technology made it possible to decrease the sublimation time by 14%, compared with the freezing method involving a constant shelf cooling rate of 1 degrees C/min. Concerning the enzyme activity recovery, the impact of the freezing protocol was observed only for the protective medium involving maltodextrin, a less effective protective agent than sucrose. Higher activity recovery results were obtained after storage when the ultrasound technology or the precooled shelf method was applied. Controlling ice nucleation during the freezing step of the lyophilization process improved the homogeneity of the sublimation rates, which will, in turn, reduce the intervial heterogeneity. The freeze-dryer prototype including the system of controlled nucleation by ultrasounds appears to be a promising tool in accelerating sublimation and improving intrabatch homogeneity.

Freeze-dried spermatozoa: An alternative biobanking option for endangered species.

PubMed

Anzalone, Debora Agata; Palazzese, Luca; Iuso, Domenico; Martino, Giuseppe; Loi, Pasqualino

2018-03-01

In addition to the iconic wild species, such as the pandas and Siberian tigers, an ever-increasing number of domestic species are also threatened with extinction. Biobanking of spermatozoa could preserve genetic heritages of extinct species, and maintain biodiversity of existing species. Because lyophilized spermatozoa retain fertilizing capacity, the aim was to assess whether freeze-dried spermatozoa are an alternative option to save endangered sheep breeds. To achieve this objective, semen was collected from an Italian endangered sheep breed (Pagliarola), and a biobank of cryopreserved and freeze-dried spermatozoa was established, and evaluated using IVF (for frozen spermatozoa) and ICSI procedures (for frozen and freeze-dried spermatozoa). As expected, the fertilizing capacity of cryopreserved Pagliarola's spermatozoa was comparable to commercial semen stocks. To evaluate the activating capability of freeze-dried spermatozoa, 108 MII sheep oocytes were subjected to ICSI, and allocated to two groups: 56 oocytes were activated by incubation with ionomycin (ICSI-FDSa) and 52 were not activated (ICSI-FDSna). Pronuclear formation (2PN) was investigated at 14-16 h after ICSI in fixed presumptive zygotes. Only artificially activated oocytes developed into blastocysts after ICSI. In the present study, freeze-dried ram spermatozoa induced blastocyst development following ICSI at a relatively high proportion, providing evidence that sperm lyophilization is an alternative, low cost storage option for biodiversity preservation of domestic species. Copyright © 2018 Elsevier B.V. All rights reserved.

NaCl stress impact on the key enzymes in glycolysis from Lactobacillus bulgaricus during freeze-drying.

PubMed

Li, Chun; Sun, Jinwei; Qi, Xiaoxi; Liu, Libo

2015-01-01

The viability of Lactobacillus bulgaricus in freeze-drying is of significant commercial interest to dairy industries. In the study, L.bulgaricus demonstrated a significantly improved (p < 0.05) survival rate during freeze-drying when subjected to a pre-stressed period under the conditions of 2% (w/v) NaCl for 2 h in the late growth phase. The main energy source for the life activity of lactic acid bacteria is related to the glycolytic pathway. To investigate the phenomenon of this stress-related viability improvement in L. bulgaricus, the activities and corresponding genes of key enzymes in glycolysis during 2% NaCl stress were studied. NaCl stress significantly enhanced (p < 0.05) glucose utilization. The activities of glycolytic enzymes (phosphofructokinase, pyruvate kinase, and lactate dehydrogenase) decreased during freeze-drying, and NaCl stress were found to improve activities of these enzymes before and after freeze-drying. However, a transcriptional analysis of the corresponding genes suggested that the effect of NaCl stress on the expression of the pfk2 gene was not obvious. The increased survival of freeze-dried cells of L. bulgaricus under NaCl stress might be due to changes in only the activity or translation level of these enzymes in different environmental conditions but have no relation to their mRNA transcription level.

Freeze-dried snake antivenoms formulated with sorbitol, sucrose or mannitol: comparison of their stability in an accelerated test.

PubMed

Herrera, María; Tattini, Virgilio; Pitombo, Ronaldo N M; Gutiérrez, José María; Borgognoni, Camila; Vega-Baudrit, José; Solera, Federico; Cerdas, Maykel; Segura, Alvaro; Villalta, Mauren; Vargas, Mariángela; León, Guillermo

2014-11-01

Freeze-drying is used to improve the long term stability of pharmaceutical proteins. Sugars and polyols have been successfully used in the stabilization of proteins. However, their use in the development of freeze-dried antivenoms has not been documented. In this work, whole IgG snake antivenom, purified from equine plasma, was formulated with different concentrations of sorbitol, sucrose or mannitol. The glass transition temperatures of frozen formulations, determined by Differential Scanning Calorimetry (DSC), ranged between -13.5 °C and -41 °C. In order to evaluate the effectiveness of the different stabilizers, the freeze-dried samples were subjected to an accelerated stability test at 40 ± 2 °C and 75 ± 5% relative humidity. After six months of storage at 40 °C, all the formulations presented the same residual humidity, but significant differences were observed in turbidity, reconstitution time and electrophoretic pattern. Moreover, all formulations, except antivenoms freeze-dried with mannitol, exhibited the same potency for the neutralization of lethal effect of Bothrops asper venom. The 5% (w:v) sucrose formulation exhibited the best stability among the samples tested, while mannitol and sorbitol formulations turned brown. These results suggest that sucrose is a better stabilizer than mannitol and sorbitol in the formulation of freeze-dried antivenoms under the studied conditions. Copyright © 2014 Elsevier Ltd. All rights reserved.

Effects of Freeze-Dried Vegetable Products on the Technological Process and the Quality of Dry Fermented Sausages.

PubMed

Eisinaite, Viktorija; Vinauskiene, Rimante; Viskelis, Pranas; Leskauskaite, Daiva

2016-09-01

The aim of this study was to compare the chemical composition of freeze-dried vegetable powders: celery, celery juice, parsnip and leek. The effect of different freeze-dried vegetables onto the ripening process and the properties of dry fermented sausages was also evaluated. Vegetable products significantly (p < 0.05) differed in their chemical composition: celery products contained higher amounts of nitrates, total phenolic compounds and lower amounts of sucrose, parsnip had higher concentration of proteins, leek was rich in fat. The analysis of pH, water activity, lactic acid bacteria, coagulase-positive staphylococci and coliforms content showed that the incorporation of freeze-dried vegetables had no negative effect on the fermentation and ripening process of dry fermented sausages. In addition, the color parameters for sausages with the added lyophilised celery products were considerable (p < 0.05) more stable during these processes. At the end of the ripening process the sausages made with lyophilised celery juice were characterised by higher lightness and lower hardness than those made with the addition of other vegetable products and control. Freeze-dried celery, celery juice, parsnip and leek have some potential for the usage as a functional ingredient or as a source for indirect addition of nitrate in the production of fermented sausages. © 2016 Institute of Food Technologists®

Effect of Carboxylmethyl Cellulose Coating and Osmotic Dehydration on Freeze Drying Kinetics of Apple Slices

PubMed Central

Rahimi, Jamshid; Singh, Ashutosh; Adewale, Peter Olusola; Adedeji, Akinbode A.; Ngadi, Michael O.; Raghavan, Vijaya

2013-01-01

The effect of different concentrations of sugar solution (hypertonic) (30%, 45% and 60% w/v) and carboxyl methyl cellulose (CMC) (0%, 1% and 2% w/v) coating on freeze drying of apple slices was studied. In total, nine treatments with respect to concentrations of hypertonic solution and coating layer were prepared to analyze their influence on the physical and chemical properties of freeze dried apple slices. It was observed that increase in the sugar solution concentration, decreased the moisture content of the apple slices significantly impacting its water activity, texture and sugar gain. Application of different concentrations of CMC coating had no significant effect on the properties of dried apple slices. A significant change was observed for color of CMC coated freeze dried apple slices pretreated with 60% sugar solution. Drying kinetics of pretreated apple slices were fitted by using two drying models, Newton’s and Page’s. Page’s model showed higher R-square and lower root mean square error (RSME) compared to Newton’s model. PMID:28239107

Evaluation of specimen preparation techniques for micro-PIXE localisation of elements in hyperaccumulating plants

NASA Astrophysics Data System (ADS)

Kachenko, Anthony G.; Siegele, Rainer; Bhatia, Naveen P.; Singh, Balwant; Ionescu, Mihail

2008-04-01

Hybanthus floribundus subsp. floribundus, a rare Australian Ni-hyperaccumulating shrub and Pityrogramma calomelanos var. austroamericana, an Australian naturalized As-hyperaccumulating fern are promising species for use in phytoremediation of contaminated sites. Micro-proton-induced X-ray emission (μ-PIXE) spectroscopy was used to map the elemental distribution of the accumulated metal(loid)s, Ca and K in leaf or pinnule tissues of the two plant species. Samples were prepared by two contrasting specimen preparation techniques: freeze-substitution in tetrahydrofuran (THF) and freeze-drying. The specimens were analysed to compare the suitability of each technique in preserving (i) the spatial elemental distribution and (ii) the tissue structure of the specimens. Further, the μ-PIXE results were compared with concentration of elements in the bulk tissue obtained by ICP-AES analysis. In H. floribundus subsp. floribundus, μ-PIXE analysis revealed Ni, Ca and K concentrations in freeze-dried leaf tissues were at par with bulk tissue concentrations. Elemental distribution maps illustrated that Ni was preferentially localised in the adaxial epidermal tissues (1% DW) and least concentration was found in spongy mesophyll tissues (0.53% DW). Conversely, elemental distribution maps of THF freeze-substituted tissues indicated significantly lower Ni, Ca and K concentrations than freeze-dried specimens and bulk tissue concentrations. Moreover, Ni concentrations were uniform across the whole specimen and no localisation was observed. In P. calomelanos var. austroamericana freeze-dried pinnule tissues, μ-PIXE revealed statistically similar As, Ca and K concentrations as compared to bulk tissue concentrations. Elemental distribution maps showed that As localisation was relatively uniform across the whole specimen. Once again, THF freeze-substituted tissues revealed a significant loss of As compared to freeze-dried specimens and the concentrations obtained by bulk tissue analysis. The results demonstrate that freeze-drying is a suitable sample preparation technique to study elemental distribution of ions in H. floribundus and P. calomelanos plant tissues using μ-PIXE spectroscopy. Furthermore, cellular structure was preserved in samples prepared using this technique.

Effect of drying method to antioxidants capacity of Limnophila aromatica

NASA Astrophysics Data System (ADS)

Yen, Tran Thi Ngoc; Vu, Nguyen Hoang

2017-09-01

Limnophila aromatica is widely used in South East Asian countries to make spices in food and medicine in traditional medicine. The use value of vegetables is known because some of the lesser constituents in plants are called antioxidants. These active ingredients have not been fully researched and their pharmacological effects are underestimated. In this study, the drying temperature at 40 °C was showed that the antioxidant activity decreased the most. The drying temperature of 50 °C is suitable for convection drying method and drying temperature of 60 °C suitable for vacuum drying, as it retains the most antioxidant properties. Regarding the drying method, freeze drying proved to be effective when retaining high antioxidant capacity. Using The convection drying at 50 °C and the vacuum drying at 60 °C, the antioxidant activity of Limnophila aromatica was not different. Over 6 weeks of preservation, the dried product has deterioration in antioxidant properties.

Investigation of PEG crystallization in frozen and freeze-dried PEGylated recombinant human growth hormone-sucrose systems: implications on storage stability.

PubMed

Bhatnagar, Bakul S; Martin, Susan W H; Hodge, Tamara S; Das, Tapan K; Joseph, Liji; Teagarden, Dirk L; Shalaev, Evgenyi Y; Suryanarayanan, Raj

2011-08-01

The objectives of the current study were to investigate (i) the phase behavior of a PEGylated recombinant human growth hormone (PEG-rhGH, ∼60 kDa) during freeze-drying and (ii) its storage stability. The phase transitions during freeze-thawing of an aqueous solution containing PEG-rhGH and sucrose were characterized by differential scanning calorimetry. Finally, PEG-rhGH and sucrose formulations containing low, medium, and high polyethylene glycol (PEG) to sucrose ratios were freeze-dried in dual-chamber syringes and stored at 4°C and 25°C. Chemical decomposition (methionine oxidation and deamidation) and irreversible aggregation were characterized by size-exclusion and ion-exchange chromatography, and tryptic mapping. PEG crystallization was facilitated when it was covalently linked with rhGH. When the solutions were frozen, phase separation into PEG-rich and sucrose-rich phases facilitated PEG crystallization and the freeze-dried cake contained crystalline PEG. Annealing caused PEG crystallization and when coupled with higher drying temperatures, the primary drying time decreased by up to 51%. When the freeze-dried cakes were stored at 4°C, while there was no change in the purity of the PEG-rhGH monomer, deamidation was highest in the formulations with the lowest PEG to sucrose ratio. When stored at 25°C, this composition also showed the most pronounced decrease in monomer purity, the highest level of aggregation, and deamidation. Furthermore, an increase in PEG crystallinity during storage was accompanied by a decrease in PEG-rhGH stability. Interestingly, during storage, there was no change in PEG crystallinity in formulations with medium and high PEG to sucrose ratios. Although PEG crystallization during freeze-drying did not cause protein degradation, crystallization during storage might have influenced protein stability. Copyright © 2011 Wiley-Liss, Inc.

Effect of different drying methods on concentrations of several phytochemicals in herbal preparation of 8 medicinal plants leaves.

PubMed

Mahanom, H; Azizah, A; Dzulkifly, M

1999-12-01

The effect of oven drying at 50ᵒC ± 1ᵒC for 9 hour, 70ᵒC ± 1ᵒC for 5 hour and freeze drying on retention of chlorophyll, riboflavin, niacin, ascorbic acid and carotenoids in herbal preparation consisting of 8 medicinal plants was evaluated. The medicinal plants selected were leaves of Apium graveolens (saderi), Averrhoa bilimbi (belimbing buluh), Centella asiatica (pegaga), Mentha arvensis (pudina), Psidium guajava (jambu batu), Sauropus androgynous (cekor manis), Solanum nigrum (terung meranti) and Polygonum minus (kesum ). Results revealed that both type and conditions of the drying treatments affected retention of all phytochemicals analysed. Herbal preparation developed using oven drying was found to have inferior phytochemicals content compared to that obtained by freeze dryer. Nevertheless, the herbal preparation developed using all treatments still retain appreciable amount of phytochemicals studied, especially carotenoids, ascorbic acid, niacin and riboflavin and thus have potential for commercial purposes.

Microencapsulation of Natural Anthocyanin from Purple Rosella Calyces by Freeze Drying

NASA Astrophysics Data System (ADS)

Nafiunisa, A.; Aryanti, N.; Wardhani, D. H.; Kumoro, A. C.

2017-11-01

Anthocyanin extract in powder form will improve its use since the powder is easier to store and more applicable. Microencapsulation method is introduced as an efficient way for protecting pigment such as anthocyanin. This research was aimed to characterise anthocyanin encapsulated products prepared from purple Roselle calyces by freeze drying. The liquid anthocyanin extracts from ultrasound-assisted extraction were freeze-dried with and without the addition of 10% w/w maltodextrins as a carrier and coating agents. The quality attributes of the powders were characterised by their colour intensity, water content, and solubility. Analysis of encapsulated material was performed for the powder added by maltodextrin. The stability of the microencapsulated pigment in solution form was determined for 11 days. Total anthocyanin content was observed through pH differential method. The results of the colour intensity analysis confirm that the product with maltodextrin addition has more intense colour with L* value of 29.69 a* value of 54.29 and b* value of 8.39. The result with the addition of maltodextrin has less moisture content and more soluble in water. It is verified that better results were obtained for powder with maltodextrin addition. Anthocyanin in the powder form with maltodextrin addition exhibits higher stability even after 11 days. In conclusion, the microencapsulation of anthocyanin with maltodextrin as a carrier and coating agent presented a potential method to produce anthocyanin powder from purple Roselle.

Identification of cyanidin glycosides as constituents of freeze-dried black raspberries which inhibit anti-benzo[a]pyrene-7,8-diol-9,10-epoxide induced NFκB and AP-1 activity

PubMed Central

Hecht, Stephen S.; Huang, Chuanshu; Stoner, Gary D.; Li, Jingxia; Kenney, Patrick M. J.; Sturla, Shana J.; Carmella, Steven G.

2010-01-01

Dietary freeze-dried black raspberries inhibit tumor induction by N-nitrosomethylbenzylamine in the rat esophagus, but the constituents responsible for this chemopreventive activity have not been identified. We fractionated freeze-dried black raspberries and used mouse epidermal JB6 Cl 41 cells stably transfected with either a nuclear factor kappa B (NFκB)- or an activator protein 1 (AP-1)-luciferase reporter, and treated with racemic anti-benzo[a]pyrene-7,8-diol-9,10-epoxide (BPDE), to assess the inhibitory effects of the fractions. The ethanol and water extracts of the freeze-dried black raspberries had inhibitory activity and these extracts were fractionated by HPLC to give several bioactive fractions. Further HPLC analysis yielded multiple subfractions, some of which inhibited BPDE-induced NFκB activity. Major constituents of the most active subfractions were identified by their spectral properties and in comparison with standards as cyanidin-3-O-glucoside, cyanidin 3-O-(2G-xylosylrutinoside) and cyanidin 3-O-rutinoside. Analysis of freeze-dried black raspberries indicated that these three components comprised ∼3.4% of the material by dry weight. Consistent with these results, standard cyanidin-3-O-glucoside and cyanidin chloride were also good inhibitors of BPDE-induced NFκB activity. The results of this study demonstrate that cyanidin glycosides of freeze-dried black raspberries are bioactive compounds which could account for at least some of the chemopreventive activity observed in animal models. PMID:16522666

Identification of cyanidin glycosides as constituents of freeze-dried black raspberries which inhibit anti-benzo[a]pyrene-7,8-diol-9,10-epoxide induced NFkappaB and AP-1 activity.

PubMed

Hecht, Stephen S; Huang, Chuanshu; Stoner, Gary D; Li, Jingxia; Kenney, Patrick M J; Sturla, Shana J; Carmella, Steven G

2006-08-01

Dietary freeze-dried black raspberries inhibit tumor induction by N-nitrosomethylbenzylamine in the rat esophagus, but the constituents responsible for this chemopreventive activity have not been identified. We fractionated freeze-dried black raspberries and used mouse epidermal JB6 Cl 41 cells stably transfected with either a nuclear factor kappa B (NFkappaB)- or an activator protein 1 (AP-1)-luciferase reporter, and treated with racemic anti-benzo[a]pyrene-7,8-diol-9,10-epoxide (BPDE), to assess the inhibitory effects of the fractions. The ethanol and water extracts of the freeze-dried black raspberries had inhibitory activity and these extracts were fractionated by HPLC to give several bioactive fractions. Further HPLC analysis yielded multiple subfractions, some of which inhibited BPDE-induced NFkappaB activity. Major constituents of the most active subfractions were identified by their spectral properties and in comparison with standards as cyanidin-3-O-glucoside, cyanidin 3-O-(2(G)-xylosylrutinoside) and cyanidin 3-O-rutinoside. Analysis of freeze-dried black raspberries indicated that these three components comprised approximately 3.4% of the material by dry weight. Consistent with these results, standard cyanidin-3-O-glucoside and cyanidin chloride were also good inhibitors of BPDE-induced NFkappaB activity. The results of this study demonstrate that cyanidin glycosides of freeze-dried black raspberries are bioactive compounds which could account for at least some of the chemopreventive activity observed in animal models.

Comparison of methods for the removal of organic carbon and extraction of chromium, iron and manganese from an estuarine sediment standard and sediment from the Calcasieu River estuary, Louisiana, U.S.A.

USGS Publications Warehouse

Simon, N.S.; Hatcher, S.A.; Demas, C.

1992-01-01

U.S. National Bureau of Standards (NBS) estuarine sediment 1646 from the Chesapeake Bay, Maryland, and surface sediment collected at two sites in the Calcasieu River estuary, Louisiana, were used to evaluate the dilute hydrochloric acid extraction of Cr, Fe and Mn from air-dried and freeze-dried samples that had been treated by one of three methods to remove organic carbon. The three methods for the oxidation and removal of organic carbon were: (1) 30% hydrogen peroxide; (2) 30% hydrogen peroxide plus 0.25 mM pyrophosphate; and (3) plasma oxidation (low-temperature ashing). There was no statistically significant difference at the 95% confidence level between air- and freeze-dried samples with respect to the percent of organic carbon removed by the three methods. Generally, there was no statistically significant difference at the 95% confidence level between air- and freeze-dried samples with respect to the concentration of Cr, Fe and Mn that was extracted, regardless of the extraction technique that was used. Hydrogen peroxide plus pyrophosphate removed the most organic carbon from sediment collected at the site in the Calcasieu River that was upstream from industrial outfalls. Plasma oxidation removed the most organic carbon from the sediment collected at a site in the Calcasieu River close to industrial outfalls and from the NBS estuarine sediment sample. Plasma oxidation merits further study as a treatment for removal of organic carbon. Operational parameters can be chosen to limit the plasma oxidation of pyrite which, unlike other Fe species, will not be dissolved by dilute hydrochloric acid. Preservation of pyrite allows the positive identification of Fe present as pyrite in sediments. ?? 1992.

Light assisted drying (LAD) for protein stabilization: optimization of laser processing parameters

NASA Astrophysics Data System (ADS)

Young, Madison A.; Antczak, Andrew T.; Elliott, Gloria D.; Trammell, Susan R.

2017-02-01

In this study, a novel light-based processing method to create an amorphous trehalose matrix for the stabilization of proteins is discussed. Near-IR radiation is used to remove water from samples, leaving behind an amorphous solid with embedded protein. This method has potential applications in the stabilization of protein-based therapeutics and diagnostics that are becoming widely used in the treatment and diagnosis of a variety of diseases. Freeze-drying or freezing are currently the standard for the preservation of proteins, but these methods are expensive and can be challenging in some environments due to a lack of available infrastructure. Light-assisted drying offers a relatively inexpensive method for drying samples. Proteins suspended in a trehalose solution are dehydrated using near-infrared laser light. The laser radiation speeds drying and as water is removed the sugar forms a protective matrix. The goal of this study is to determine processing parameters that result in fast processing times and low end moisture contents (EMC), while maintaining the functionality of embedded proteins. We compare the effect of changing processing wavelength, power and resulting sample temperature, and substrate material on the EMC for two NIR laser sources (1064 nm and 1850 nm). The 1850 nm laser resulted in the lowest EMC (0.1836+/-0.09 gH2O/gDryWeight) after 10 minutes of processing on borosilicate glass microfiber paper. This suggests a storage temperature of 3°C.

A study on friability, hardness and fiber content analysis of fiber enriched milk tablet

NASA Astrophysics Data System (ADS)

Suzihaque, M. U. H.; Irfan, M. H.; Ibrahim, U. K.

2017-06-01

This study was performed to analyze the friability, hardness and fiber content of fiber enriched milk tablet derived from five different local fiber sources such as carrot, spinach, dragon fruit, mango and watermelon. Cow milk was mixed to complement with the tablet as a protein source. The powder were spray dried at 100°C, 120°C and 140°C and freeze dried at -60°C. The mixture of fruits and milk were made into equal ratio with the addition of 15 maltodextrin as a carrier. Tablets formed were used for friability and hardness test while dried powder were used for fiber content analysis. Dragon fruit tablet dried at 140°C have the highest friability with 11. 42 of weight loss. The second highest friability was spinach tablet dried at 100°C and 120°C drying temp erature with 9.30 and 9.28 respectively. The lowest friability was exhibited by carrot, mango and watermelon tablet at 100°C and dragon fruit at 120°C while carrot and spinach at 140°C. In contras t, none of the freeze dried tablets showed any weight loss hence they are not friable. For hardness test, all of the freeze dried showed to have higher tensile strength than spray dried, where carrot showed to be the highest at 2.27 Newton and the lowest were spray dried mango at 0.16 Newton. In fiber content analysis, freeze dried mango have the highest fiber content followed by freeze dried carrot and 140°C s pray dried carrot. It can be concluded that the higher the spray dry temperature, the more friable is the tablet. While, high friability leads to lower hardness of tablets. In terms of fiber content, the higher the spray dry temperature, the lower the fiber content found.

Use of a non-linear method for including the mass uncertainty of gravimetric standards and system measurement errors in the fitting of calibration curves for XRFA freeze-dried UNO/sub 3/ standards

DOE Office of Scientific and Technical Information (OSTI.GOV)

Pickles, W.L.; McClure, J.W.; Howell, R.H.

1978-05-01

A sophisticated nonlinear multiparameter fitting program was used to produce a best fit calibration curve for the response of an x-ray fluorescence analyzer to uranium nitrate, freeze dried, 0.2% accurate, gravimetric standards. The program is based on unconstrained minimization subroutine, VA02A. The program considers the mass values of the gravimetric standards as parameters to be fit along with the normal calibration curve parameters. The fitting procedure weights with the system errors and the mass errors in a consistent way. The resulting best fit calibration curve parameters reflect the fact that the masses of the standard samples are measured quantities withmore » a known error. Error estimates for the calibration curve parameters can be obtained from the curvature of the ''Chi-Squared Matrix'' or from error relaxation techniques. It was shown that nondispersive XRFA of 0.1 to 1 mg freeze-dried UNO/sub 3/ can have an accuracy of 0.2% in 1000 s.« less

Freeze drying formulation using microscale and design of experiment approaches: a case study using granulocyte colony-stimulating factor.

PubMed

Grant, Yitzchak; Matejtschuk, Paul; Bird, Christopher; Wadhwa, Meenu; Dalby, Paul A

2012-04-01

The lyophilization of proteins in microplates, to assess and optimise formulations rapidly, has been applied for the first time to a therapeutic protein and, in particular, one that requires a cell-based biological assay, in order to demonstrate the broader usefulness of the approach. Factorial design of experiment methods were combined with lyophilization in microplates to identify optimum formulations that stabilised granulocyte colony-stimulating factor during freeze drying. An initial screen rapidly identified key excipients and potential interactions, which was then followed by a central composite face designed optimisation experiment. Human serum albumin and Tween 20 had significant effects on maintaining protein stability. As previously, the optimum formulation was then freeze-dried in stoppered vials to verify that the microscale data is relevant to pilot scales. However, to validate the approach further, the selected formulation was also assessed for solid-state shelf-life through the use of accelerated stability studies. This approach allows for a high-throughput assessment of excipient options early on in product development, while also reducing costs in terms of time and quantity of materials required.

Stability of prothrombin and factor VII in freeze-dried plasma

PubMed Central

Brozović, M.; Gurd, L. J.; Robertson, I.; Bangham, D. R.

1971-01-01

The stability of prothrombin and factor VII was studied using accelerated degradation tests in three preparations of freeze-dried pooled normal plasmas. In a previous report (Brozović, Gurd, Robertson, and Bangham, 1971) factor X was shown to be relatively unstable in these preparations of freeze-dried plasma: it was calculated that up to 8% of the original factor X activity would be lost after 10 years at −20°C, up to 54% at 4°C, and up to 90% at room temperature. The losses of factor VII activity were estimated to be negligible at −20°C, between 2 and 18% at 4°C, and between 20 and 70% of the original activity at 20°C, after 10 years of storage. Prothrombin was found to be less stable than factor VII: the expected loss in 10 years at −20°C may be up to 4%, at 4°C up to 30%, and at 20°C up to 83% of the initial activity. These findings indicate that in freeze-dried plasma prothrombin as well as factor X may be insufficiently stable for plasma to serve as long-term reference material for the standardization of the one-stage prothrombin time. Moreover, the loss of prothrombin and factor X in freeze-dried plasma stored at 4°C may be so high that when it is required to preserve these factors it may be necessary to store freeze-dried plasma at lower temperatures. PMID:5130534

Graphene oxide foams and their excellent adsorption ability for acetone gas

DOE Office of Scientific and Technical Information (OSTI.GOV)

He, Yongqiang; School of Science, Tianjin University, Tianjin 300072; Zhang, Nana

2013-09-01

Graphical abstract: - Highlights: • GO and RGO foams were prepared using a simple and green method, unidirectional freeze-drying. • The porous structure of the foams can be adjusted by changing GO concentrations. • GO and RGO foams show good adsorption efficiency for acetone gas. - Abstract: Graphene oxide (GO) and reduced graphene oxide (RGO) foams were prepared using a unidirectional freeze-drying method. These porous carbon materials were characterized by thermal gravimetric analysis, differential scanning calorimetry, X-ray photoelectron spectroscopy and scanning electron microscopy. The adsorption behavior of the two kinds of foams for acetone was studied. The result showed thatmore » the saturated adsorption efficiency of the GO foams was over 100%, and was higher than that of RGO foams and other carbon materials.« less

Effect of different drying techniques on flowability characteristics and chemical properties of natural carbohydrate-protein Gum from durian fruit seed

PubMed Central

2013-01-01

Background A natural carbohydrate biopolymer was extracted from the agricultural biomass waste (durian seed). Subsequently, the crude biopolymer was purified by using the saturated barium hydroxide to minimize the impurities. Finally, the effect of different drying techniques on the flow characteristics and functional properties of the purified biopolymer was investigated. The present study elucidated the main functional characteristics such as flow characteristics, water- and oil-holding capacity, solubility, and foaming capacity. Results In most cases except for oven drying, the bulk density decreased, thus increasing the porosity. This might be attributed to the increase in the inter-particle voids of smaller sized particles with larger contact surface areas per unit volume. The current study revealed that oven-dried gum and freeze-dried gum had the highest and lowest compressibility index, thus indicating the weakest and strongest flowability among all samples. In the present work, the freeze-dried gum showed the lowest angle of repose, bulk, tapped and true density. This indicates the highest porosity degree of freeze dried gum among dried seed gums. It also exhibited the highest solubility, and foaming capacity thus providing the most desirable functional properties and flow characteristics among all drying techniques. Conclusion The present study revealed that freeze drying among all drying techniques provided the most desirable functional properties and flow characteristics for durian seed gum. PMID:23289739

Influence of Freeze-Drying and Oven-Drying Post Blanching on the Nutrient Composition of the Edible Insect Ruspolia differens.

PubMed

Fombong, Forkwa Tengweh; Van Der Borght, Mik; Vanden Broeck, Jozef

2017-09-16

The longhorn grasshopper, Ruspolia differens (Serville), plays an important role as a food source across Sub-Saharan Africa, where it is consumed as a delicacy in both rural and urban areas. The effect of two drying methods (freeze-drying and oven-drying), employed after blanching, on the proximate, fatty acid and mineral composition of the two most common morphs was determined. Ruspolia differens grasshoppers were harvested in Uganda and Kenya from wild swarms during the rainy periods of November-December 2016. Based on cuticular coloration, we identified three morphs, green, brown and purple, which occurred at a ratio of 65:33:2, respectively. Results indicated that these insects have a high lipid content of 36%, as well as significant protein levels ranging between 33% and 46% dry matter. Oleic acid (44%) and palmitic acid (28%) were the two most abundant fatty acids; while the presence of arachidonic acid (0.6%) and docosahexaenoic acid (0.21%) suggests that Ruspolia differens is also a source of polyunsaturated fatty acids. The observed amino acid profile showed similar trends in all morphs, and all essential amino acids were present. Calcium (896-1035 mg/100 g), potassium (779-816 mg/100 g) and phosphorus (652-685 mg/100 g) were quite high among the minerals. The presence of the trace elements iron (217-220 mg/100 g), zinc (14.2-14.6 mg/100 g), manganese (7.4-8.3 mg/100 g) and copper (1.66 mg/100 g) suggests that inclusion of these grasshoppers in human diets may aid in combatting micronutrient deficiencies. Oven-drying Ruspolia differens delivered the same nutritional quality as freeze-drying. Hence, both drying approaches can be adequately used to formulate insect-based food products without noticeable nutritional changes.

Development of freeze-dried albumin-free formulation of recombinant factor VIII SQ.

PubMed

Osterberg, T; Fatouros, A; Mikaelsson, M

1997-07-01

To develop a stable freeze-dried formulation of recombinant factor VIII-SQ (r-VIII SQ) without the addition of albumin. Different formulations were evaluated for their protective effect during sterile filtration, freeze-thawing, freeze-drying, reconstitution and long term storage. Factor VIII activity (VIII:C), visual inspection, clarity, solubility, moisture content and soluble aggregates and/ or fragments were assayed. A combination of non-crystallising excipients (L-histidine and sucrose), a non-ionic surfactant (polysorbate 80) and a crystalline bulking agent (sodium chloride) was found to preserve the factor VIII activity during formulation, freeze-drying and storage. Calcium chloride was included to prevent dissociation of the heavy and light chains of r-VIII SQ. Sodium chloride was chosen as the primary bulking agent since the concentration of sodium chloride necessary for dissolution of r-VIII SQ in the buffer will inhibit the crystallization of many potential cake formers. It was found that L-histidine, besides functioning as a buffer, also protected r-VIII SQ during freeze-drying and storage. A pH close to 7 was found to be optimal. Some potential macromolecular stabilisers, PEG 4000, Haes-steril and Haemaccel, were evaluated but they did not improve the recovery of VIII:C. The freeze-dried formulation was stable for at least two years at 7 degrees C and for at least one year at 25 degrees C. The reconstituted solution was stable for at least 100 hours at 25 degrees C. The albumin-free formulation resulted in consistently high recovery of VIII:C, very low aggregate formation and good storage stability. The stability of the reconstituted solution makes the formulation suitable for continuous administration via infusion pump. The formulation strategy described here may also be useful for other proteins which require a high ionic strength.

Optimization of the secondary drying step in freeze drying using TDLAS technology.

PubMed

Schneid, Stefan C; Gieseler, Henning; Kessler, William J; Luthra, Suman A; Pikal, Michael J

2011-03-01

The secondary drying phase in freeze drying is mostly developed on a trial-and-error basis due to the lack of appropriate noninvasive process analyzers. This study describes for the first time the application of Tunable Diode Laser Absorption Spectroscopy, a spectroscopic and noninvasive sensor for monitoring secondary drying in laboratory-scale freeze drying with the overall purpose of targeting intermediate moisture contents in the product. Bovine serum albumin/sucrose mixtures were used as a model system to imitate high concentrated antibody formulations. First, the rate of water desorption during secondary drying at constant product temperatures (-22 °C, -10 °C, and 0 °C) was investigated for three different shelf temperatures. Residual moisture contents of sampled vials were determined by Karl Fischer titration. An equilibration step was implemented to ensure homogeneous distribution of moisture (within 1%) in all vials. The residual moisture revealed a linear relationship to the water desorption rate for different temperatures, allowing the evaluation of an anchor point from noninvasive flow rate measurements without removal of samples from the freeze dryer. The accuracy of mass flow integration from this anchor point was found to be about 0.5%. In a second step, the concept was successfully tested in a confirmation experiment. Here, good agreement was found for the initial moisture content (anchor point) and the subsequent monitoring and targeting of intermediate moisture contents. The present approach for monitoring secondary drying indicated great potential to find wider application in sterile operations on production scale in pharmaceutical freeze drying. © 2011 American Association of Pharmaceutical Scientists

The effect of freezing and drying on leaching of DOM from above ground vascular plant material from the Alaskan Arctic

NASA Astrophysics Data System (ADS)

Khosh, M. S.; McClelland, J. W.

2014-12-01

Our understanding of the seasonal dynamics of fluvial dissolved organic matter (DOM) concentrations and fluxes in Arctic catchments has increased substantially during recent years, especially during the spring, which historically has been an under-sampled time period. While a number of studies have observed peaks in both DOM concentrations and fluxes during the spring snowmelt, our knowledge of the mechanisms that control these observations are still lacking. During the initial snowmelt period, frozen ground and the snow matrix act to constrain melt-water to the soil surface. We hypothesize that restriction of flow during this time facilitates leaching of DOM from senescent above ground vegetation and detritus contributing to the high DOM concentrations observed during the spring melt. This study focuses on the effect of freezing and drying on the leaching of dissolved organic carbon and nitrogen (DOC and DON) from above ground vascular plant material. Specifically, we examined the treatment effects of freezing, drying, and freeze-drying on three genera of common Alaskan Arctic vascular plants; Eriophorum (spp.), Carex (spp.), and Salix (spp.). Frozen and freeze-dried plant material released more DOC over the experimental 96 hour leaching period compared to plant material that was only dried. Qualitatively, these patterns were similar among the different plant types, while quantitatively Salix leached more DOC than either Eriophorum or Carex in all treatments. Similar patterns were also seen for DON between the different treatments and among the different plant types. Compositionally, DOM that was leached from frozen and freeze-dried material had higher C:N ratios than material that was only dried. Comparatively, DOM leached from Salix had much higher C:N ratios than either Eriophorum or Carex. During the first 24 hours of leaching, C:N ratios tended to increase followed by a subsequent leveling or decrease, suggesting that the composition of leached DOM varied during the 96 hour time period. Our findings suggest that the seasonal timing of freezing and drying conditions experienced by senesced plant material during the late summer, fall, and winter may impact DOM leaching dynamics on that same plant material the following spring during snowmelt.

Optimization of Freeze Drying Conditions for Purified Pectinase from Mango (Mangifera indica cv. Chokanan) Peel

PubMed Central

Mehrnoush, Amid; Mustafa, Shuhaimi; Yazid, Abdul Manap Mohd

2012-01-01

Response surface methodology (RSM) along with central composite design (CCD) was applied to optimize the freeze drying conditions for purified pectinase from mango (Mangifera indica cv. Chokanan) peel. The effect of pectinase content (−2.66, 62.66 mg/mL), Arabic gum (−1.21, 10.21%, w/v), and maltodextrin (0.73, 7.26%, w/v) as independent variables on activity, yield, and storage stability of freeze-dried enzyme was evaluated. Storage stability of pectinase was investigated after one week at 4 °C and yield percentage of the enzyme after encapsulation was also determined. The independent variables had the most significant (p < 0.05) effect on pectinase activity and yield of the enzyme. It was observed that the interaction effect of Arabic gum and maltodextrin improved the enzymatic properties of freeze-dried pectinase. The optimal conditions for freeze-dried pectinase from mango peel were obtained using 30 mg/mL of pectinase content, 4.5 (%, w/v) of Arabic gum, and 4 (%, w/v) of maltodextrin. Under these conditions, the maximum activity (11.12 U/mL), yield (86.4%) and storage stability (84.2%) of encapsulated pectinase were achieved. PMID:22489134

Optimization of freeze drying conditions for purified pectinase from mango (Mangifera indica cv. Chokanan) peel.

PubMed

Mehrnoush, Amid; Mustafa, Shuhaimi; Yazid, Abdul Manap Mohd

2012-01-01

Response surface methodology (RSM) along with central composite design (CCD) was applied to optimize the freeze drying conditions for purified pectinase from mango (Mangifera indica cv. Chokanan) peel. The effect of pectinase content (-2.66, 62.66 mg/mL), Arabic gum (-1.21, 10.21%, w/v), and maltodextrin (0.73, 7.26%, w/v) as independent variables on activity, yield, and storage stability of freeze-dried enzyme was evaluated. Storage stability of pectinase was investigated after one week at 4 °C and yield percentage of the enzyme after encapsulation was also determined. The independent variables had the most significant (p < 0.05) effect on pectinase activity and yield of the enzyme. It was observed that the interaction effect of Arabic gum and maltodextrin improved the enzymatic properties of freeze-dried pectinase. The optimal conditions for freeze-dried pectinase from mango peel were obtained using 30 mg/mL of pectinase content, 4.5 (%, w/v) of Arabic gum, and 4 (%, w/v) of maltodextrin. Under these conditions, the maximum activity (11.12 U/mL), yield (86.4%) and storage stability (84.2%) of encapsulated pectinase were achieved.

Gap-freezing approach for shortening the lyophilization cycle time of pharmaceutical formulations-demonstration of the concept.

PubMed

Kuu, Wei Y; Doty, Mark J; Rebbeck, Christine L; Hurst, William S; Cho, Yong K

2013-08-01

During gap freezing, vials are placed on a metal tray, which is separated from the shelf surface with a small air gap that eliminates significant conductive heat transfer from the shelf to the bottom of the vial. The purpose of this freezing approach is to reduce the lyophilization cycle time of various amorphous formulations by nearly isothermal freezing. Such isothermal freezing promotes the formation of large ice crystals, and thus large pores throughout the cake, which subsequently accelerates the primary drying rate. The nucleation temperature using gap freezing, for the experimental conditions tested, was in the range of -1°C to -6°C, much higher than the range of -10°C to -14°C found using conventional shelf freezing. Isothermal freezing becomes effective when the gap is greater than 3 mm. The pore sizes and cake resistance during primary drying for various formulations were determined using the pore diffusion model developed by Kuu et al. (Pharm Dev Technol, 2011, 16(4): 343-357). Reductions in primary drying time were 42% (for 10% sucrose), 45% (for 10% trehalose), and 33% (for 5% sucrose). Copyright © 2013 Wiley Periodicals, Inc.

Porosity and water activity effects on stability of crystalline β-carotene in freeze-dried solids.

PubMed

Harnkarnsujarit, Nathdanai; Charoenrein, Sanguansri; Roos, Yrjö H

2012-11-01

Stability of entrapped crystalline β-carotene as affected by water activity, solids microstructure, and composition of freeze-dried systems was investigated. Aliquots (1000 mm(3) , 20% w/w solids) of solutions of maltodextrins of various dextrose equivalents (M040:DE6, M100:DE11, and M250:DE25.5), M100-sugars (1:1 glucose, fructose and sucrose), and agar for gelation with dispersed β-carotene were frozen at -20, -40, or -80 °C and freeze-dried. Glass transition and α-relaxation temperatures were determined with differential scanning calorimetry and dynamic mechanical analysis, respectively. β-Carotene contents were monitored spectrophotometrically. In the glassy solids, pore microstructure had a major effect on β-carotene stability. Small pores with thin walls and large surface area allowed β-carotene exposure to oxygen which led to a higher loss, whereas structural collapse enhanced stability of β-carotene by decreasing exposure to oxygen. As water plasticized matrices, an increase in molecular mobility in the matrix enhanced β-carotene degradation. Stability of dispersed β-carotene was highest at around 0.2 a(w) , but decreasing structural relaxation times above the glass transition correlated well with the rate of β-carotene degradation at higher a(w) . Microstructure, a(w) , and component mobility are important factors in the control of stability of β-carotene in freeze-dried solids. β-Carotene expresses various nutritional benefits; however, it is sensitive to oxygen and the degradation contributes to loss of nutritional values as well as product color. To increase stability of β-carotene in freeze-dried foods, the amount of oxygen penetration need to be limited. The modification of freeze-dried food structures, for example, porosity and structural collapse, components, and humidity effectively enhance the stability of dispersed β-carotene in freeze-dried solids. © 2012 Institute of Food Technologists®

Antioxidant and anti-inflammatory activities of freeze-dried grapefruit phenolics as affected by gum arabic and bamboo fibre addition and microwave pretreatment.

PubMed

García-Martínez, Eva; Andújar, Isabel; Yuste Del Carmen, Alberto; Prohens, Jaime; Martínez-Navarrete, Nuria

2018-06-01

Recent epidemiological studies have suggested that phenolic compounds present in grapefruit play an important role in the bioactive properties of this fruit. However, the consumption of fresh grapefruit is low. Freeze-dried powdered grapefruit can be an alternative to promote this fruit consumption. To improve the quality and stability of the powdered fruit, encapsulating and anticaking agents can be added. In the present study, different grapefruit powders obtained by freeze-drying with the addition of gum arabic (1.27 g per 100 g) and bamboo fibre (0.76 g per 100 g) with and without a pre-drying microwave treatment were compared with the fresh and freeze-dried fruit with no carriers added, aiming to evaluate the effect of these preservation processes on phenolics content and on its antioxidant [1,1-diphenyl-2-picrylhydrazyl (DPPH), 2,2'-azinobis(3-ethylbenzothiazoline-6-sulphonic acid) (ABTS) and ferric reducing ability of plasma (FRAP)] and anti-inflamatory (evaluated in RAW 264.7 macrophages) capacities. Freeze-drying and gum arabic and bamboo fibre addition significantly increased total phenolics, as well as the antioxidant and anti-inflammatory activities (by inhibiting nitric oxide production of lipopolysaccharide activated RAW 264.7 macrophages), of grapefruit. An additional increase in these parameters was obtained with microwave pretreatment before freeze-drying. The combined addition of gum arabic and bamboo fibre to grapefruit puree and the application of a microwave pretreatment improve the functional properties of the fruit without showing cytotoxicity in vitro. © 2017 Society of Chemical Industry. © 2017 Society of Chemical Industry.

Heat transfer characteristics of current primary packaging systems for pharmaceutical freeze-drying.

PubMed

Hibler, Susanne; Gieseler, Henning

2012-11-01

In the field of freeze-drying, the primary packaging material plays an essential role. Here, the packaging system not only contains and protects the drug product during storage and shipping, but it is also directly involved in the freeze-drying process itself. The heat transfer characteristics of the actual container system influence product temperature and therefore product homogeneity and quality as well as process performance. Consequently, knowledge of the container heat transfer characteristics is of vital importance for process optimization. It is the objective of this review article to provide a summary of research focused on heat transfer characteristics of different container systems for pharmaceutical freeze-drying. Besides the common tubing and molded glass vials and metal trays, more recent packaging solutions like polymer vials, LYOGUARD® trays, syringes, and blister packs are discussed. Recent developments in vial manufacturing are also taken into account. Copyright © 2012 Wiley Periodicals, Inc.

Effects of dehydration methods on quality characteristics of yellow passion fruit co-products.

PubMed

Silva, Neiton C; Duarte, Claudio R; Barrozo, Marcos As

2017-11-01

The production and processing of fruits generate a large amount of residues, which are usually disposed of or under-used, representing losses of raw material and energy. The present paper investigates the effect of four dehydration techniques (convective, infrared, microwave and freeze-drying) on yellow passion fruit (Passiflora edulis f. flavicarpa) co-products and the influence of the main variables on moisture removal and bioactive compounds. The compounds analyzed were total phenolics, total flavonoids, ascorbic acid and pectin. The content of phenolics and flavonoids increased after dehydration in all techniques investigated and the process temperatures directly affected the ascorbic acid content. Microwave dehydration showed the best results for most bioactive compounds analyzed, if performed in suitable process conditions. However, the highest levels of pectin content were obtained by freeze-drying and convective dehydration. This study reinforces the importance of the adequate use of passion fruit co-products due to the high levels of bioactive compounds in this material. Microwave dehydration presented the best results, which indicates the potential use of this technique for a better exploitation of fruit co-products. Larger quantities of pectin were extracted from samples dehydrated through methodologies with long-time process and low temperatures, such as convective drying and freeze-drying. © 2017 Society of Chemical Industry. © 2017 Society of Chemical Industry.

Non-invasive product temperature determination during primary drying using tunable diode laser absorption spectroscopy.

PubMed

Schneid, Stefan C; Gieseler, Henning; Kessler, William J; Pikal, Michael J

2009-09-01

The goal of this work was to demonstrate the application of Tunable Diode Laser Absorption Spectroscopy (TDLAS) as a non-invasive method to determine the average product temperature of the batch during primary drying. The TDLAS sensor continuously measures the water vapor concentration and the vapor flow velocity in the spool connecting the freeze-dryer chamber and condenser. Vapor concentration and velocity data were then used to determine the average sublimation rate (g/s) which was subsequently integrated to evaluate the amount of water removed from the product. Position dependent vial heat transfer coefficients (K(v)) were evaluated using the TDLAS sensor data for 20 mL vials during sublimation tests with pure water. TDLAS K(v) data showed good agreement to K(v) data obtained by the traditional gravimetric procedure. K(v) for edge vials was found to be about 20-30% higher than that of center vials. A weighted K(v) was then used to predict a representative average product temperature from TDLAS data in partial and full load freeze drying runs with 5%, 7.5%, or 10% (w/w) sucrose, mannitol, and glycine solutions. TDLAS product temperatures for all freeze-drying runs were within 1-2 degrees C of "center vial" steady state thermocouple data.

Modeling of heat and mass transfer processes for the gap-lyophilization system using the mannitol-trehalose-NaCl formulation.

PubMed

Kuu, Wei Y; Doty, Mark J; Nisipeanu, Eugen; Rebbeck, Christine L; Cho, Yong K; Smit, Mark H

2014-09-01

Gap freezing (GF) is a new concept that was developed to reduce the primary drying time using an alternative freezing process. The purpose of this investigation was to determine the gap-tray heat transfer coefficient, Kgtr , and to investigate the effect of gap lyophilization on cycle reduction of a mannitol-trehalose-NaCl (MTN) formulation. The values of Kgtr were measured using the product temperature profiles in three different configurations: (1) shelf freezing followed by shelf drying (denoted as SF-SD), (2) GF followed by SD (denoted as GF-SD), and (3) GF followed by gap drying (denoted as GF-GD). For the lyophilization cycle using shelf drying (SF-SD), 80% of the heat transferred during primary drying was from the bottom shelf to the vial, versus 20% via radiation from the top shelf. For the lyophilization cycle using gap drying (GF-GD), only 37% of the heat transferred during primary drying was from the bottom shelf to the vial versus 63% via radiation from the top shelf. Furthermore, GF in conjunction with annealing significantly reduces the dry layer resistance of the MTN formulation, which is the opposite of what was observed with a conventional freezing cycle. © 2014 Wiley Periodicals, Inc. and the American Pharmacists Association.

Phytochemical Profiles and Antimicrobial Activities of Allium cepa Red cv. and A. sativum Subjected to Different Drying Methods: A Comparative MS-Based Metabolomics.

PubMed

Farag, Mohamed A; Ali, Sara E; Hodaya, Rashad H; El-Seedi, Hesham R; Sultani, Haider N; Laub, Annegret; Eissa, Tarek F; Abou-Zaid, Fouad O F; Wessjohann, Ludger A

2017-05-08

Plants of the Allium genus produce sulphur compounds that give them a characteristic (alliaceous) flavour and mediate for their medicinal use. In this study, the chemical composition and antimicrobial properties of Allium cepa red cv. and A. sativum in the context of three different drying processes were assessed using metabolomics. Bulbs were dried using either microwave, air drying, or freeze drying and further subjected to chemical analysis of their composition of volatile and non-volatile metabolites. Volatiles were collected using solid phase micro-extraction (SPME) coupled to gas chromatography-mass spectrometry (GC/MS) with 42 identified volatiles including 30 sulphur compounds, four nitriles, three aromatics, and three esters. Profiling of the polar non-volatile metabolites via ultra-performance liquid chromatography coupled to high resolution MS (UPLC/MS) annotated 51 metabolites including dipeptides, flavonoids, phenolic acids, and fatty acids. Major peaks in GC/MS or UPLC/MS contributing to the discrimination between A. sativum and A. cepa red cv. were assigned to sulphur compounds and flavonoids. Whereas sulphur conjugates amounted to the major forms in A. sativum , flavonoids predominated in the chemical composition of A. cepa red cv. With regard to drying impact on Allium metabolites, notable and clear separations among specimens were revealed using principal component analysis (PCA). The PCA scores plot of the UPLC/MS dataset showed closer metabolite composition of microwave dried specimens to freeze dried ones, and distant from air dried bulbs, observed in both A. cepa and A. sativum . Compared to GC/MS, the UPLC/MS derived PCA model was more consistent and better in assessing the impact of drying on Allium metabolism. A phthalate derivative was found exclusively in a commercial garlic preparation via GC/MS, of yet unknown origin. The freeze dried samples of both Allium species exhibited stronger antimicrobial activities compared to dried specimens with A. sativum being in general more active than A. cepa red cv.

The Freeze-Drying of Wet and Waterlogged Materials from Archaeological Excavations

ERIC Educational Resources Information Center

Watson, Jacqui

2004-01-01

Large quantities of wood and leather have been found in the waterlogged layers on archaeological excavations. Centuries of burial, however, have left these materials in a very degraded and vulnerable state such that if they dry out they will fall apart. This paper discusses the physics behind the freeze-drying techniques that allow the…

Kinetics, biocompounds, antioxidant activity, and sensory attributes of quinces as affected by drying method.

PubMed

Szychowski, Przemysław J; Lech, Krzysztof; Sendra-Nadal, Esther; Hernández, Francisca; Figiel, Adam; Wojdyło, Aneta; Carbonell-Barrachina, Ángel A

2018-07-30

Quinces are attracting interest due to their health and nutritional benefits. Drying kinetics, bioactive compounds, antioxidant activity, and the main sensory parameters were determined in dried quinces, cultivar Leskovač, as affected by the drying method. The highest total polyphenols content was observed in dried samples obtained after freeze drying and convective drying at 50 °C. The best drying treatment, considering only sensory attributes, was vacuum-microwave drying at 480 W, because it led to intermediate dark color and high intensities of basic tastes and key flavor attributes. The studied parameters were finally used to recommend convective drying at 60 °C as the most appropriate drying method for quinces, because it had a high content of total phenolic compounds (2nd best treatment out of 10), a good sensory profile, was cheap, and caused no negative effects on nutritional or sensory parameters; the only disadvantage was its long drying time. Copyright © 2018 Elsevier Ltd. All rights reserved.

Innovative procedure for the determination of gross-alpha/gross-beta activities in drinking water.

PubMed

Wisser, S; Frenzel, E; Dittmer, M

2006-03-01

An alternative sample preparation method for the determination of gross-alpha/beta activity concentrations in drinking water is introduced in this paper. After the freeze-drying of tap water samples, determination by liquid scintillation counting can be applied utilizing alpha/beta separation. It has been shown that there is no adsorption or loss of solid radionuclides during the freeze-drying procedure. However, the samples have to be measured quickly after the preparation since the ingrowth of daughter isotopes negatively effects the measurement. The limits of detection for gross-alpha and gross-beta activity are in the range 25-210 mBq/l, respectively, for a measurement time of only 8-9 h.

Effect of the aerated structure on selected properties of freeze-dried hydrocolloid gels

NASA Astrophysics Data System (ADS)

Ciurzyńska, Agnieszka; Lenart, Andrzej

2016-01-01

The ability to create diverse structures and studies on the effect of the aerated structure on selected properties with the use of freeze-dried gels may provide knowledge about the properties of dried foods. Such gels can be a basis for obtaining innovative food products. For the gel preparation, 3 types of hydrocolloids were used: low-methoxyl pectin, a mixture of xanthan gum and locust-bean gum, and a mixture of xanthan gum and guar gum. Gels were aerated for 3 and 7 min, frozen at a temperature of -45°C 2 h-1, and freeze-dried at a temperature of 30°C. For the samples obtained, structure, porosity, shrinkage, rehydration, and colour were investigated. It was shown that the type of the hydrocolloid and aeration time influence the structure of freeze-dried gels, which determines such properties of samples as porosity, shrinkage, density, rehydration, and colour. The bigger pores of low-methoxyl pectin gels undergo rehydration in the highest degree. The delicate and aerated structure of gels with the mixture of xanthan gum and locust-bean gum was damaged during freeze-drying and shrinkage exhibited the highest value. Small pores of samples with the mixture of xanthan gum and guar gum were responsible for the lower rehydration properties, but the highest porosity value contributed to the highest lightness value.

Potential of Near-Infrared Chemical Imaging as Process Analytical Technology Tool for Continuous Freeze-Drying.

PubMed

Brouckaert, Davinia; De Meyer, Laurens; Vanbillemont, Brecht; Van Bockstal, Pieter-Jan; Lammens, Joris; Mortier, Séverine; Corver, Jos; Vervaet, Chris; Nopens, Ingmar; De Beer, Thomas

2018-04-03

Near-infrared chemical imaging (NIR-CI) is an emerging tool for process monitoring because it combines the chemical selectivity of vibrational spectroscopy with spatial information. Whereas traditional near-infrared spectroscopy is an attractive technique for water content determination and solid-state investigation of lyophilized products, chemical imaging opens up possibilities for assessing the homogeneity of these critical quality attributes (CQAs) throughout the entire product. In this contribution, we aim to evaluate NIR-CI as a process analytical technology (PAT) tool for at-line inspection of continuously freeze-dried pharmaceutical unit doses based on spin freezing. The chemical images of freeze-dried mannitol samples were resolved via multivariate curve resolution, allowing us to visualize the distribution of mannitol solid forms throughout the entire cake. Second, a mannitol-sucrose formulation was lyophilized with variable drying times for inducing changes in water content. Analyzing the corresponding chemical images via principal component analysis, vial-to-vial variations as well as within-vial inhomogeneity in water content could be detected. Furthermore, a partial least-squares regression model was constructed for quantifying the water content in each pixel of the chemical images. It was hence concluded that NIR-CI is inherently a most promising PAT tool for continuously monitoring freeze-dried samples. Although some practicalities are still to be solved, this analytical technique could be applied in-line for CQA evaluation and for detecting the drying end point.

Comparison of blueberry powder produced via foam-mat freeze-drying versus spray-drying: evaluation of foam and powder properties.

PubMed

Darniadi, Sandi; Ho, Peter; Murray, Brent S

2018-03-01

Blueberry juice powder was developed via foam-mat freeze-drying (FMFD) and spray-drying (SD) via addition of maltodextrin (MD) and whey protein isolate (WPI) at weight ratios of MD/WPI = 0.4 to 3.2 (with a fixed solids content of 5 wt% for FMFD and 10 wt% for SD). Feed rates of 180 and 360 mL h -1 were tested in SD. The objective was to evaluate the effect of the drying methods and carrier agents on the physical properties of the corresponding blueberry powders and reconstituted products. Ratios of MD/WPI = 0.4, 1.0 and 1.6 produced highly stable foams most suitable for FMFD. FMFD gave high yields and low bulk density powders with flake-like particles of large size that were also dark purple with high red values. SD gave low powder recoveries. The powders had higher bulk density and faster rehydration times, consisting of smooth, spherical and smaller particles than in FMFD powders. The SD powders were bright purple but less red than FMFD powders. Solubility was greater than 95% for both FMFD and SD powders. The FMFD method is a feasible method of producing blueberry juice powder and gives products retaining more characteristics of the original juice than SD. © 2017 Society of Chemical Industry. © 2017 Society of Chemical Industry.

Application of process analytical technology for monitoring freeze-drying of an amorphous protein formulation: use of complementary tools for real-time product temperature measurements and endpoint detection.

PubMed

Schneid, Stefan C; Johnson, Robert E; Lewis, Lavinia M; Stärtzel, Peter; Gieseler, Henning

2015-05-01

Process analytical technology (PAT) and quality by design have gained importance in all areas of pharmaceutical development and manufacturing. One important method for monitoring of critical product attributes and process optimization in laboratory scale freeze-drying is manometric temperature measurement (MTM). A drawback of this innovative technology is that problems are encountered when processing high-concentrated amorphous materials, particularly protein formulations. In this study, a model solution of bovine serum albumin and sucrose was lyophilized at both conservative and aggressive primary drying conditions. Different temperature sensors were employed to monitor product temperatures. The residual moisture content at primary drying endpoints as indicated by temperature sensors and batch PAT methods was quantified from extracted sample vials. The data from temperature probes were then used to recalculate critical product parameters, and the results were compared with MTM data. The drying endpoints indicated by the temperature sensors were not suitable for endpoint indication, in contrast to the batch methods endpoints. The accuracy of MTM Pice data was found to be influenced by water reabsorption. Recalculation of Rp and Pice values based on data from temperature sensors and weighed vials was possible. Overall, extensive information about critical product parameters could be obtained using data from complementary PAT tools. © 2015 Wiley Periodicals, Inc. and the American Pharmacists Association.

Angular absorption of light used for evaluation of structural damage to porcine meat caused by aging, drying and freezing.

PubMed

Kaspar, Pavel; Prokopyeva, Elena; Tománek, Pavel; Grmela, Lubomír

2017-04-01

Meat as a rich source of protein is sought after by people from all over the world. It is also very susceptible to decay because of many internal and external processes affecting it. In this work an easy and quick method of detection of structural damage caused by decay or mishandling the meat is attempted by the method of angular absorption of light. The difference between structural changes due to aging, drying and freezing is explored and the resulting changes in light absorption in meat samples are presented. This work demonstrates that the measurement of optical angular dependency of absorption in relation to the muscle fibers in muscle tissue has the potential of detecting structural damage to the sample for meat quality control purposes. Copyright © 2016 Elsevier Ltd. All rights reserved.

De-alloyed platinum nanoparticles

DOEpatents

Strasser, Peter [Houston, TX; Koh, Shirlaine [Houston, TX; Mani, Prasanna [Houston, TX; Ratndeep, Srivastava [Houston, TX

2011-08-09

A method of producing de-alloyed nanoparticles. In an embodiment, the method comprises admixing metal precursors, freeze-drying, annealing, and de-alloying the nanoparticles in situ. Further, in an embodiment de-alloyed nanoparticle formed by the method, wherein the nanoparticle further comprises a core-shell arrangement. The nanoparticle is suitable for electrocatalytic processes and devices.

Development of freeze dried vegetables

NASA Technical Reports Server (NTRS)

Larson, R. W.

1970-01-01

The development of freeze dried vegetables to be used in the Apollo food system is discussed. After the initial selection and screening of vegetables, several types of freeze dried vegetables were prepared in small batches. From these small batches, two vegetables were judged satisfactory for further testing and evaluation. These vegetables, mashed potatoes and asparagus, were subjected to storage at 100 deg plus or minus 5 F. for two weeks and then taste tested. The vegetables were also tested to determine if they complied with the microbiological requirements for Apollo food. The space food prototype production guide for the vegetables is submitted.

Corroboration of naringin effects on the intestinal absorption and pharmacokinetic behavior of candesartan cilexetil solid dispersions using in-situ rat models.

PubMed

Surampalli, Gurunath; K Nanjwade, Basavaraj; Patil, P A

2015-01-01

The aim of this study was to corroborate the effects of naringin, a P-glycoprotein inhibitor, on the intestinal absorption and pharmacokinetics of candesartan (CDS) from candesartan cilexetil (CAN) solid dispersions using in-situ rat models. Intestinal transport and absorption studies were examined by in-situ single pass perfusion and closed-loop models. We evaluated the intestinal membrane damage in the presence of naringin by measuring the release of protein and alkaline phosphatase (ALP). We noticed 1.47-fold increase in Peff of CDS from freeze-dried CAN-loaded solid dispersions with naringin (15 mg/kg, w/w) when compared with freeze-dried solid dispersion without naringin using in-situ single pass intestinal perfusion model. However, no intestinal membrane damage was observed in the presence of naringin. Our findings from in-situ closed-loop pharmacokinetic studies showed 1.34-fold increase in AUC with elevated Cmax and shortened tmax for freeze-dried solid dispersion with naringin as compared to freeze-dried solid dispersion without naringin. This study demonstrated that increased solubilization (favored by freeze-dried solid dispersion) and efflux pump inhibition (using naringin), the relative bioavailability of CDS can be increased, suggesting an alternative potential for improving oral bioavailability of CAN.

In Vitro Impact of Conditioned Medium From Demineralized Freeze-Dried Bone on Human Umbilical Endothelial Cells.

PubMed

Harnik, Branko; Miron, Richard J; Buser, Daniel; Gruber, Reinhard

2017-03-01

Angiogenesis is essential for the consolidation of bone allografts. The underlying molecular mechanism, however, remains unclear. Soluble factors released from demineralized freeze-dried bone target mesenchymal cells; however, their effect on endothelial cells has not been investigated so far. The aim of the present study was therefore to examine the effect of conditioned medium from demineralized freeze-dried bone on human umbilical endothelial cells in vitro. Conditioned medium was first prepared from demineralized freeze-dried bone following 24 hours incubation at room temperature to produce demineralized bone conditioned media. Thereafter, conditioned medium was used to stimulate human umbilical vein endothelial cells in vitro by determining the cell response based on viability, proliferation, expression of apoptotic genes, a Boyden chamber to determine cell migration, and the formation of branches. The authors report here that conditioned medium decreased viability and proliferation of endothelial cells. Neither of the apoptotic marker genes was significantly altered when endothelial cells were exposed to conditioned medium. The Boyden chamber revealed that endothelial cells migrate toward conditioned medium. Moreover, conditioned medium moderately stimulated the formation of branches. These findings support the concept that conditioned medium from demineralized freeze-dried bone targets endothelial cells by decreasing their proliferation and enhancing their motility under these in vitro conditions.

Use of manometric temperature measurement (MTM) and SMART freeze dryer technology for development of an optimized freeze-drying cycle.

PubMed

Gieseler, Henning; Kramer, Tony; Pikal, Michael J

2007-12-01

This report provides, for the first time, a summary of experiments using SMART Freeze Dryer technology during a 9 month testing period. A minimum ice sublimation area of about 300 cm(2) for the laboratory freeze dryer, with a chamber volume 107.5 L, was found consistent with data obtained during previous experiments with a smaller freeze dryer (52 L). Good reproducibility was found for cycle design with different type of excipients, formulations, and vials used. SMART primary drying end point estimates were accurate in the majority of the experiments, but showed an over prediction of primary cycle time when the product did not fully achieve steady state conditions before the first MTM measurement was performed. Product resistance data for 5% sucrose mixtures at varying fill depths were very reproducible. Product temperature determined by SMART was typically in good agreement with thermocouple data through about 50% of primary drying time, with significant deviations occurring near the end of primary drying, as expected, but showing a bias much earlier in primary drying for high solid content formulations (16.6% Pfizer product) and polyvinylpyrrolidone (40 kDa) likely due to water "re-adsorption" by the amorphous product during the MTM test. (c) 2007 Wiley-Liss, Inc.

SOS gene induction and possible mutagenic effects of freeze-drying in Escherichia coli and Salmonella typhimurium.

PubMed

Rosen, Rachel; Buchinger, Sebastian; Pfänder, Ramona; Pedhazur, Rami; Reifferscheid, Georg; Belkin, Shimshon

2016-11-01

We report the results of a study of the potential negative effects of the freeze-drying process, normally considered a benign means for long-term conservation of living cells and the golden standard in bacterial preservation. By monitoring gene induction using a whole-cell Escherichia coli bioreporter panel, in which diverse stress-responsive gene promoters are fused to luminescent or fluorescent reporting systems, we have demonstrated that DNA repair genes belonging to the SOS operon (recA, sulA, uvrA, umuD, and lexA) were induced upon resuscitation from the freeze-dried state, whereas other stress-responsive promoters such as grpE, katG, phoA, soxS, and sodA were not affected. This observation was confirmed by the UMU-chromotest (activation of the umuD gene promoter) in Salmonella typhimurium, as well as by real-time PCR analyses of selected E. coli SOS genes. We further show that a functional SOS operon is important in viability maintenance following resuscitation, but that at the same time, this repair system may introduce significantly higher mutation rates, comparable to those induced by high concentrations of a known mutagen. Our results also indicate that the entire freeze-drying process, rather than either freezing or drying separately, is instrumental in the induction of DNA damage.

Investigation of drying stresses on proteins during lyophilization: differentiation between primary and secondary-drying stresses on lactate dehydrogenase using a humidity controlled mini freeze-dryer.

PubMed

Luthra, Sumit; Obert, Jean-Philippe; Kalonia, Devendra S; Pikal, Michael J

2007-01-01

This article describes the design, performance testing, and application of a controlled humidity mini-freeze-dryer in studying the physical stability of lactate dehydrogenase during lyophilization. Performance evaluation of the mini-freeze-dryer was conducted with tests, namely water sublimation, radiation heat exchange, lowest achievable temperature, and leak testing. Protein stability studies were conducted by comparing protein activity at various stages of lyophilization with the initial activity. The shelf and condenser temperature were stable at <-40 degrees C, wall temperature was within 2 degrees C of the shelf temperature, and the leak rate was small. The chamber pressure was controlled by the ice on the condenser and the product temperature during sublimation was equal to the shelf temperature. Addition of Tween 80 prevented activity loss in solution and after freeze-thaw. No activity loss was observed after primary-drying even in absence of lyoprotectants and with collapse of cake structure. Five percent (w/w) sucrose concentration was required to achieve full stabilization. In conclusion, performance testing established that the mini-freeze-dryer was suitable for mechanistic freeze-drying studies. Secondary-drying was the critical step for protein stability. The concentration of sucrose required to stabilize the protein completely was several orders of magnitude higher than that required to satisfy the direct interaction requirement of the protein. (c) 2006 Wiley-Liss, Inc. and the American Pharmacists Association.

Atmospheric Spray Freeze-Drying: Numerical Modeling and Comparison With Experimental Measurements.

PubMed

Borges Sebastião, Israel; Robinson, Thomas D; Alexeenko, Alina

2017-01-01

Atmospheric spray freeze-drying (ASFD) represents a novel approach to dry thermosensitive solutions via sublimation. Tests conducted with a second-generation ASFD equipment, developed for pharmaceutical applications, have focused initially on producing a light, fine, high-grade powder consistently and reliably. To better understand the heat and mass transfer physics and drying dynamics taking place within the ASFD chamber, 3 analytical models describing the key processes are developed and validated. First, by coupling the dynamics and heat transfer of single droplets sprayed into the chamber, the velocity, temperature, and phase change evolutions of these droplets are estimated for actual operational conditions. This model reveals that, under typical operational conditions, the sprayed droplets require less than 100 ms to freeze. Second, because understanding the heat transfer throughout the entire freeze-drying process is so important, a theoretical model is proposed to predict the time evolution of the chamber gas temperature. Finally, a drying model, calibrated with hygrometer measurements, is used to estimate the total time required to achieve a predefined final moisture content. Results from these models are compared with experimental data. Copyright © 2016 American Pharmacists Association®. Published by Elsevier Inc. All rights reserved.

Effect of freeze-drying and self-ignition process on the microstructural and electrochemical properties of Li{sub 4}Ti{sub 5}O{sub 12}

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jamin, Claire; Traina, Karl; APTIS, Department of Physics, B5a, University of Liège, Sart-Tilman, 4000 Liège

2013-11-15

Graphical abstract: - Highlights: • Li{sub 4}Ti{sub 5}O{sub 12} is prepared by a method involving self-ignition of a freeze-dried gel. • Addition of NH{sub 4}NO{sub 3} modifies the self-ignition propagation mode. • Well-crystallized Li{sub 4}Ti{sub 5}O{sub 12} phase is obtained after only 2 h at 800 °C. • Li{sub 4}Ti{sub 5}O{sub 12} powder has 161 mAh g{sup −1} capacity and good retention at C/4 rate. - Abstract: Crystalline Li{sub 4}Ti{sub 5}O{sub 12} is synthesized by a method involving the freeze-drying and self-ignition of a gel prepared from titanium isopropoxide, lithium nitrate and hydroxypropylmethylcellulose (HPMC). This synthesis route yields crystalline Li{submore » 4}Ti{sub 5}O{sub 12} particles after calcination at 800 °C for 2 h. In an alternative route, addition of ammonium nitrate shifts the self-ignition mode from wave-like propagation to simultaneous. Powders with different microstructures are thereby obtained. Electrochemical characterization shows that the best results for Li{sup +} intercalation/desintercalation are obtained for the powder prepared without ammonium nitrate addition. These results highlight the necessity for a control of the self-ignition mode to obtain adequate properties.« less

Studies on target tissue distribution of ginsenosides and epimedium flavonoids in rats after intravenous administration of Jiweiling freeze-dried powder.

PubMed

Liu, Minyan; Wang, Hongtao; Zhao, Shaohua; Shi, Xiaowei; Zhang, Yongfeng; Xu, Honghui; Wang, Yufeng; Li, Xiangjun; Zhang, Lantong

2011-11-01

A simple and rapid liquid chromatography-mass spectrometry (LC-MS) method was developed and validated for analysis of ginsenoside Rb1, Rb2, Rc, Rd, Re, Rf, Rg1, icariin and epimedin A, B, C in rat target tissues (spinal cord, brain, muscle and sciatic nerve) after intravenous administration of Jiweiling freeze-dried powder using genistein as an internal standard (IS). The tissue samples were treated by protein precipitation with methanol prior to HPLC and chromatographic separation was performed on a C18 column utilizing a gradient elution program with acetonitrile and 0.1% formic acid aqueous. Electrospray ionization (ESI) source was employed and the 11 analytes and IS were detected by multiple reaction monitoring (MRM) scanning under the negative ionization mode. Higher sensitivity was achieved and the optimized mass transition ion-pairs (m/z) for quantitation were selected. The calibration curves were linear over the investigated concentration ranges with correlation coefficients higher than 0.995. The intra- and inter-day RSDs were all less than 10% with the relative error (RE) within ± 9.3%. The mean extraction recoveries for all compounds were between 93.3 and 106%. The proposed method was successfully applied to investigate the target tissue distribution of the 11 compounds in rat after intravenous administration of Jiweiling freeze-dried powder. Copyright © 2011 John Wiley & Sons, Ltd.

Enhanced dissolution and oral bioavailability of valsartan solid dispersions prepared by a freeze-drying technique using hydrophilic polymers.

PubMed

Xu, Wei-Juan; Xie, Hong-Juan; Cao, Qing-Ri; Shi, Li-Li; Cao, Yue; Zhu, Xiao-Yin; Cui, Jing-Hao

2016-01-01

This study aimed to improve the dissolution rate and oral bioavailability of valsartan (VAL), a poorly soluble drug using solid dispersions (SDs). The SDs were prepared by a freeze-drying technique with polyethylene glycol 6000 (PEG6000) and hydroxypropylmethylcellulose (HPMC 100KV) as hydrophilic polymers, sodium hydroxide (NaOH) as an alkalizer, and poloxamer 188 as a surfactant without using any organic solvents. In vitro dissolution rate and physicochemical properties of the SDs were characterized using the USP paddle method, differential scanning calorimetry (DSC), X-ray diffractometry (XRD) and Fourier transform-infrared (FT-IR) spectroscopy, respectively. In addition, the oral bioavailability of SDs in rats was evaluated by using VAL (pure drug) as a reference. The dissolution rates of the SDs were significantly improved at pH 1.2 and pH 6.8 compared to those of the pure drug. The results from DSC, XRD showed that VAL was molecularly dispersed in the SDs as an amorphous form. The FT-IR results suggested that intermolecular hydrogen bonding had formed between VAL and its carriers. The SDs exhibited significantly higher values of AUC 0-24 h and Cmax in comparison with the pure drug. In conclusion, hydrophilic polymer-based SDs prepared by a freeze-drying technique can be a promising method to enhance dissolution rate and oral bioavailability of VAL.

Quality properties and adsorption behavior of freeze-dried beef meat from the Biceps femoris and Semimembranosus muscles.

PubMed

Aykın, Elif; Erbaş, Mustafa

2016-11-01

The aim of this research was to determine the quality properties and adsorption behavior of freeze-dried beef meat from the Biceps femoris and Semimembranosus muscles. Most quality properties of both muscles were similar apart from total fat content. Freeze-dried meat pieces were kept in ten different equilibrium levels of relative humidity (2.0-97.3%) at 5, 15, 25 and 30°C. The experimental data were evaluated using BET (Brunauer-Emmett-Teller) and GAB (Guggenheim, Anderson and deBoer) models. The equilibrium moisture contents of freeze-dried Biceps femoris were lower than those of Semimembranosus at all water activities and temperature. The constants m0 and C of BET and GAB equations were determined to be between 6.27 and 8.07g/100g dry matter and 9.32-13.73, respectively. Constant k was about 0.90 at all temperatures, and the GAB equation exhibited a better fit to the experimental data of both muscles as a result of all %E values being approximately equal to 10%. Copyright © 2016 Elsevier Ltd. All rights reserved.

Effects of freezing, freeze drying and convective drying on in vitro gastric digestion of apples.

PubMed

Dalmau, Maria Esperanza; Bornhorst, Gail M; Eim, Valeria; Rosselló, Carmen; Simal, Susana

2017-01-15

The influence of processing (freezing at -196°C in liquid N2, FN sample; freeze-drying at -50°C and 30Pa, FD sample; and convective drying at 60°C and 2m/s, CD sample) on apple (var. Granny Smith) behavior during in vitro gastric digestion was investigated. Dried apples (FD and CD samples) were rehydrated prior to digestion. Changes in carbohydrate composition, moisture, soluble solids, acidity, total polyphenol content (TPC), and antioxidant activity (AA) of apple samples were measured at different times during digestion. Processing resulted in disruption of the cellular structure during digestion, as observed by scanning electron microscopy, light microscopy, and changes in carbohydrate composition. Moisture content increased (6-11% dmo), while soluble solids (55-78% dmo), acidity (44-72% dmo), total polyphenol content (30-61% dmo), and antioxidant activity (41-87%) decreased in all samples after digestion. Mathematical models (Weibull and exponential models) were used to better evaluate the influence of processing on apple behavior during gastric digestion. Copyright © 2016 Elsevier Ltd. All rights reserved.

Large scale synthesis of nanostructured zirconia-based compounds from freeze-dried precursors

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gomez, A.; Villanueva, R.; Vie, D.

2013-01-15

Nanocrystalline zirconia powders have been obtained at the multigram scale by thermal decomposition of precursors resulting from the freeze-drying of aqueous acetic solutions. This technique has equally made possible to synthesize a variety of nanostructured yttria or scandia doped zirconia compositions. SEM images, as well as the analysis of the XRD patterns, show the nanoparticulated character of those solids obtained at low temperature, with typical particle size in the 10-15 nm range when prepared at 673 K. The presence of the monoclinic, the tetragonal or both phases depends on the temperature of the thermal treatment, the doping concentration and themore » nature of the dopant. In addition, Rietveld refinement of the XRD profiles of selected samples allows detecting the coexistence of the tetragonal and the cubic phases for high doping concentration and high thermal treatment temperatures. Raman experiments suggest the presence of both phases also at relatively low treatment temperatures. - Graphical abstract: Zr{sub 1-x}A{sub x}O{sub 2-x/2} (A=Y, Sc; 0{<=}x{<=}0.12) solid solutions have been prepared as nanostructured powders by thermal decomposition of precursors obtained by freeze-drying, and this synthetic procedure has been scaled up to the 100 g scale. Highlights: Black-Right-Pointing-Pointer Zr{sub 1-x}A{sub x}O{sub 2-x/2} (A=Y, Sc; 0{<=}x{<=}0.12) solid solutions have been prepared as nanostructured powders. Black-Right-Pointing-Pointer The synthetic method involves the thermal decomposition of precursors obtained by freeze-drying. Black-Right-Pointing-Pointer The temperature of the thermal treatment controls particle sizes. Black-Right-Pointing-Pointer The preparation procedure has been scaled up to the 100 g scale. Black-Right-Pointing-Pointer This method is appropriate for the large-scale industrial preparation of multimetallic systems.« less

Preparation and characterization of nanoparticles of carboxymethyl cellulose acetate butyrate containing acyclovir

NASA Astrophysics Data System (ADS)

Vedula, Venkata Bharadwaz; Chopra, Maulick; Joseph, Emil; Mazumder, Sonal

2016-02-01

Nanoparticles of carboxymethyl cellulose acetate butyrate complexed with the poorly soluble antiviral drug acyclovir (ACV) were produced by precipitation process and the formulation process and properties of nanoparticles were investigated. Two different particle synthesis methods were explored—a conventional precipitation method and a rapid precipitation in a multi-inlet vortex mixer. The particles were processed by rotavap followed by freeze-drying. Particle diameters as measured by dynamic light scattering were dependent on the synthesis method used. The conventional precipitation method did not show desired particle size distribution, whereas particles prepared by the mixer showed well-defined particle size ~125-450 nm before and after freeze-drying, respectively, with narrow polydispersity indices. Fourier transform infrared spectroscopy showed chemical stability and intactness of entrapped drug in the nanoparticles. Differential scanning calorimetry showed that the drug was in amorphous state in the polymer matrix. ACV drug loading was around 10 wt%. The release studies showed increase in solution concentration of drug from the nanoparticles compared to the as-received crystalline drug.

Effects of four different drying methods on the carotenoid composition and antioxidant capacity of dried Gac peel.

PubMed

Chuyen, Hoang V; Roach, Paul D; Golding, John B; Parks, Sophie E; Nguyen, Minh H

2017-03-01

Gac fruit (Momordica cochinchinensis Spreng.) is a rich source of carotenoids for the manufacture of powder, oil and capsules for food, cosmetic and pharmaceutical uses. Currently, only the aril of the Gac fruit is processed and the peel, similar to the other components, is discarded, although it contains high level of carotenoids, which could be extracted for commercial use. In the present study, four different drying methods (hot-air, vacuum, heat pump and freeze drying), different temperatures and drying times were investigated for producing dried Gac peel suitable for carotenoid extraction. The drying methods and drying temperatures significantly affected the drying time, carotenoid content and antioxidant capacity of the dried Gac peel. Among the investigated drying methods, hot-air drying at 80  o C and vacuum drying at 50  o C produced dried Gac peel that exhibited the highest retention of carotenoids and the strongest antioxidant capacity. Hot-air drying at 80  o C and vacuum drying at 50  o C are recommended for the drying of Gac peel. © 2016 Society of Chemical Industry. © 2016 Society of Chemical Industry.

Microstructure of bentonite in iron ore green pellets.

PubMed

Bhuiyan, Iftekhar U; Mouzon, Johanne; Schröppel, Birgit; Kaech, Andres; Dobryden, Illia; Forsmo, Seija P E; Hedlund, Jonas

2014-02-01

Sodium-activated calcium bentonite is used as a binder in iron ore pellets and is known to increase strength of both wet and dry iron ore green pellets. In this article, the microstructure of bentonite in magnetite pellets is revealed for the first time using scanning electron microscopy. The microstructure of bentonite in wet and dry iron ore pellets, as well as in distilled water, was imaged by various imaging techniques (e.g., imaging at low voltage with monochromatic and decelerated beam or low loss backscattered electrons) and cryogenic methods (i.e., high pressure freezing and plunge freezing in liquid ethane). In wet iron ore green pellets, clay tactoids (stacks of parallel primary clay platelets) were very well dispersed and formed a voluminous network occupying the space available between mineral particles. When the pellet was dried, bentonite was drawn to the contact points between the particles and formed solid bridges, which impart strength to the solid compact.

DNA-based methodologies for the quantification of live and dead cells in formulated biocontrol products based on Pantoea agglomerans CPA-2.

PubMed

Soto-Muñoz, Lourdes; Torres, Rosario; Usall, Josep; Viñas, Inmaculada; Solsona, Cristina; Teixidó, Neus

2015-10-01

Pantoea agglomerans strain CPA-2 is an effective biocontrol agent (BCA) against the major postharvest pathogens present on pome and citrus fruits. Dehydration, such as freeze-drying, spray-drying and fluidized bed drying is one of the best ways to formulate BCAs. In this work, the survival of CPA-2 cells after formulation was determined by dilution plating and molecular methods as qPCR alone and combined with a sample pretreatment with a propidium monoazide dye (PMA-qPCR) and they were used to calculate treatment concentrations in efficacy trials on postharvest oranges. Furthermore, no significant differences in CPA-2 survival were observed as determined by dilution plating and PMA-qPCR after both the freeze drying and fluidized bed drying processes; however, an interesting significant difference was observed in the spray dried product comparing all quantitative methods. A difference of 0.48 and 2.17 log10 CFU or cells g/dw was observed among PMA-qPCR with qPCR and dilution plating, respectively. According to our study, dilution plating was shown to be an unreliable tool for monitoring the survival of CPA-2 after spray drying. In contrast, the combination of PMA and qPCR enabled a quick and unequivocal methodology to enumerate viable and VBNC CPA-2 cells under stress-dried conditions. Efficacy trials showed that, after 3 days, spray drying formulation rehydrated with 10% non-fat skimmed milk (NFSM) was as effective as fresh cells to control Penicillium digitatum in oranges. Copyright © 2015 Elsevier B.V. All rights reserved.

Inhalational system for Etoposide liposomes: formulation development and in vitro deposition.

PubMed

Parmar, J J; Singh, D J; Lohade, A A; Hegde, Darshana D; Soni, P S; Samad, A; Menon, Mala D

2011-11-01

Etoposide is a semisynthetic compound, widely used in treatment of non small cell lung cancer. However, frequent dosing and adverse effects remain a major concern in the use of etoposide. Liposomal systems for pulmonary drug delivery have been particularly attractive because of their compatibility with lung surfactant components. In the present investigation, pulmonary liposomal delivery system of etoposide was prepared by film hydration method. Various parameters were optimized with respect to entrapment efficiency as well as particle size of etoposide liposomes. For better shelf life of etoposide liposomes, freeze drying using trehalose as cryoprotectant was carried out. The liposomes were characterized for entrapment efficiency, particle size, surface topography, and in vitro drug release was carried out in simulated lung fluid at 37° at pH 7.4. The respirable or fine particle fraction was determined by using twin stage impinger. The stability study of freeze dried as well as aqueous liposomal systems was carried out at 2-8° and at ambient temperature (28±4°). The freeze dried liposomes showed better fine particle fraction and drug content over the period of six months at ambient as well as at 2-8° storage condition compared to aqueous dispersion of liposomes.

Doxycycline hydrochloride-metronidazole solid lipid microparticles gels for treatment of periodontitis: development, in-vitro and in-vivo clinical evaluation.

PubMed

Gad, Heba A; Kamel, Amany O; Ezzat, Ola M; El Dessouky, Hadir F; Sammour, Omaima A

2017-11-01

To formulate solid lipid microparticles (SLMs) encapsulating doxycycline hydrochloride (DH) and metronidazole (MT) for the treatment of periodontal diseases. SLMs were prepared applying hot homogenization method, using different types of lipids and stabilized with various types and concentrations of surfactants. The optimized formula was subjected to freeze-drying followed by incorporation into poloxamer gel. Microbiological and clinical evaluation of the selected SLMs on patients suffering from periodontal diseases was performed. SLMs could entrap high percentage of both drugs (81.14% and 68.75 % for doxycycline hydrochloride and metronidazole respectively). Transmission electron microscopy images of SLMs showed nearly spherical particles. Freeze-dried SLMs showed satisfactory stability for three months. Combined drugs were molecularly dispersed in SLMs. Incorporation of the freeze-dried SLMs powder in poloxamer gel could control the drugs release for 72 h. In-vivo study revealed effective and safe use of SLMs gel for periodontitis treatment. Significant improvement in both microbiological and clinical parameters was observed as compared to scaling and root planing alone. The formulated SLMs gel offers an applicable dosage form that can be injected directly into the periodontal pocket as adjunctive to scaling and root planing.

Evaluation of cryoanalysis as a tool for analyzing elemental distribution in "live" tardigrades using micro-PIXE

NASA Astrophysics Data System (ADS)

Nilsson, E. J. C.; Pallon, J.; Przybylowicz, W. J.; Wang, Y. D.; Jönsson, K. I.

2014-08-01

Although heavy on labor and equipment, thus not often applied, cryoanalysis of frozen hydrated biological specimens can provide information that better reflects the living state of the organism, compared with analysis in the freeze-dried state. In this paper we report a study where the cryoanalysis facility with cryosectioning capabilities at Materials Research Department, iThemba LABS, South Africa was employed to evaluate the usefulness of combining three ion beam analytical methods (μPIXE, RBS and STIM) to analyze a biological target where a better elemental compositional description is needed - the tardigrade. Imaging as well as quantification results are of interest. In a previous study, the element composition and redistribution of elements in the desiccated and active states of two tardigrade species was investigated. This study included analysis of both whole and sectioned tardigrades, and the aim was to analyze each specimen twice; first frozen hydrated and later freeze-dried. The combination of the three analytical techniques proved useful: elements from C to Rb in the tardigrades could be determined and certain differences in distribution of elements between the frozen hydrated and the freeze-dried states were observed. RBS on frozen hydrated specimens provided knowledge of matrix elements.

A study of the impact of freezing on the lyophilization of a concentrated formulation with a high fill depth.

PubMed

Liu, Jinsong; Viverette, Todd; Virgin, Marlin; Anderson, Mitch; Paresh, Dalal

2005-01-01

The objective of this study was to evaluate the impact of freezing on the lyophilization of a concentrated formulation with a high fill depth. A model system consisting of a 15-mL fill of 15% (w/w) sulfobutylether 7-beta-cyclodextrin (SBECD) solution in a 30-mL vial was selected for this study. Various freezing methods including single-step freezing, two-step freezing with a super-cooling holding, annealing, vacuum-induced freezing, changing ice habit using tert-butyl-alcohol (TBA), ice nucleation with silver iodide (AgI), as well as combinations of some of the methods, were used in the lyophilization of this model system. This work demonstrated that the freezing process had a significant impact on primary drying rate and product quality of a concentrated formulation with a high fill depth. Annealing, vacuum-induced freezing, and addition of either TBA or an ice nucleating agent (AgI) to the formulation accelerated the subsequent ice sublimation process. Two-step freezing or addition of TBA improved the product quality by eliminating vertical heterogeneity within the cake. The combination of two-step freezing in conjunction with an annealing step was shown to be a method of choice for freezing in the lyophilization of a product with a high fill depth. In addition to being an effective method of freezing, it is most applicable for scaling up. An alternative approach is to add a certain amount of TBA to the formulation, if the TBA-formulation interaction or regulatory concerns can be demonstrated as not being an issue. An evaluation of vial size performed in this study showed that although utilizing large-diameter vials to reduce the fill depth can greatly shorten the cycle time of a single batch, it will substantially decrease the product throughput in a large-scale freeze-dryer.

Challenges of biological sample preparation for SIMS imaging of elements and molecules at subcellular resolution

NASA Astrophysics Data System (ADS)

Chandra, Subhash

2008-12-01

Secondary ion mass spectrometry (SIMS) based imaging techniques capable of subcellular resolution characterization of elements and molecules are becoming valuable tools in many areas of biology and medicine. Due to high vacuum requirements of SIMS, the live cells cannot be analyzed directly in the instrument. The sample preparation, therefore, plays a critical role in preserving the native chemical composition for SIMS analysis. This work focuses on the evaluation of frozen-hydrated and frozen freeze-dried sample preparations for SIMS studies of cultured cells with a CAMECA IMS-3f dynamic SIMS ion microscope instrument capable of producing SIMS images with a spatial resolution of 500 nm. The sandwich freeze-fracture method was used for fracturing the cells. The complimentary fracture planes in the plasma membrane were characterized by field-emission secondary electron microscopy (FESEM) in the frozen-hydrated state. The cells fractured at the dorsal surface were used for SIMS analysis. The frozen-hydrated SIMS analysis of individual cells under dynamic primary ion beam (O 2+) revealed local secondary ion signal enhancements correlated with the water image signals of 19(H 3O) +. A preferential removal of water from the frozen cell matrix in the Z-axis was also observed. These complications render the frozen-hydrated sample type less desirable for subcellular dynamic SIMS studies. The freeze-drying of frozen-hydrated cells, either inside the instrument or externally in a freeze-drier, allowed SIMS imaging of subcellular chemical composition. Morphological evaluations of fractured freeze-dried cells with SEM and confocal laser scanning microscopy (CLSM) revealed well-preserved mitochondria, Golgi apparatus, and stress fibers. SIMS analysis of fractured freeze-dried cells revealed well-preserved chemical composition of even the most highly diffusible ions like K + and Na + in physiologically relevant concentrations. The high K-low Na signature in individual cells provided a rule-of-thumb criterion for the validation of sample preparation. The fractured freeze-dried cells allowed 3-D SIMS imaging and localization of 13C 15N labeled molecules and therapeutic drugs containing an elemental tag. Examples are shown to demonstrate that both diffusible elements and molecules are prone to artifact-induced relocation at subcellular scale if the sample preparation is compromised. The sample preparation is problem dependent and may vary widely between the diverse sample types of biological systems and the type of instrument used for SIMS analysis. The sample preparation, however, must be validated so that SIMS can be applied with confidence in biology and medicine.

The effect of dryer load on freeze drying process design.

PubMed

Patel, Sajal M; Jameel, Feroz; Pikal, Michael J

2010-10-01

Freeze-drying using a partial load is a common occurrence during the early manufacturing stages when insufficient amounts of active pharmaceutical ingredient (API) are available. In such cases, the immediate production needs are met by performing lyophilization with less than a full freeze dryer load. However, it is not obvious at what fractional load significant deviations from full load behavior begin. The objective of this research was to systematically study the effects of variation in product load on freeze drying behavior in laboratory, pilot and clinical scale freeze-dryers. Experiments were conducted with 5% mannitol (high heat and mass flux) and 5% sucrose (low heat and mass flux) at different product loads (100%, 50%, 10%, and 2%). Product temperature was measured in edge as well as center vials with thermocouples. Specific surface area (SSA) was measured by BET gas adsorption analysis and residual moisture was measured by Karl Fischer. In the lab scale freeze-dryer, the molar flux of inert gas was determined by direct flow measurement using a flowmeter and the molar flux of water vapor was determined by manometric temperature measurement (MTM) and tunable diode laser absorption spectroscopy (TDLAS) techniques. Comparative pressure measurement (capacitance manometer vs. Pirani) was used to determine primary drying time. For both 5% mannitol and 5% sucrose, primary drying time decreases and product temperature increases as the load on the shelves decreases. No systematic variation was observed in residual moisture and vapor composition as load decreased. Further, SSA data suggests that there are no significant freezing differences under different load conditions. Independent of dryer scale, among all the effects, variation in radiation heat transfer from the chamber walls to the product seems to be the dominant effect resulting in shorter primary drying time as the load on the shelf decreases (i.e., the fraction of edge vials increases).

Functionalised Silk Fibres

DTIC Science & Technology

2012-07-30

rubber moulds (14 x 5 x 6 mm; RL060, ProSciTech, QLD), frozen at -20ºC overnight, and placed in a freeze - dryer (FD355DMP, FTS Systems) for 24 hours...surface area, low volume materials: electrospun fibres and freeze -dried sponges (Figure 9). Each new material type is described in detail below...surface area materials generated from recombinant honeybee silk proteins. (A) Electrospun fibres, scale bar is 200 nm. (B) Freeze dried sponges

Summer Freezing Resistance: A Critical Filter for Plant Community Assemblies in Mediterranean High Mountains

PubMed Central

Pescador, David S.; Sierra-Almeida, Ángela; Torres, Pablo J.; Escudero, Adrián

2016-01-01

Assessing freezing community response and whether freezing resistance is related to other functional traits is essential for understanding alpine community assemblages, particularly in Mediterranean environments where plants are exposed to freezing temperatures and summer droughts. Thus, we characterized the leaf freezing resistance of 42 plant species in 38 plots at Sierra de Guadarrama (Spain) by measuring their ice nucleation temperature, freezing point (FP), and low-temperature damage (LT50), as well as determining their freezing resistance mechanisms (i.e., tolerance or avoidance). The community response to freezing was estimated for each plot as community weighted means (CWMs) and functional diversity (FD), and we assessed their relative importance with altitude. We established the relationships between freezing resistance, growth forms, and four key plant functional traits (i.e., plant height, specific leaf area, leaf dry matter content (LDMC), and seed mass). There was a wide range of freezing resistance responses and more than in other alpine habitats. At the community level, the CWMs of FP and LT50 responded negatively to altitude, whereas the FD of both traits increased with altitude. The proportion of freezing-tolerant species also increased with altitude. The ranges of FP and LT50 varied among growth forms, and only leaf dry matter content was negatively correlated with freezing-resistance traits. Summer freezing events represent important abiotic filters for assemblies of Mediterranean high mountain communities, as suggested by the CWMs. However, a concomitant summer drought constraint may also explain the high freezing resistance of species that thrive in these areas and the lower FD of freezing resistance traits at lower altitudes. Leaves with high dry matter contents may maintain turgor at lower water potential and enhance drought tolerance in parallel to freezing resistance. This adaptation to drought seems to be a general prerequisite for plants found in xeric mountains. PMID:26941761

Determination of free amino acids and 18 elements in freeze-dried strawberry and blueberry fruit using an Amino Acid Analyzer and ICP-MS with micro-wave digestion.

PubMed

Zhang, Hua; Wang, Zhen-Yu; Yang, Xin; Zhao, Hai-Tian; Zhang, Ying-Chun; Dong, Ai-Jun; Jing, Jing; Wang, Jing

2014-03-15

The objective of this study was to investigate the level of 18 trace elements of two freeze-dried samples from the Blueberry (Vaccinium corymbosum) and the Strawberry (Fragaria × Ananassa). The total free amino acid composition in the blueberry and strawberry was determined by an Amino Acid Analyzer. Eleven free amino acids were found in both berries. The trace elements in each dried fruit sample were determined by ICP-MS with microwave digestion. The linearity range of the standard curves was 0-1250.0 μg L(-1) (Mg, P, K, Ca),while in all cases, except for B, Na, Al, Cr, Mn, Fe, Ni, Cu, Zn, Se, Cd, Pb, Ge and As, which was 125.0 μg mL(-1), all related coefficients were above 0.9999; recovery was in the range of 79.0-106.8%. Minor concentrations of nutritional elements were found in each freeze-dried berry. In sum, the toxic trace element analysis found the content of toxic trace elements in each freeze-dried berry sample was safe for human consumption and that the overall quality of the blueberry surpassed that of the strawberry. The results certify that the two freeze-dried berries have potential for human consumption in value-added products and have a certain theoretical and practical significance. Crown Copyright © 2013. Published by Elsevier Ltd. All rights reserved.

Current Trends in Preservation Research and Development.

ERIC Educational Resources Information Center

Cunha, George Martin

1990-01-01

Overview of current trends in the preservation of library materials discusses collections conservation and management; climate control; insect and mold control; fire control; the effects of compact shelving; freezing and freeze-drying; space drying; alkaline paper; recycled paper; mass deacidification; and paper strengthening. (27 notes and…

Water-Hydrogel Binding Affinity Modulates Freeze-Drying-Induced Micropore Architecture and Skeletal Myotube Formation.

PubMed

Rich, Max H; Lee, Min Kyung; Marshall, Nicholas; Clay, Nicholas; Chen, Jinrong; Mahmassani, Ziad; Boppart, Marni; Kong, Hyunjoon

2015-08-10

Freeze-dried hydrogels are increasingly used to create 3D interconnected micropores that facilitate biomolecular and cellular transports. However, freeze-drying is often plagued by variance in micropore architecture based on polymer choice. We hypothesized that water-polymer binding affinity plays a significant role in sizes and numbers of micropores formed through freeze-drying, influencing cell-derived tissue quality. Poly(ethylene glycol)diacrylate (PEGDA) hydrogels with alginate methacrylate (AM) were used due to AM's higher binding affinity for water than PEGDA. PEGDA-AM hydrogels with larger AM concentrations resulted in larger sizes and numbers of micropores than pure PEGDA hydrogels, attributed to the increased mass of water binding to the PEGDA-AM gel. Skeletal myoblasts loaded in microporous PEGDA-AM hydrogels were active to produce 3D muscle-like tissue, while those loaded in pure PEGDA gels were localized on the gel surface. We propose that this study will be broadly useful in designing and improving the performance of various microporous gels.

High-density 3D graphene-based monolith and related materials, methods, and devices

DOEpatents

Worsley, Marcus A.; Baumann, Theodore F.; Biener, Juergen; Charnvanichborikarn, Supakit; Kucheyev, Sergei; Montalvo, Elizabeth; Shin, Swanee; Tylski, Elijah

2017-03-21

A composition comprising at least one high-density graphene-based monolith, said monolith comprising a three-dimensional structure of graphene sheets crosslinked by covalent carbon bonds and having a density of at least 0.1 g/cm.sup.3. Also provided is a method comprising: preparing a reaction mixture comprising a suspension and at least one catalyst, said suspension selected from a graphene oxide (GO) suspension and a carbon nanotube suspension; curing the reaction mixture to produce a wet gel; drying the wet gel to produce a dry gel, said drying step is substantially free of supercritical drying and freeze drying; and pyrolyzing the dry gel to produce a high-density graphene-based monolith. Exceptional combinations of properties are achieved including high conductive and mechanical properties.

Stability Studies of a Freeze-Dried Recombinant Human Epidermal Growth Factor Formulation for Wound Healing.

PubMed

Santana, Héctor; García, Gerardo; Vega, Maribel; Beldarraín, Alejandro; Páez, Rolando

2015-01-01

We report on the stability assessment of a recombinant human epidermal growth factor (rhEGF) freeze-dried formulation for wound healing by intra-lesional injections. The suitability of packaging material for the light protection of finished dried powder was evaluated after stressed exposure conditions. Degradation kinetics of powder for injection was investigated at concentrations of 25-250 μg/vial and temperatures of 45, 60, and 70 °C. The long-term stability was evaluated after storage at 25 ± 2 °C/60 ± 5% relative humidity (6 months) and 2-8 °C (24 months) in the dark and analyzed at several time points. The stability after reconstitution with various diluents was also assessed after 24 h storage at 2-8 °C. The rhEGF samples were analyzed for structural integrity by reversed-phase high-performance liquid chromatography (RP-HPLC), size-exclusion HPLC, and sodium dodecyl sulfate polyacrylamide gel electrophoresis (SDS-PAGE). Biological activity was investigated by measuring the cell proliferation in a murine fibroblast cell line. Results show that freeze-dried rhEGF in primary packaging only was photosensitive, as degradation by RP-HPLC that was completely suppressed by the secondary carton package was revealed. An increase in freeze-dried rhEGF stability was observed with the increase in protein concentration from 25 to 250 μg/vial. The long-term stability study showed no significant rhEGF degradation or physical change within the freeze-dried formulations containing 25 or 250 μg/vial of rhEGF. No physical, chemical or biological changes were observed for rhEGF after reconstitution in water for injection or 0.9% sodium chloride during the storage conditions studied. The stability of a recombinant human epidermal growth factor (rhEGF) freeze-dried formulation for wound healing by intra-lesional injections was assessed. The suitability of packaging material for the light protection of finished dried powder was evaluated after stressed exposure conditions. Degradation kinetics of powder for injection was investigated at concentrations of 25-250 μg/vial and temperatures of 45, 60, and 70 °C. The accelerated, long-term, and reconstitution stabilities were examined according to ICH guidelines for their utility time. The stability of rhEGF samples was analyzed by different chemical, physical, and biological activity assays. Results show that freeze-dried rhEGF in primary packaging only was photosensitive, as degradation by reversed-phase high performance liquid chromatography that was completely suppressed by the secondary carton package was revealed. An increase in freeze-dried rhEGF stability was observed with the increase in protein concentration. No significant rhEGF degradation or physical changes were observed within the freeze-dried formulations after 6 months storage at 25 ± 2 °C/60 ± 5% relative humidity or 24 months storage at 2-8 °C. No physical, chemical, or biological changes were observed for rhEGF after reconstitution in water for injection or 0.9% sodium chloride after 24 h storage at 2-8 °C. © PDA, Inc. 2015.

Microencapsulation of grape (Vitis labrusca var. Bordo) skin phenolic extract using gum Arabic, polydextrose, and partially hydrolyzed guar gum as encapsulating agents.

PubMed

Kuck, Luiza Siede; Noreña, Caciano Pelayo Zapata

2016-03-01

Bordo grape skin extract was microencapsulated by spray-drying and freeze-drying, using gum arabic (GA), partially hydrolyzed guar gum (PHGG), and polydextrose (PD) as encapsulating agents. Total phenolics and total monomeric anthocyanin, antioxidant activity, color, moisture, water activity (aw), solubility, hygroscopicity, glass transition temperature (Tg), particle size, and microstructure of the powders were evaluated. The retention of phenolics and anthocyanins ranged from 81.4% to 95.3%, and 80.8% to 99.6%, respectively, while the retention of antioxidant activity ranged from 45.4% to 83.7%. Treatments subjected to spray-drying had lower moisture, aw, and particle size, and greater solubility, while the freeze-dried samples were less hygroscopic. Tg values ranged from 10.1 to 52.2°C, and the highest values corresponded to the spray-dried microparticles. The spray-dried particles had spherical shape, while the freeze-dried powders showed irregular structures. The spray drying technique and the use of 5% PHGG and 5% PD has proven to be the best treatment. Copyright © 2015 Elsevier Ltd. All rights reserved.

A comprehensive laboratory study on the immersion freezing behavior of illite NX particles: a comparison of 17 ice nucleation measurement techniques

NASA Astrophysics Data System (ADS)

Hiranuma, N.; Augustin-Bauditz, S.; Bingemer, H.; Budke, C.; Curtius, J.; Danielczok, A.; Diehl, K.; Dreischmeier, K.; Ebert, M.; Frank, F.; Hoffmann, N.; Kandler, K.; Kiselev, A.; Koop, T.; Leisner, T.; Möhler, O.; Nillius, B.; Peckhaus, A.; Rose, D.; Weinbruch, S.; Wex, H.; Boose, Y.; DeMott, P. J.; Hader, J. D.; Hill, T. C. J.; Kanji, Z. A.; Kulkarni, G.; Levin, E. J. T.; McCluskey, C. S.; Murakami, M.; Murray, B. J.; Niedermeier, D.; Petters, M. D.; O'Sullivan, D.; Saito, A.; Schill, G. P.; Tajiri, T.; Tolbert, M. A.; Welti, A.; Whale, T. F.; Wright, T. P.; Yamashita, K.

2015-03-01

Immersion freezing is the most relevant heterogeneous ice nucleation mechanism through which ice crystals are formed in mixed-phase clouds. In recent years, an increasing number of laboratory experiments utilizing a variety of instruments have examined immersion freezing activity of atmospherically relevant ice-nucleating particles. However, an intercomparison of these laboratory results is a difficult task because investigators have used different ice nucleation (IN) measurement methods to produce these results. A remaining challenge is to explore the sensitivity and accuracy of these techniques and to understand how the IN results are potentially influenced or biased by experimental parameters associated with these techniques. Within the framework of INUIT (Ice Nuclei Research Unit), we distributed an illite-rich sample (illite NX) as a representative surrogate for atmospheric mineral dust particles to investigators to perform immersion freezing experiments using different IN measurement methods and to obtain IN data as a function of particle concentration, temperature (T), cooling rate and nucleation time. A total of 17 measurement methods were involved in the data intercomparison. Experiments with seven instruments started with the test sample pre-suspended in water before cooling, while 10 other instruments employed water vapor condensation onto dry-dispersed particles followed by immersion freezing. The resulting comprehensive immersion freezing data set was evaluated using the ice nucleation active surface-site density, ns, to develop a representative ns(T) spectrum that spans a wide temperature range (-37 °C < T < -11 °C) and covers 9 orders of magnitude in ns. In general, the 17 immersion freezing measurement techniques deviate, within a range of about 8 °C in terms of temperature, by 3 orders of magnitude with respect to ns. In addition, we show evidence that the immersion freezing efficiency expressed in ns of illite NX particles is relatively independent of droplet size, particle mass in suspension, particle size and cooling rate during freezing. A strong temperature dependence and weak time and size dependence of the immersion freezing efficiency of illite-rich clay mineral particles enabled the ns parameterization solely as a function of temperature. We also characterized the ns(T) spectra and identified a section with a steep slope between -20 and -27 °C, where a large fraction of active sites of our test dust may trigger immersion freezing. This slope was followed by a region with a gentler slope at temperatures below -27 °C. While the agreement between different instruments was reasonable below ~ -27 °C, there seemed to be a different trend in the temperature-dependent ice nucleation activity from the suspension and dry-dispersed particle measurements for this mineral dust, in particular at higher temperatures. For instance, the ice nucleation activity expressed in ns was smaller for the average of the wet suspended samples and higher for the average of the dry-dispersed aerosol samples between about -27 and -18 °C. Only instruments making measurements with wet suspended samples were able to measure ice nucleation above -18 °C. A possible explanation for the deviation between -27 and -18 °C is discussed. Multiple exponential distribution fits in both linear and log space for both specific surface area-based ns(T) and geometric surface area-based ns(T) are provided. These new fits, constrained by using identical reference samples, will help to compare IN measurement methods that are not included in the present study and IN data from future IN instruments.

A comprehensive laboratory study on the immersion freezing behavior of illite NX particles: a comparison of seventeen ice nucleation measurement techniques

NASA Astrophysics Data System (ADS)

Hiranuma, N.; Augustin-Bauditz, S.; Bingemer, H.; Budke, C.; Curtius, J.; Danielczok, A.; Diehl, K.; Dreischmeier, K.; Ebert, M.; Frank, F.; Hoffmann, N.; Kandler, K.; Kiselev, A.; Koop, T.; Leisner, T.; Möhler, O.; Nillius, B.; Peckhaus, A.; Rose, D.; Weinbruch, S.; Wex, H.; Boose, Y.; DeMott, P. J.; Hader, J. D.; Hill, T. C. J.; Kanji, Z. A.; Kulkarni, G.; Levin, E. J. T.; McCluskey, C. S.; Murakami, M.; Murray, B. J.; Niedermeier, D.; Petters, M. D.; O'Sullivan, D.; Saito, A.; Schill, G. P.; Tajiri, T.; Tolbert, M. A.; Welti, A.; Whale, T. F.; Wright, T. P.; Yamashita, K.

2014-08-01

Immersion freezing is the most relevant heterogeneous ice nucleation mechanism through which ice crystals are formed in mixed-phase clouds. In recent years, an increasing number of laboratory experiments utilizing a variety of instruments have examined immersion freezing activity of atmospherically relevant ice nucleating particles (INPs). However, an inter-comparison of these laboratory results is a difficult task because investigators have used different ice nucleation (IN) measurement methods to produce these results. A remaining challenge is to explore the sensitivity and accuracy of these techniques and to understand how the IN results are potentially influenced or biased by experimental parameters associated with these techniques. Within the framework of INUIT (Ice Nucleation research UnIT), we distributed an illite rich sample (illite NX) as a representative surrogate for atmospheric mineral dust particles to investigators to perform immersion freezing experiments using different IN measurement methods and to obtain IN data as a function of particle concentration, temperature (T), cooling rate and nucleation time. Seventeen measurement methods were involved in the data inter-comparison. Experiments with seven instruments started with the test sample pre-suspended in water before cooling, while ten other instruments employed water vapor condensation onto dry-dispersed particles followed by immersion freezing. The resulting comprehensive immersion freezing dataset was evaluated using the ice nucleation active surface-site density (ns) to develop a representative ns(T) spectrum that spans a wide temperature range (-37 °C < T < -11 °C) and covers nine orders of magnitude in ns. Our inter-comparison results revealed a discrepancy between suspension and dry-dispersed particle measurements for this mineral dust. While the agreement was good below ~ -26 °C, the ice nucleation activity, expressed in ns, was smaller for the wet suspended samples and higher for the dry-dispersed aerosol samples between about -26 and -18 °C. Only instruments making measurement techniques with wet suspended samples were able to measure ice nucleation above -18 °C. A possible explanation for the deviation between -26 and -18 °C is discussed. In general, the seventeen immersion freezing measurement techniques deviate, within the range of about 7 °C in terms of temperature, by three orders of magnitude with respect to ns. In addition, we show evidence that the immersion freezing efficiency (i.e., ns) of illite NX particles is relatively independent on droplet size, particle mass in suspension, particle size and cooling rate during freezing. A strong temperature-dependence and weak time- and size-dependence of immersion freezing efficiency of illite-rich clay mineral particles enabled the ns parameterization solely as a function of temperature. We also characterized the ns (T) spectra, and identified a section with a steep slope between -20 and -27 °C, where a large fraction of active sites of our test dust may trigger immersion freezing. This slope was followed by a region with a gentler slope at temperatures below -27 °C. A multiple exponential distribution fit is expressed as ns(T) = exp(23.82 × exp(-exp(0.16 × (T + 17.49))) + 1.39) based on the specific surface area and ns(T) = exp(25.75 × exp(-exp(0.13 × (T + 17.17))) + 3.34) based on the geometric area (ns and T in m-2 and °C, respectively). These new fits, constrained by using an identical reference samples, will help to compare IN measurement methods that are not included in the present study and, thereby, IN data from future IN instruments.

Characterization of konjac glucomannan-gelatin IPN physical hydrogel scaffold

NASA Astrophysics Data System (ADS)

Chen, Xiliang; Chen, Qinghua; Yan, Tingting; Liu, Jinkun

2017-06-01

A novel IPN hydrogel scaffold is prepared by freeze-drying method, in which konjac galactomannan (KGM) and gelatin are physically crosslinked respectively. This scaffold is thermostable, and the structure of this scaffold is analysed by scanning electron microscope, Fourier transform infrared spectrum, and X-ray diffraction method. The FT-IR results show that hydrogen bonds are formed between KGM and gelatin molecules, which hinder the formation of their respective crosslinking. This is consistent with the XRD results that the crystallinity gets lower in the IPN gels compared with pure gelatin and KGM gels. The morphologies of freeze-dried hydrogels are observed by SEM and the mechanical properties of the scaffolds are tested to analyse the relationship between the structures and properties. Although this novel IPN hydrogel is physical gel, it shows rubber-like performance as chemical gels. And it is nontoxic, so it can be used as the scaffold for cartilage tissue engineering that embedded in human bodies.

Optimization of cell disruption methods for efficient recovery of bioactive metabolites via NMR of three freshwater microalgae (chlorophyta).

PubMed

Ma, Nyuk Ling; Teh, Kit Yinn; Lam, Su Shiung; Kaben, Anne Marie; Cha, Thye San

2015-08-01

This study demonstrates the use of NMR techniques coupled with chemometric analysis as a high throughput data mining method to identify and examine the efficiency of different disruption techniques tested on microalgae (Chlorella variabilis, Scenedesmus regularis and Ankistrodesmus gracilis). The yield and chemical diversity from the disruptions together with the effects of pre-oven and pre-freeze drying prior to disruption techniques were discussed. HCl extraction showed the highest recovery of oil compounds from the disrupted microalgae (up to 90%). In contrast, NMR analysis showed the highest intensity of bioactive metabolites obtained for homogenized extracts pre-treated with freeze-drying, indicating that homogenizing is a more favorable approach to recover bioactive substances from the disrupted microalgae. The results show the potential of NMR as a useful metabolic fingerprinting tool for assessing compound diversity in complex microalgae extracts. Copyright © 2015 Elsevier Ltd. All rights reserved.

Structure influence on mechanical and acoustic properties of freeze-dried gels obtained with the use of hydrocolloids.

PubMed

Ciurzyńska, Agnieszka; Marzec, Agata; Mieszkowska, Arleta; Lenart, Andrzej

2017-04-01

The influence of the structure formed by the type of hydrocolloids (low-methoxyl pectin, the mixture of xanthan gum, and locust bean gum, and mixture of xanthan gum, and guar gum) and the aeration time (3, 5, 7, and 9 min) on textural properties of freeze-dried gels were investigated. The hardest texture generating the strongest acoustic emission was obtained by freeze-dried pectin gel, characterised by the lowest porosity and the largest pore diameter. Aeration time significantly affected mechanical and acoustic properties of the pectin gel lyophilisate. No effect of gel aeration time on tested characteristics of samples with mixture of hydrocolloids was observed. Strong positive correlations between acoustic energy as well as the maximum force and work and negative ones between porosity and pore diameter indicate that greater resilience and stronger acoustic emission of freeze-dried gels was caused by the reduction of porosity and the increase in the pore size of the material. The research is expected to show the phenomenon of structure formation when preparing and freeze-drying gels and explain the influence of the process parameters (time of aeration, the type of hydrocolloids) on the formation of the internal structure and physical properties of a dried product, especially mechanical and acoustic properties. This achievement will contribute to the development of the science of food and human nutrition, especially within the context of the popular research on aerated diet products. The expected result will be the ability to develop a new technology for producing food with a delicate texture, using the phenomenon of sublimation. As a result, designing changes in the structure of freeze-dried fruit gels with a delicate structure will be possible due to the choice of ingredients and aeration parameters in order to develop innovative food characterised by favorable nutritional, health and functional properties, which will be attractive for the consumers. © 2016 Wiley Periodicals, Inc.

Easy Meal

NASA Technical Reports Server (NTRS)

1978-01-01

The woman pictured below is sitting down to a nutritious, easily-prepared meal similar to those consumed by Apollo astronauts. The appetizing dishes shown were created simply by adding water to the contents of a Mountain House* Easy Meal package of freeze dried food. The Easy Meal line is produced by Oregon Freeze Dry Foods, Inc., Albany, Oreaon, a pioneer in freeze drying technology and a company long associated with NASA in developing suitable preparations for use on manned spacecraft. Designed to provide nutritionally balanced, attractive hot meals for senior adults, Easy Meal is an offshoot of a 1975-77 demonstration project managed by Johnson Space Center and called Meal System for the Elderly. The project sought ways to help the estimated 3.5 million elderly Americans who are unable to take advantage of existing meal programs. Such services are provided by federal, state and local agencies, but they are not available to many who live in rural areas, or others who are handicapped, temporarily ill or homebound for other reasons. Oregon Freeze Dry Foods was a participant in that multi-agency cooperative project. With its Easy Meal assortment of convenience foods pictured above left, the company is making commercially available meal packages similar to those distributed in the Meal System for the Elderly program. In the freeze drying process, water is extracted from freshly-cooked foods by dehydration at very low temperatures, as low as 50 I degrees below zero. Flavor is locked in by packaging the dried food in pouches which block out moisture and oxygen, the principal causes of food deterioration; thus the food can be stored for long periods without refrigeration. Meals are reconstituted by adding hot or cold water, depending on the type of food, and they are table ready in five to 10 minutes. Oregon Freeze Dry Foods offers five different meal packages and plans to expand the line.

Tomato is a highly effective vehicle for expression and oral immunization with Norwalk virus capsid protein.

PubMed

Zhang, Xiuren; Buehner, Norene A; Hutson, Anne M; Estes, Mary K; Mason, Hugh S

2006-07-01

Norwalk virus (NV) is an important agent of epidemic gastroenteritis, and an oral subunit vaccine shows potential for protection. Recombinant Norwalk virus (rNV) capsid protein expressed in plants assembles virus-like particles (VLPs) that are orally immunogenic in mice and humans. In this article we examine rNV expression in tomato and potato using a plant-optimized gene, and test the immunogenicity of dried tomato fruit and potato tuber fed to mice. The synthetic gene increased rNV expression fourfold in tomato and potato plants, which assembled VLP. Four doses of 0.4 g freeze-dried tomato fruit containing 64 microg rNV (40 microg VLPs) induced NV-specific serum IgG and mucosal IgA in > or = 80% of mice, while doses of 0.8 g elicited systemic and mucosal antibody responses in all mice. Feedings of 1 g freeze-dried potato tuber containing 120 microg rNV (90 microg VLPs) were required to produce 100% responsiveness. Oxidation of phenolic compounds upon rehydration of dried tuber caused significant VLP instability, thus decreasing immunogenicity. Air-dried tomato fruit stimulated stronger immune responses than freeze-dried fruit of the same mass, perhaps by limiting the destruction of plant cell matrix and membrane systems that occurs with freeze-drying. Thus, rNV in dried transgenic tomato fruit was a more potent immunogen than that in dried potato tubers, based on the total VLPs ingested. These findings support the use of stabilized, dried tomato fruit for oral delivery of subunit vaccines.

Robustness testing in pharmaceutical freeze-drying: inter-relation of process conditions and product quality attributes studied for a vaccine formulation.

PubMed

Schneid, Stefan C; Stärtzel, Peter M; Lettner, Patrick; Gieseler, Henning

2011-01-01

The recent US Food and Drug Administration (FDA) legislation has introduced the evaluation of the Design Space of critical process parameters in manufacturing processes. In freeze-drying, a "formulation" is expected to be robust when minor deviations of the product temperature do not negatively affect the final product quality attributes. To evaluate "formulation" robustness by investigating the effect of elevated product temperature on product quality using a bacterial vaccine solution. The vaccine solution was characterized by freeze-dry microscopy to determine the critical formulation temperature. A conservative cycle was developed using the SMART™ mode of a Lyostar II freeze dryer. Product temperature was elevated to imitate intermediate and aggressive cycle conditions. The final product was analyzed using X-ray powder diffraction (XRPD), scanning electron microscopy (SEM), Karl Fischer, and modulated differential scanning calorimetry (MDSC), and the life cell count (LCC) during accelerated stability testing. The cakes processed at intermediate and aggressive conditions displayed larger pores with microcollapse of walls and stronger loss in LCC than the conservatively processed product, especially during stability testing. For all process conditions, a loss of the majority of cells was observed during storage. For freeze-drying of life bacterial vaccine solutions, the product temperature profile during primary drying appeared to be inter-related to product quality attributes.

Antioxidant Activity, Total Phenolics Content, Anthocyanin, and Color Stability of Isotonic Model Beverages Colored with Andes Berry (Rubus glaucus Benth) Anthocyanin Powder

PubMed Central

Estupiñan, D.C.; Schwartz, S.J.; Garzón, G.A.

2013-01-01

The stability of anthocyanin (ACN) freeze-dried powders from Andes berry (Rubus glaucus Benth) as affected by storage, addition of maltodextrin as a carrier agent, and illumination was evaluated in isotonic model beverages. The ethanolic ACN extract was freeze dried with and without maltodextrin DE 20. Isotonic model beverages were colored with freeze-dried ACN powder (FDA), freeze-dried ACN powder with maltodextrin (MFDA), and red nr 40. Beverages were stored in the dark and under the effect of illumination. Half life of the ACNs, changes in color, total phenolics content (TPC), and antioxidant activity were analyzed for 71 d. Addition of maltodextrin and absence of light stabilized the color of beverages and improved ACN and TPC stability during storage. The antioxidant activity of the beverages was higher when they were colored with MFDA and highly correlated with ACN content. There was no correlation between antioxidant activity and TPC. It is concluded that addition of maltodextrin DE 20 as a carrier agent during freeze-drying improves the color and stability of nutraceutical antioxidants present in Andes berry extract. This suggests a protective enclosing of ACNs within a maltodextrin matrix with a resulting powder that could serve as a supplement or additive to naturally color and to enhance the antioxidant capacity of isotonic beverages. PMID:21535712

Antioxidant activity, total phenolics content, anthocyanin, and color stability of isotonic model beverages colored with Andes berry (Rubus glaucus Benth) anthocyanin powder.

PubMed

Estupiñan, D C; Schwartz, S J; Garzón, G A

2011-01-01

The stability of anthocyanin (ACN) freeze-dried powders from Andes berry (Rubus glaucus Benth) as affected by storage, addition of maltodextrin as a carrier agent, and illumination was evaluated in isotonic model beverages. The ethanolic ACN extract was freeze dried with and without maltodextrin DE 20. Isotonic model beverages were colored with freeze-dried ACN powder (FDA), freeze-dried ACN powder with maltodextrin (MFDA), and red nr 40. Beverages were stored in the dark and under the effect of illumination. Half life of the ACNs, changes in color, total phenolics content (TPC), and antioxidant activity were analyzed for 71 d. Addition of maltodextrin and absence of light stabilized the color of beverages and improved ACN and TPC stability during storage. The antioxidant activity of the beverages was higher when they were colored with MFDA and highly correlated with ACN content. There was no correlation between antioxidant activity and TPC. It is concluded that addition of maltodextrin DE 20 as a carrier agent during freeze-drying improves the color and stability of nutraceutical antioxidants present in Andes berry extract. This suggests a protective enclosing of ACNs within a maltodextrin matrix with a resulting powder that could serve as a supplement or additive to naturally color and to enhance the antioxidant capacity of isotonic beverages.

Evaluation of 3D-Printed Polycaprolactone Scaffolds Coated with Freeze-Dried Platelet-Rich Plasma for Bone Regeneration.

PubMed

Li, Junda; Chen, Meilin; Wei, Xiaoying; Hao, Yishan; Wang, Jinming

2017-07-19

Three-dimensional printing is one of the most promising techniques for the manufacturing of scaffolds for bone tissue engineering. However, a pure scaffold is limited by its biological properties. Platelet-rich plasma (PRP) has been shown to have the potential to improve the osteogenic effect. In this study, we improved the biological properties of scaffolds by coating 3D-printed polycaprolactone (PCL) scaffolds with freeze-dried and traditionally prepared PRP, and we evaluated these scaffolds through in vitro and in vivo experiments. In vitro, we evaluated the interaction between dental pulp stem cells (DPSCs) and the scaffolds by measuring cell proliferation, alkaline phosphatase (ALP) activity, and osteogenic differentiation. The results showed that freeze-dried PRP significantly enhanced ALP activity and the mRNA expression levels of osteogenic genes (ALP, RUNX2 (runt-related gene-2), OCN (osteocalcin), OPN (osteopontin)) of DPSCs ( p < 0.05). In vivo, 5 mm calvarial defects were created, and the PRP-PCL scaffolds were implanted. The data showed that compared with traditional PRP-PCL scaffolds or bare PCL scaffolds, the freeze-dried PRP-PCL scaffolds induced significantly greater bone formation ( p < 0.05). All these data suggest that coating 3D-printed PCL scaffolds with freeze-dried PRP can promote greater osteogenic differentiation of DPSCs and induce more bone formation, which may have great potential in future clinical applications.

Evaluation of analytical markers characterising different drying methods of parsley leaves (Petroselinum crispum L.).

PubMed

Lechtenberg, M; Zumdick, S; Gerhards, C; Schmidt, T J; Hensel, A

2007-12-01

Drying process of parsley leaves from Petroselinum crispum L. can influence the sensory qualities and aromatic taste of this herbal product. Beside oven-dried material, freeze-dried parsley is getting increasingly into the market. In the course of a search for analytical tools to differentiate oven-dried and lyophilised parsley, a HPLC determination of the 6"-O-malonylapiin to apiin ratio was shown to be a suitable marker system. While the ratio is high for fresh and lyophilised leave material, oven-drying leads to demalonylation and, subsequently, to a low malonylapiin--apiin ratio. Additionally, L*a*b colour measurement can be used for quality control to differentiate between different dried parsley raw materials.

Effect of freeze-dryer design on drying rate of an amorphous protein-formulation determined with a gravimetric technique.

PubMed

Gieseler, Henning; Lee, Geoffrey

2008-01-01

A freeze-drying balance was used to determine momentary drying-rate, m(t), of a sucrose/BSA formulation contained in a vial with varying shelf packing density, Ø2. A comparison between two different laboratory-scale freeze-dryers was made. The effects of Ø2 on m(t) differed between the two units, attributed to drying chamber design and its effects on heat transfer. At high Ø2 the differences are annulled because of the shielding effects of surrounding vials. Parallel effects of Ø2 were also found on product temperature, Tb, measured in the balance vial. Tb was used to calculate vial heat transfer coefficient, Kv. Kv was strongly reduced with increasing Ø2, but reached a plateau value at high Ø2.

Characteristics and functionality of appetite-reducing thylakoid powders produced by three different drying processes.

PubMed

Östbring, Karolina; Sjöholm, Ingegerd; Sörenson, Henrietta; Ekholm, Andrej; Erlanson-Albertsson, Charlotte; Rayner, Marilyn

2018-03-01

Thylakoids, a chloroplast membrane extracted from green leaves, are a promising functional ingredient with appetite-reducing properties via their lipase-inhibiting effect. Thylakoids in powder form have been evaluated in animal and human models, but no comprehensive study has been conducted on powder characteristics. The aim was to investigate the effects of different isolation methods and drying techniques (drum-drying, spray-drying, freeze-drying) on thylakoids' physicochemical and functional properties. Freeze-drying yielded thylakoid powders with the highest lipase-inhibiting capacity. We hypothesize that the specific macromolecular structures involved in lipase inhibition were degraded to different degrees by exposure to heat during spray-drying and drum-drying. We identified lightness (Hunter's L-value), greenness (Hunter's a-value), chlorophyll content and emulsifying capacity to be correlated to lipase-inhibiting capacity. Thus, to optimize the thylakoids functional properties, the internal membrane structure indicated by retained green colour should be preserved. This opens possibilities to use chlorophyll content as a marker for thylakoid functionality in screening processes during process optimization. Thylakoids are heat sensitive, and a mild drying technique should be used in industrial production. Strong links between physicochemical parameters and lipase inhibition capacity were found that can be used to predict functionality. The approach from this study can be applied towards production of standardized high-quality functional food ingredients. © 2017 Society of Chemical Industry. © 2017 Society of Chemical Industry.

Influence of Freeze-Drying and Oven-Drying Post Blanching on the Nutrient Composition of the Edible Insect Ruspolia differens

PubMed Central

Fombong, Forkwa Tengweh; Van Der Borght, Mik; Vanden Broeck, Jozef

2017-01-01

The longhorn grasshopper, Ruspolia differens (Serville), plays an important role as a food source across Sub-Saharan Africa, where it is consumed as a delicacy in both rural and urban areas. The effect of two drying methods (freeze-drying and oven-drying), employed after blanching, on the proximate, fatty acid and mineral composition of the two most common morphs was determined. Ruspolia differens grasshoppers were harvested in Uganda and Kenya from wild swarms during the rainy periods of November–December 2016. Based on cuticular coloration, we identified three morphs, green, brown and purple, which occurred at a ratio of 65:33:2, respectively. Results indicated that these insects have a high lipid content of 36%, as well as significant protein levels ranging between 33% and 46% dry matter. Oleic acid (44%) and palmitic acid (28%) were the two most abundant fatty acids; while the presence of arachidonic acid (0.6%) and docosahexaenoic acid (0.21%) suggests that Ruspolia differens is also a source of polyunsaturated fatty acids. The observed amino acid profile showed similar trends in all morphs, and all essential amino acids were present. Calcium (896–1035 mg/100 g), potassium (779–816 mg/100 g) and phosphorus (652–685 mg/100 g) were quite high among the minerals. The presence of the trace elements iron (217–220 mg/100 g), zinc (14.2–14.6 mg/100 g), manganese (7.4–8.3 mg/100 g) and copper (1.66 mg/100 g) suggests that inclusion of these grasshoppers in human diets may aid in combatting micronutrient deficiencies. Oven-drying Ruspolia differens delivered the same nutritional quality as freeze-drying. Hence, both drying approaches can be adequately used to formulate insect-based food products without noticeable nutritional changes. PMID:28926949

Optimization of a pharmaceutical freeze-dried product and its process using an experimental design approach and innovative process analyzers.

PubMed

De Beer, T R M; Wiggenhorn, M; Hawe, A; Kasper, J C; Almeida, A; Quinten, T; Friess, W; Winter, G; Vervaet, C; Remon, J P

2011-02-15

The aim of the present study was to examine the possibilities/advantages of using recently introduced in-line spectroscopic process analyzers (Raman, NIR and plasma emission spectroscopy), within well-designed experiments, for the optimization of a pharmaceutical formulation and its freeze-drying process. The formulation under investigation was a mannitol (crystalline bulking agent)-sucrose (lyo- and cryoprotector) excipient system. The effects of two formulation variables (mannitol/sucrose ratio and amount of NaCl) and three process variables (freezing rate, annealing temperature and secondary drying temperature) upon several critical process and product responses (onset and duration of ice crystallization, onset and duration of mannitol crystallization, duration of primary drying, residual moisture content and amount of mannitol hemi-hydrate in end product) were examined using a design of experiments (DOE) methodology. A 2-level fractional factorial design (2(5-1)=16 experiments+3 center points=19 experiments) was employed. All experiments were monitored in-line using Raman, NIR and plasma emission spectroscopy, which supply continuous process and product information during freeze-drying. Off-line X-ray powder diffraction analysis and Karl-Fisher titration were performed to determine the morphology and residual moisture content of the end product, respectively. In first instance, the results showed that - besides the previous described findings in De Beer et al., Anal. Chem. 81 (2009) 7639-7649 - Raman and NIR spectroscopy are able to monitor the product behavior throughout the complete annealing step during freeze-drying. The DOE approach allowed predicting the optimum combination of process and formulation parameters leading to the desired responses. Applying a mannitol/sucrose ratio of 4, without adding NaCl and processing the formulation without an annealing step, using a freezing rate of 0.9°C/min and a secondary drying temperature of 40°C resulted in efficient freeze-drying supplying end products with a residual moisture content below 2% and a mannitol hemi-hydrate content below 20%. Finally, using Monte Carlo simulations it became possible to determine how varying the factor settings around their optimum still leads to fulfilled response criteria, herewith having an idea about the probability to exceed the acceptable response limits. This multi-dimensional combination and interaction of input variables (factor ranges) leading to acceptable response criteria with an acceptable probability reflects the process design space. Copyright © 2010 Elsevier B.V. All rights reserved.

Kinetic Self-Assembly of DNA Tiles and Bricks

DTIC Science & Technology

2016-08-26

research, and educa- tion. This is achieved by freeze drying cell-free systems into paper and other porous substrates to create materials with the...different toehold switches on paper . Experiments were performed by freeze drying the recombinant PT7 expression system onto paper discs, along with linear...DNA encoding specific switch RNAs. The paper discs were rehy- drated with or without the complementary RNA trigger 24 hr after drying and then

Technological Development of Brewing in Domestic Refrigerator Using Freeze-Dried Raw Materials.

PubMed

Gialleli, Angelika-Ioanna; Ganatsios, Vassilios; Terpou, Antonia; Kanellaki, Maria; Bekatorou, Argyro; Koutinas, Athanasios A; Dimitrellou, Dimitra

2017-09-01

Development of a novel directly marketable beer brewed at low temperature in a domestic refrigerator combined with yeast immobilization technology is presented in this study. Separately, freeze-dried wort and immobilized cells of the cryotolerant yeast strain Saccharomyces cerevisiae AXAZ-1 on tubular cellulose were used in low-temperature fermentation (2, 5 and 7 °C). The positive effect of tubular cellulose during low-temperature brewing was examined, revealing that freeze-dried immobilized yeast cells on tubular cellulose significantly reduced the fermentation rates in contrast to freeze-dried free cells, although they are recommended for home-made beer production. Immobilization also enhanced the yeast resistance at low-temperature fermentation, reducing the minimum brewing temperature value from 5 to 2 °C. In the case of high-quality beer production, the effect of temperature and initial sugar concentration on the fermentation kinetics were assessed. Sensory enrichment of the produced beer was confirmed by the analysis of the final products, revealing a low diacetyl concentration, together with improved polyphenol content, aroma profile and clarity. The proposed process for beer production in a domestic refrigerator can easily be commercialized and applied by dissolving the content of two separate packages in tap water; one package containing dried wort and the other dried immobilized cells on tubular cellulose suspended in tap water.

Effects of drying process on the physicochemical properties of nopal cladodes at different maturity stages.

PubMed

Contreras-Padilla, Margarita; Gutiérrez-Cortez, Elsa; Valderrama-Bravo, María Del Carmen; Rojas-Molina, Isela; Espinosa-Arbeláez, Diego Germán; Suárez-Vargas, Raúl; Rodríguez-García, Mario Enrique

2012-03-01

Chemical proximate analysis was done in order to determine the changes of nutritional characteristics of nopal powders from three different maturity stages 50, 100, and 150 days and obtained by three different drying processes: freeze dried, forced air oven, and tunnel. Results indicate that nopal powder obtained by the process of freeze dried retains higher contents of protein, soluble fiber, and fat than the other two processes. Also, freeze dried process had less effect on color hue variable. No changes were observed in insoluble fiber content, chroma and lightness with the three different drying processes. Furthermore, the soluble fibers decreased with the age of nopal while insoluble fibers and ash content shows an opposite trend. In addition, the luminosity and hue values did not show differences among the maturity stages studied. The high content of dietary fibers of nopal pad powder could to be an interesting source of these important components for human diets and also could be used in food, cosmetics and pharmaceutical industry.

Effect of process technology on the nutritional, functional, and physical quality of grapefruit powder.

PubMed

Agudelo, C; Igual, M; Camacho, M M; Martínez-Navarrete, N

2017-01-01

The health properties of fruit are widely known. Powdered fruit may be a practical format to be offered to the consumer. Nevertheless, the process used to obtain the powder must ensure the maximum retention of the bioactive compounds and the functional value of the fruit while retaining adequate physical properties. The aim of this study was to compare freeze-drying and spray drying as the drying technologies to obtain grapefruit powder. The obtained results allow freeze-drying to be proposed as a better technology than spray drying in order to obtain a product with a higher content of vitamin C and total carotenoids. Moreover, all of the edible part of the fruit is used in this case, so a greater quantity of healthy compounds is preserved and by-product generation is avoided. Adding about 6 g water, 4 g Arabic gum and 0.6 g bamboo fibre/100 g grapefruit pulp is recommended before freeze-drying. © The Author(s) 2016.

Effect of different drying methods on chlorophyll, ascorbic acid and antioxidant compounds retention of leaves of Hibiscus sabdariffa L.

PubMed

Kumar, Sandopu Sravan; Manoj, Prabhakaran; Shetty, Nandini P; Giridhar, Parvatam

2015-07-01

Use of the indigenous, easily accessible leafy vegetable roselle (Hibiscus sabdariffa L.) for value addition is gaining impetus as its nutritive and nutraceutical compounds are exposed by investigations. Being a perishable, storage is challenging, hence different methods of drying have been an attractive alternative for its postharvest usage in foods without much compromising its quality and antioxidant potential. Room- and freeze-dried samples were found to have best quality in terms of colour, total flavonoid content (18.53 ± 2.39 and 18.66 ± 1.06 g kg(-1) respectively), total phenolic content (17.76 ± 1.93 and 18.91 ± 0.48 g kg(-1)), chlorophyll content (1.59 ± 0.001 and 1.55 ± 0.001 g kg(-1)) and ascorbic acid content (11.11 ± 1.04 and 8.92 ± 0.94 g kg(-1)) compared with those subjected to infrared, crossflow, microwave, oven or sun drying. Samples treated by room and freeze drying retained maximum antioxidant potential as shown by the phosphomolybdate method and the 2,2-diphenyl-1-picrylhydrazyl free radical-scavenging activity and ferric-reducing antioxidant power assays. Cold water and hot water extracts showed significantly higher total phenolic content and total antioxidant activity owing to the greater solubility of phenolics and destruction of cellular components in polar solvents than in organic solvents. The data obtained show the potential for retaining quality parameters of roselle leaf under suitable drying methods. © 2014 Society of Chemical Industry.

Antibacterial effect of citrus press-cakes dried by high speed and far-infrared radiation drying methods

PubMed Central

Samarakoon, Kalpa; Senevirathne, Mahinda; Lee, Won-Woo; Kim, Young-Tae; Kim, Jae-Il; Oh, Myung-Cheol

2012-01-01

In this study, the antibacterial effect was evaluated to determine the benefits of high speed drying (HSD) and far-infrared radiation drying (FIR) compared to the freeze drying (FD) method. Citrus press-cakes (CPCs) are released as a by-product in the citrus processing industry. Previous studies have shown that the HSD and FIR drying methods are much more economical for drying time and mass drying than those of FD, even though FD is the most qualified drying method. The disk diffusion assay was conducted, and the minimum inhibitory concentration (MIC) and minimum bactericidal concentration (MBC) were determined with methanol extracts of the dried CPCs against 11 fish and five food-related pathogenic bacteria. The disk diffusion results indicated that the CPCs dried by HSD, FIR, and FD prevented growth of all tested bacteria almost identically. The MIC and MBC results showed a range from 0.5-8.0 mg/mL and 1.0-16.0 mg/mL respectively. Scanning electron microscopy indicated that the extracts changed the morphology of the bacteria cell wall, leading to destruction. These results suggest that CPCs dried by HSD and FIR showed strong antibacterial activity against pathogenic bacteria and are more useful drying methods than that of the classic FD method in CPCs utilization. PMID:22808341

The application of A.C. impedance spectroscopy on the durability of hydrated cement paste subjected to various environmental conditions

NASA Astrophysics Data System (ADS)

Perron, Stacey

Harsh Canadian winters cause many problems in reinforced concrete structures due to damaging freezing-thawing cycles which is exacerbated by the heavy use of de-icing salts on roadways. Evaluation of concrete durability with current ASTM methods may give unreliable results and are destructive to the structure. A relatively new and novel approach to evaluating the durability of concrete uses A. C. Impedance Spectroscopy (ACIS). Hydrated cement paste (hcp), mortar, brick and vycor glass were evaluated using ACIS during drying-rewetting and freezing-thawing cycles. Thermal mechanical analysis (TMA), and differential scanning calorimetry (DSC) tests were also conducted and used as references. Results indicate that ACIS can be used to successfully evaluate the pore structure of hcp. The results from the drying-rewetting cycles are consistent with the pore coarsening theory. ACIS revealed pore structure changes consistent with the mechanical strains and pore solution chemistry. Increased pore continuity with each drying-rewetting cycle was indicated by a reduction in sample resistance. Unique tests were conducted on hydrated cement paste, mortar, brick and vycor glass that measured the ACIS and mechanical strains simultaneously while undergoing temperature changes. The temperature was lowered from 5°C to -80°C and then raised to +20°C. The ACIS results indicate that durability of the material can be assessed using the parameters R, material resistance, and phi, indicative of the frequency dispersion angle. The resistance on freezing values correlates with the amount of pore water freezing. The phi values on freezing are representative of the pore size distribution of the test sample. Resistance and phi data from freezing-thawing tests can be analyzed to assess durability of the sample. A material that is durable to freezing-thawing cycles can be described as having a high resistance at room temperature, a low freezing resistance and small changes in phi. Results were consistent among all the materials tested. Freezing-thawing tests were also conducted on specimens resaturated with salt solutions (5%, 10%, 15%). The results of these tests indicated a lower incipient freezing temperature, increase in pore blockage temperatures, and increased mobility of the pore water during freezing (increase in the change to phi). A series of test were conducted to evaluate the electrode polarization effects associated with the permittivity values at low frequencies. Teflon sheets were used to minimize the electrode polarization effects. It is shown that electrode polarization effects dominate over bulk polarization effects. Effects vary with the porosity of the material.

Optimization of a cryoprotective medium to increase the viability of freeze-dried Streptococcus thermophilus by response surface methodology

USDA-ARS?s Scientific Manuscript database

Streptococcus thermophilus normally exhibits different survival rates in different bacteria medium during freeze-drying. In this study, response surface methodology (RSM) was applied on the design of experiments for optimizing the cryoprotective medium. Results showed that the most significant facto...

Effect of different drying techniques on bioactive components, fatty acid composition, and volatile profile of robusta coffee beans.

PubMed

Dong, Wenjiang; Hu, Rongsuo; Chu, Zhong; Zhao, Jianping; Tan, Lehe

2017-11-01

This study investigated the effect of different drying techniques, namely, room-temperature drying (RTD), solar drying (SD), heat-pump drying (HPD), hot-air drying (HAD), and freeze drying (FD), on bioactive components, fatty acid composition, and the volatile compound profile of robusta coffee beans. The data showed that FD was an effective method to preserve fat, organic acids, and monounsaturated fatty acids. In contrast, HAD was ideal for retaining polyunsaturated fatty acids and amino acids. Sixty-two volatile compounds were identified in the differently dried coffee beans, representing 90% of the volatile compounds. HPD of the coffee beans produced the largest number of volatiles, whereas FD resulted in the highest volatile content. A principal component analysis demonstrated a close relationship between the HPD, SD, and RTD methods whereas the FD and HAD methods were significantly different. Overall, the results provide a basis for potential application to other similar thermal sensitive materials. Copyright © 2017 Elsevier Ltd. All rights reserved.

Modification of physical properties of freeze-dried rice

NASA Technical Reports Server (NTRS)

Huber, C. S.

1971-01-01

Freeze cycling process consists of alternately freezing and thawing precooked rice for two cycles, rice is then frozen and freeze-dehydrated in vacuum sufficient to remove water from rice by sublimitation. Process modifies rice grain structure and porosity, enabling complete rehydration in one minute in hot water.

Improvement of a dry formulation of Pseudomonas fluorescens EPS62e for fire blight disease biocontrol by combination of culture osmoadaptation with a freeze-drying lyoprotectant.

PubMed

Cabrefiga, J; Francés, J; Montesinos, E; Bonaterra, A

2014-10-01

To study the effect of lyoprotectants and osmoadaptation on viability of Pseudomonas fluorescens EPS62e during freeze-drying and storage and to evaluate the formulation in terms of efficacy in biocontrol and fitness on pear flowers. A wettable powder formulation of a biocontrol agent of fire blight was optimized by means of lyoprotectants and culture osmoadaptation. Freeze-drying was used to obtain dehydrated cells, and the best viability (70% of survival) was obtained using lactose as lyoprotectant. Survival during lyophilization was additionally improved using physiological adaptation of cells during cultivation under salt-amended medium (osmoadaptation). The procedure increased the survival of cells after freeze-drying attaining viability values close to a 100% in the lactose-formulated product (3 × 10(11) CFU g(-1) ), and through the storage period of 1 year at 4°C. The dry formulation showed also an improved biocontrol efficacy and survival of EPS62e on pear flowers under low relative humidity conditions. Cell viability after freeze-drying was improved using lactose as lyoprotectant combined with a procedure of osmoadaptation during cultivation. The powder-formulated product remained active for 12 months and retained biocontrol levels similar to that of fresh cells. The formulation showed an improved survival of EPS62e on flowers and an increase of the efficacy of biocontrol of fire blight at low relative humidity. The results have a potential value for commercial application in biocontrol agents not only of fire blight but also of other plant diseases. © 2014 The Society for Applied Microbiology.

Influence of deposition and spray pattern of nasal powders on insulin bioavailability.

PubMed

Pringels, E; Callens, C; Vervaet, C; Dumont, F; Slegers, G; Foreman, P; Remon, J P

2006-03-09

The influence of the deposition pattern and spray characteristics of nasal powder formulations on the insulin bioavailability was investigated in rabbits. The formulations were prepared by freeze drying a dispersion containing a physical mixture of drum dried waxy maize starch (DDWM)/Carbopol 974P (90/10, w/w) or a spray-dried mixture of Amioca starch/Carbopol 974P (25/75, w/w). The deposition in the nasal cavity of rabbits and in a silicone human nose model after actuation of three nasal delivery devices (Monopowder, Pfeiffer and experimental system) was compared and related to the insulin bioavailability. Posterior deposition of the powder formulation in the nasal cavity lowered the insulin bioavailability. To study the spray pattern, the shape and cross-section of the emitted powder cloud were analysed. It was concluded that the powder bulk density of the formulation influenced the spray pattern. Consequently, powders of different bulk density were prepared by changing the solid fraction of the freeze dried dispersion and by changing the freezing rate during freeze drying. After nasal delivery of these powder formulations no influence of the powder bulk density and of the spray pattern on the insulin bioavailability was observed.

A validated solid-liquid extraction method for the HPLC determination of polyphenols in apple tissues Comparison with pressurised liquid extraction.

PubMed

Alonso-Salces, Rosa M; Barranco, Alejandro; Corta, Edurne; Berrueta, Luis A; Gallo, Blanca; Vicente, Francisca

2005-02-15

A solid-liquid extraction procedure followed by reversed-phase high-performance liquid chromatography (RP-HPLC) coupled with a photodiode array detector (DAD) for the determination of polyphenols in freeze-dried apple peel and pulp is reported. The extraction step consists in sonicating 0.5g of freeze-dried apple tissue with 30mL of methanol-water-acetic acid (30:69:1, v/v/v) containing 2g of ascorbic acid/L, for 10min in an ultrasonic bath. The whole method was validated, concluding that it is a robust method that presents high extraction efficiencies (peel: >91%, pulp: >95%) and appropriate precisions (within day: R.S.D. (n = 5) <5%, and between days: R.S.D. (n = 5) <7%) at the different concentration levels of polyphenols that can be found in apple samples. The method was compared with one previously published, consisting in a pressurized liquid extraction (PLE) followed by RP-HPLC-DAD determination. The advantages and disadvantages of both methods are discussed.

Effects of euthanasia method on stable-carbon and stable-nitrogen isotope analysis for an ectothermic vertebrate.

PubMed

Atwood, Meredith A

2013-04-30

Stable isotope analysis is a critical tool for understanding ecological food webs; however, results can be sensitive to sample preparation methods. To limit the possibility of sample contamination, freezing is commonly used to euthanize invertebrates and preserve non-lethal samples from vertebrates. For destructive sampling of vertebrates, more humane euthanasia methods are preferred to freezing and it is essential to evaluate how these euthanasia methods affect stable isotope results. Stable isotope ratios and elemental composition of carbon and nitrogen were used to evaluate whether the euthanasia method compromised the integrity of the sample for analysis. Specifically, the stable isotope and C:N ratios were compared for larval wood frogs (Rana sylvatica  =  Lithobates sylvaticus), an ectothermic vertebrate, that had been euthanized by freezing with four different humane euthanasia methods: CO2, benzocaine, MS-222 (tricaine methanesulfonate), and 70% ethanol. The euthanasia method was not related to the δ(13)C or δ(15)N values and the comparisons revealed no differences between freezing and any of the other treatments. However, there were slight (non-significant) differences in the isotope ratios of benzocaine and CO2 when each was compared with freezing. The elemental composition was altered by the euthanasia method employed. The percentage nitrogen was higher in CO2 treatments than in freezing, and similar (non-significant) trends were seen for ethanol treatments relative to freezing. The resulting C:N ratios were higher for benzocaine treatments than for both CO2 and ethanol. Similar (non-significant) trends suggested that the C:N ratios were also higher for animals euthanized by freezing than for both CO2 and ethanol euthanasia methods. The euthanasia method had a larger effect on elemental composition than stable isotope ratios. The percentage nitrogen and the subsequent C:N ratios were most affected by the CO2 and ethanol euthanasia methods, whereas non-significant trends suggested that benzocaine and CO2 altered the stable isotope ratios. It appears that the use of MS-222 and freezing with dry ice are the most appropriate euthanasia methods for ectothermic vertebrates. Copyright © 2013 John Wiley & Sons, Ltd.

The effect of drying method temperature, collection method, and marker type on apparent ileal amino acid digestibility in 21-day-old broilers fed corn-soybean meal-barley based diet.

PubMed

Olojede, O C; Ford, M J; Jacob, J P; Ao, T; Pescatore, A J; Adedokun, S A

2018-06-01

For accurate estimation of nutrient digestibility, an ideal drying and sampling method is required to preserve the quality of the digesta. A standard corn-soybean meal (corn-SBM) broiler starter diet was fed from d 0 to 10 before birds were placed on the experimental diets until d 21. One hundred and sixty-eight male Cobb 500 broiler chicks were used to evaluate the effect of two drying methods (freeze-dryer vs. forced air-oven) and two drying temperatures (40 vs. 55°C) (Exp 1), while ninety-six chicks were used to evaluate the effect of flushing and squeezing as well as marker types (titanium vs. chromium) on apparent ileal DM, N, Ca, P, and AA digestibility (Exp 2). There were seven (Exp 1) or eight (Exp 2) replicate cages per treatment with 6 birds/cage. Digesta from the distal two thirds of the ileum was obtained from birds following euthanasia on d 21 by squeezing (Exp 1) and squeezing or flushing (Exp 2). Samples collected were stored in the freezer at -20°C until they were either freeze-dried (FD) or oven-dried (OD) at 40 or 55°C. There were no interactions between the drying methods and drying temperatures (Exp 1) on apparent ileal DM, N, and AA digestibility. Met had the highest (92.3%) while Cys had the lowest (73.8%) digestibility value. In Exp 2, no interaction between sampling methods and marker types was observed. The effect of sampling methods was not significant except for Arg and Met where squeezing resulted in higher (P < 0.05) digestibility values. Furthermore, apparent ileal His, Ile, Cys, Ser, and Tyr digestibility tended to be higher (P < 0.1) in squeezed digesta compared to the flushed digesta. Results from these studies showed that OD ileal digesta at 40 or 55°C had no negative effect on apparent ileal AA digestibility. Likewise, marker type did not influence apparent ileal AA digestibility values.

Moisture transfer from stopper to product and resulting stability implications.

PubMed

Pikal, M J; Shah, S

1992-01-01

Since the stability of a freeze-dried product is often sensitive to the level of moisture, control of residual moisture by attention to the secondary drying phase of the freeze-drying process is of considerable importance. However, several reports in the literature as well as our own experience suggest that low residual moisture immediately after manufacture does not ensure low moisture throughout the shelf life of the product. Equilibration of the product with moisture in the stopper can lead to significant increases in product water content. This research is a study of the kinetic and equilibrium aspects of moisture transfer from stopper to product at 5 degrees C, 25 degrees C, and 40 degrees C for two amorphous materials: vancomycin (highly hygroscopic) and lactose (moderately hygroscopic). Stoppers are 13 mm butyl rubber (#1816, West Co.) slotted freeze-drying stoppers which were studied: (a) "U"-with no treatment; (b) "SV1"-steam-sterilized followed by 1 hr vacuum drying; and (c) "SV8"-steam sterilized followed by 8 hrs vacuum drying. No evidence was found for moisture transmission through the stopper. Rather, the product moisture content increases with time and reaches an apparent equilibrium value characteristic of the product, amount of product, and stopper treatment method ("SV1" much greater than "U" greater than "SV1"). As a first approximation, the rate of approach to "equilibrium" depends only on temperature (t1/2 approximately 10 months at 5 degrees C to approximately 4 days at 40 degrees C) with the "equilibrium" water content being independent of temperature. The "equilibrium" moisture content increases as the dose decreases and is larger for vancomycin than for lactose. The "equilibrium" moisture contents range from 5.0% (25 mg vancomycin, "SV1" stoppers) to 0.68% (100 mg lactose, "SV8" stoppers).

Effects of drying processes on starch-related physicochemical properties, bioactive components and antioxidant properties of yam flours.

PubMed

Chen, Xuetao; Li, Xia; Mao, Xinhui; Huang, Hanhan; Wang, Tingting; Qu, Zhuo; Miao, Jing; Gao, Wenyuan

2017-06-01

The effects of five different drying processes, air drying (AD), sulphur fumigation drying (SFD), hot air drying (HAD), freeze drying (FD) and microwave drying (MWD) for yams in terms of starch-related properties and antioxidant activity were studied. From the results of scanning electron microscopy (SEM), polarized optical microscopy (POM), X-ray diffraction (XRD), and Fourier transform infrared (FT-IR), the MWD sample was found to contain gelatinized starch granules. The FD yam had more slow digestible (SDS) and resistant starches (RS) compared with those processed with other modern drying methods. The bioactive components and the reducing power of the dried yams, were lower than those of fresh yam. When five dried samples were compared by principal component analysis, the HAD and SFD samples were observed to have the highest comprehensive principal component values. Based on our results, HAD would be a better method for yam drying than the more traditional SFD. Copyright © 2016 Elsevier Ltd. All rights reserved.

Effect of drying procedures on the physicochemical properties and antioxidant activities of polysaccharides from Crassostrea gigas

PubMed Central

Zheng, Yaxu; Qu, Min; Jin, Qiao; Tong, Changqing

2017-01-01

Crassostrea gigas polysaccharides (CGP) were obtained by different drying methods: freeze-drying (FD), spray-drying (SD) or rotary evaporation-drying (RED). The physicochemical properties of CGP were evaluated on the basis of polysaccharide content, protein content, color characteristics, FT-IR spectroscopy, differential scanning calorimetry (DSC), and scanning electron microscopy (SEM). Antioxidant activities were researched three different free radicals, including DPPH free radicals, ABTS free radicals and reducing power. The results demonstrated that FDCGP, SDCGP and REDCGP have different physicochemical properties and antioxidant activities. Contrasted with FDCGP and REDCGP, SDCGP exhibited stronger antioxidant abilities. Therefore, considering the polysaccharides appearances and antioxidant activities, the spray drying method is a decent selection for the preparation of such polysaccharides, and it should be selected for application in the food industry. PMID:29176846

Preserving elemental content in adherent mammalian cells for analysis by synchrotron-based x-ray fluorescence microscopy

DOE PAGES

Jin, Qiaoling; Paunesku, Tatjana; Lai, Barry; ...

2016-08-31

Trace metals play important roles in biological function, and x-ray fluorescence microscopy (XFM) provides a way to quantitatively image their distribution within cells. The faithfulness of these measurements is dependent on proper sample preparation. Using mouse embryonic fibroblast NIH/3T3 cells as an example, we compare various approaches to the preparation of adherent mammalian cells for XFM imaging under ambient temperature. Direct side-by-side comparison shows that plunge-freezing-based cryoimmobilization provides more faithful preservation than conventional chemical fixation for most biologically important elements including P, S, Cl, K, Fe, Cu, Zn and possibly Ca in adherent mammalian cells. Although cells rinsed with freshmore » media had a great deal of extracellular background signal for Cl and Ca, this approach maintained cells at the best possible physiological status before rapid freezing and it does not interfere with XFM analysis of other elements. If chemical fixation has to be chosen, the combination of 3% paraformaldehyde and 1.5 % glutaraldehyde preserves S, Fe, Cu and Zn better than either fixative alone. Lastly, when chemically fixed cells were subjected to a variety of dehydration processes, air drying was proved to be more suitable than other drying methods such as graded ethanol dehydration and freeze drying. This first detailed comparison for x-ray fluorescence microscopy shows how detailed quantitative conclusions can be affected by the choice of cell preparation method.« less

Preserving elemental content in adherent mammalian cells for analysis by synchrotron-based x-ray fluorescence microscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jin, Qiaoling; Paunesku, Tatjana; Lai, Barry

Trace metals play important roles in biological function, and x-ray fluorescence microscopy (XFM) provides a way to quantitatively image their distribution within cells. The faithfulness of these measurements is dependent on proper sample preparation. Using mouse embryonic fibroblast NIH/3T3 cells as an example, we compare various approaches to the preparation of adherent mammalian cells for XFM imaging under ambient temperature. Direct side-by-side comparison shows that plunge-freezing-based cryoimmobilization provides more faithful preservation than conventional chemical fixation for most biologically important elements including P, S, Cl, K, Fe, Cu, Zn and possibly Ca in adherent mammalian cells. Although cells rinsed with freshmore » media had a great deal of extracellular background signal for Cl and Ca, this approach maintained cells at the best possible physiological status before rapid freezing and it does not interfere with XFM analysis of other elements. If chemical fixation has to be chosen, the combination of 3% paraformaldehyde and 1.5 % glutaraldehyde preserves S, Fe, Cu and Zn better than either fixative alone. Lastly, when chemically fixed cells were subjected to a variety of dehydration processes, air drying was proved to be more suitable than other drying methods such as graded ethanol dehydration and freeze drying. This first detailed comparison for x-ray fluorescence microscopy shows how detailed quantitative conclusions can be affected by the choice of cell preparation method.« less

Freeze Technology for Nuclear Applications - 13590

DOE Office of Scientific and Technical Information (OSTI.GOV)

Rostmark, Susanne C.; Knutsson, Sven; Lindberg, Maria

2013-07-01

Freezing of soil materials is a complicated process of a number of physical processes: - freezing of pore water in a thermal gradient, - cryogenic suction causing water migration and - ice formation expanding pores inducing frost heave. Structural changes due to increase of effective stress during freezing also take place. The over consolidation gives a powerful dewatering/drying effect and the freeze process causes separation of contaminates. Artificial ground freezing (AGF is a well established technique first practiced in south Wales, as early as 1862. AGF is mostly used to stabilize tunnels and excavations. During the last ten years underwatermore » applications of freeze technologies based on the AGF have been explored in Sweden. The technology can, and has been, used in many different steps in a remediation action. Freeze Sampling where undisturbed samples are removed in both soft and hard sediment/sludge, Freeze Dredging; retrieval of sediment with good precision and minimal redistribution, and Freeze Drying; volume reduction of contaminated sludge/sediment. The application of these technologies in a nuclear or radioactive environment provides several advantages. Sampling by freezing gives for example an advantage of an undisturbed sample taken at a specified depth, salvaging objects by freezing or removal of sludges is other applications of this, for the nuclear industry, novel technology. (authors)« less

Graphene oxide for acid catalyzed-reactions: Effect of drying process

NASA Astrophysics Data System (ADS)

Gong, H. P.; Hua, W. M.; Yue, Y. H.; Gao, Z.

2017-03-01

Graphene oxides (GOs) were prepared by Hummers method through various drying processes, and characterized by XRD, SEM, FTIR, XPS and N2 adsorption. Their acidities were measured using potentiometric titration and acid-base titration. The catalytic properties were investigated in the alkylation of anisole with benzyl alcohol and transesterification of triacetin with methanol. GOs are active catalysts for both reaction, whose activity is greatly affected by their drying processes. Vacuum drying GO exhibits the best performance in transesterification while freezing drying GO is most active for alkylation. The excellent catalytic behavior comes from abundant surface acid sites as well as proper surface functional groups, which can be obtained by selecting appropriate drying process.

THE INTRARENAL DISTRIBUTION OF TRITIATED PARA-AMINOHIPPURIC ACID DETERMINED BY A MODIFIED TECHNIQUE OF SECTION FREEZE-DRY RADIOAUTOGRAPHY

PubMed Central

Bordier, Betrand; Ornstein, Leonard; Wedeen, Richard P.

1970-01-01

Section freeze-dry radioautography has been used to examine the intrarenal distribution of a water-soluble organic acid (para-aminohippuric acid (PAH-3H)) under constant-infusion, steady-state conditions in mouse and rat kidney in vivo. The technique described here has the following advantages: (a) Sectioning and freeze-drying are accomplished in a closed cryostat at temperatures below -40°C; (b) Handling of the section is facilitated by mounting of the section-to-be on adhesive-coated Saran Wrap prior to cutting; (c) Unembedded freeze-dried sections are attached to photographic film at ambient temperature in the dark room; (d) Fixation follows completion of radioautographic exposure and precedes photographic development; (e) Permanent close contact is maintained between tissue and film. Morphologic preservation compared favorably with that obtained by optimal fixation techniques, which, however, permit diffusion. Cellular accumulation of PAH-3H during secretion was demonstrated in the proximal tubule under steady-state conditions in vivo. The cellular concentration of PAH-3H was uniform throughout the length of the proximal tubule in mouse and rat kidney. PMID:4349130

Self-healing Characteristics of Collagen Coatings with Respect to Surface Abrasion

PubMed Central

Kim, Chang-Lae; Kim, Dae-Eun

2016-01-01

A coating based on collagen with self-healing properties was developed for applications in mechanical components that are prone to abrasion due to contact with a counter surface. The inherent swelling behavior of collagen in water was exploited as the fundamental mechanism behind self-healing of a wear scar formed on the surface. The effects of freeze-drying process and water treatment of the collagen coatings on their mechanical and self-healing properties were analyzed. Water was also used as the medium to trigger the self-healing effect of the collagen coatings after the wear test. It was found that collagen coatings without freeze-drying did not demonstrate any self-healing effect whereas the coatings treated by freeze-drying process showed remarkable self-healing effect. Overall, collagen coatings that were freeze-dried and water treated showed the best friction and self-healing properties. Repeated self-healing ability of these coatings with respect to wear scar was also demonstrated. It was also confirmed that the self-healing property of the collagen coating was effective over a relatively wide range of temperature. PMID:27010967

Self-healing Characteristics of Collagen Coatings with Respect to Surface Abrasion

NASA Astrophysics Data System (ADS)

Kim, Chang-Lae; Kim, Dae-Eun

2016-03-01

A coating based on collagen with self-healing properties was developed for applications in mechanical components that are prone to abrasion due to contact with a counter surface. The inherent swelling behavior of collagen in water was exploited as the fundamental mechanism behind self-healing of a wear scar formed on the surface. The effects of freeze-drying process and water treatment of the collagen coatings on their mechanical and self-healing properties were analyzed. Water was also used as the medium to trigger the self-healing effect of the collagen coatings after the wear test. It was found that collagen coatings without freeze-drying did not demonstrate any self-healing effect whereas the coatings treated by freeze-drying process showed remarkable self-healing effect. Overall, collagen coatings that were freeze-dried and water treated showed the best friction and self-healing properties. Repeated self-healing ability of these coatings with respect to wear scar was also demonstrated. It was also confirmed that the self-healing property of the collagen coating was effective over a relatively wide range of temperature.

Freeze substitution in 3 hours or less.

PubMed

McDonald, K L; Webb, R I

2011-09-01

Freeze substitution is a process for low temperature dehydration and fixation of rapidly frozen cells that usually takes days to complete. New methods for freeze substitution have been developed that require only basic laboratory tools: a platform shaker, liquid nitrogen, a metal block with holes for cryotubes and an insulated container such as an ice bucket. With this equipment, excellent freeze substitution results can be obtained in as little as 90 min for cells of small volume such as bacteria and tissue culture cells. For cells of greater volume or that have significant diffusion barriers such as cuticles or thick cell walls, one can extend the time to 3 h or more with dry ice. The 3-h method works well for all manner of specimens, including plants and Caenorhabditis elegans as well as smaller samples. Here, we present the basics of the techniques and some results from Nicotiana leaves, C. elegans adult worms, Escherichia coli and baby hamster kidney tissue culture cells. © 2011 The Authors Journal of Microscopy © 2011 Royal Microscopical Society.

Switchable hydrophilicity solvents for lipid extraction from microalgae for biofuel production.

PubMed

Boyd, Alaina R; Champagne, Pascale; McGinn, Patrick J; MacDougall, Karen M; Melanson, Jeremy E; Jessop, Philip G

2012-08-01

A switchable hydrophilicity solvent (SHS) was studied for its effectiveness at extracting lipids from freeze-dried samples of Botryococcus braunii microalgae. The SHS N,N-dimethylcyclohexylamine extracted up to 22 wt.% crude lipid relative to the freeze-dried cell weight. The solvent was removed from the extract with water saturated with carbon dioxide at atmospheric pressure and recovered from the water upon de-carbonation of the mixture. Liquid chromatography-mass spectrometry (LC-MS) showed that the extracted lipids contained high concentrations of long chain tri-, di- and mono-acylglycerols, no phospholipids, and only 4-8% of residual solvent. Unlike extractions with conventional organic solvents, this new method requires neither distillation nor the use of volatile, flammable or chlorinated organic solvents. Copyright © 2012 Elsevier Ltd. All rights reserved.

Inhalational System for Etoposide Liposomes: Formulation Development and In Vitro Deposition

PubMed Central

Parmar, J. J.; Singh, D. J.; Lohade, A. A.; Hegde, Darshana D.; Soni, P. S.; Samad, A.; Menon, Mala D.

2011-01-01

Etoposide is a semisynthetic compound, widely used in treatment of non small cell lung cancer. However, frequent dosing and adverse effects remain a major concern in the use of etoposide. Liposomal systems for pulmonary drug delivery have been particularly attractive because of their compatibility with lung surfactant components. In the present investigation, pulmonary liposomal delivery system of etoposide was prepared by film hydration method. Various parameters were optimized with respect to entrapment efficiency as well as particle size of etoposide liposomes. For better shelf life of etoposide liposomes, freeze drying using trehalose as cryoprotectant was carried out. The liposomes were characterized for entrapment efficiency, particle size, surface topography, and in vitro drug release was carried out in simulated lung fluid at 37° at pH 7.4. The respirable or fine particle fraction was determined by using twin stage impinger. The stability study of freeze dried as well as aqueous liposomal systems was carried out at 2-8° and at ambient temperature (28±4°). The freeze dried liposomes showed better fine particle fraction and drug content over the period of six months at ambient as well as at 2-8° storage condition compared to aqueous dispersion of liposomes. PMID:23112400

Development and evaluation of inhalational liposomal system of budesonide for better management of asthma.

PubMed

Parmar, J J; Singh, D J; Hegde, Darshana D; Lohade, A A; Soni, P S; Samad, A; Menon, Mala D

2010-07-01

Budesonide is a corticosteroid used by inhalation in the prophylactic management of asthma. However, frequent dosing and adverse effects (local and systemic) remain a major concern in the use of budesonide. Liposomal systems for sustained pulmonary drug delivery have been particularly attractive because of their compatibility with lung surfactant components. In the present investigation, pulmonary liposomal delivery system of budesonide was prepared by film hydration method and evaluated for sustained release. Various parameters were optimized with respect to entrapment efficiency as well as particle size of budesonide liposomes. For better shelf life of budesonide liposomes, they were freeze dried using trehalose as cryoprotectant. The liposomes were characterized for entrapment efficiency, particle size, and surface topography; in vitro drug release was evaluated out in simulated lung fluid at 37° at pH 7.4. The respirable or fine particle fraction was determined by using twin stage impinger. The stability study of freeze dried as well as aqueous liposomal systems was carried out at 2-8° and at ambient temperature (28±40). The freeze dried liposomes showed better fine particle fraction and drug content over the period of six months at ambient as well as at 2-8° storage condition compared to aqueous dispersion of liposomes.

Development and Evaluation of Inhalational Liposomal System of Budesonide for Better Management of Asthma

PubMed Central

Parmar, J. J.; Singh, D. J.; Hegde, Darshana D.; Lohade, A. A.; Soni, P. S.; Samad, A.; Menon, Mala D.

2010-01-01

Budesonide is a corticosteroid used by inhalation in the prophylactic management of asthma. However, frequent dosing and adverse effects (local and systemic) remain a major concern in the use of budesonide. Liposomal systems for sustained pulmonary drug delivery have been particularly attractive because of their compatibility with lung surfactant components. In the present investigation, pulmonary liposomal delivery system of budesonide was prepared by film hydration method and evaluated for sustained release. Various parameters were optimized with respect to entrapment efficiency as well as particle size of budesonide liposomes. For better shelf life of budesonide liposomes, they were freeze dried using trehalose as cryoprotectant. The liposomes were characterized for entrapment efficiency, particle size, and surface topography; in vitro drug release was evaluated out in simulated lung fluid at 37° at pH 7.4. The respirable or fine particle fraction was determined by using twin stage impinger. The stability study of freeze dried as well as aqueous liposomal systems was carried out at 2-8° and at ambient temperature (28±40). The freeze dried liposomes showed better fine particle fraction and drug content over the period of six months at ambient as well as at 2-8° storage condition compared to aqueous dispersion of liposomes. PMID:21218054

Optimisation of phenolic extraction from Averrhoa carambola pomace by response surface methodology and its microencapsulation by spray and freeze drying.

PubMed

Saikia, Sangeeta; Mahnot, Nikhil Kumar; Mahanta, Charu Lata

2015-03-15

Optimised of the extraction of polyphenol from star fruit (Averrhoa carambola) pomace using response surface methodology was carried out. Two variables viz. temperature (°C) and ethanol concentration (%) with 5 levels (-1.414, -1, 0, +1 and +1.414) were used to design the optimisation model using central composite rotatable design where, -1.414 and +1.414 refer to axial values, -1 and +1 mean factorial points and 0 refers to centre point of the design. The two variables, temperature of 40°C and ethanol concentration of 65% were the optimised conditions for the response variables of total phenolic content, ferric reducing antioxidant capacity and 2,2-diphenyl-1-picrylhydrazyl scavenging activity. The reverse phase-high pressure liquid chromatography chromatogram of the polyphenol extract showed eight phenolic acids and ascorbic acid. The extract was then encapsulated with maltodextrin (⩽ DE 20) by spray and freeze drying methods at three different concentrations. Highest encapsulating efficiency was obtained in freeze dried encapsulates (78-97%). The obtained optimised model could be used for polyphenol extraction from star fruit pomace and microencapsulates can be incorporated in different food systems to enhance their antioxidant property. Copyright © 2014 Elsevier Ltd. All rights reserved.

[Optimization of lyophilization procedures for freeze-drying of human red blood cells].

PubMed

Chen, Lin-feng; Liu, Jing-han; Wang, De-qing; Ouyang, Xi-lin; Zhuang, Yuan; Che, Ji; Yu, Yang; Li, Hui

2010-09-01

To investigate the different parameters of the lyophilization procedures that affect the recovery of the rehydrated red blood cells (RBCs). Human RBCs loaded in tubes were cooled with 4 different modes and subjected to water bath at 25 degrees celsius;. The morphological changes of the RBCs were observed to assess the degree of vitrification, and the specimens were placed in the freeze-dryer with the temperature set up at 40, -50, -60, -70 and -80 degrees celsius;. The rates of temperature rise of the main and secondary drying in the lyophilization procedures were compared, and the water residue in the specimens was determined. The protectant did not show ice crystal in the course of freezing and thawing. No significant difference was found in the recovery rate of the rehydrated RBCs freeze-dried at the minimum temperature of -70 degrees celsius; and -80 degrees celsius; (P > 0.05). The E procedure resulted in the maximum recovery of the RBCs (83.14% ± 9.55%) and Hb (85.33% ± 11.42%), showing significant differences from the other groups(P < 0.01 or 0.05). The recovery of the RBCs showed a positive correlation to the water residue in the samples. Fast cooling in liquid nitrogen and shelf precooling at -70 degrees celsius; with a moderate rate of temperature rise in lyophylization and a start dry temperature close to the shelf equilibrium temperature produce optimal freeze-drying result of human RBCs.

A green salt-leaching technique to produce sericin/PVA/glycerin scaffolds with distinguished characteristics for wound-dressing applications.

PubMed

Aramwit, Pornanong; Ratanavaraporn, Juthamas; Ekgasit, Sanong; Tongsakul, Duangta; Bang, Nipaporn

2015-05-01

Sericin/PVA/glycerin scaffolds could be fabricated using the freeze-drying technique; they showed good physical and biological properties and can be applied as wound dressings. However, freeze-drying is an energy- and time-consuming process with a high associated cost. In this study, an alternative, solvent-free, energy- and time-saving, low-cost salt-leaching technique is introduced as a green technology to produce sericin/PVA/glycerin scaffolds. We found that sericin/PVA/glycerin scaffolds were successfully fabricated without any crosslinking using a salt-leaching technique. The salt-leached sericin/PVA/glycerin scaffolds had a porous structure with pore interconnectivity. The sericin in the salt-leached scaffolds had a crystallinity that was as high as that of the freeze-dried scaffolds. Compared to the freeze-dried scaffolds with the same composition, the salt-leached sericin/PVA/glycerin scaffolds has larger pores, a lower Young's modulus, and faster rates of biodegradation and sericin release. When cultured with L929 mouse fibroblast cells, a higher number of cells were found in the salt-leached scaffolds. Furthermore, the salt-leached scaffolds were less adhesive to the wound, which would reduce pain upon removal. Therefore, salt-leached sericin/PVA/glycerin scaffolds with distinguished characteristics were introduced as another choice of wound dressing, and their production process was simpler, more energy efficient, and saved time and money compared to the freeze-dried scaffolds. © 2014 Wiley Periodicals, Inc.

Application of the freeze-dried bioluminescent bioreporter Pseudomonas putida mt-2 KG1206 to the biomonitoring of groundwater samples from monitoring wells near gasoline leakage sites.

PubMed

Ko, Kyung-Seok; Kong, In Chul

2017-02-01

This study examined the applicability of a freeze-dried bioluminescent bioreporter, Pseudomonas putida mt-2 KG1206 (called KG1206), to the biomonitoring of groundwater samples. Samples were collected from the monitoring wells of gas station tanks or old pipeline leakage sites in Korea. In general, the freeze-dried strain in the presence of pure inducer chemicals showed low bioluminescence activity and a different activity order compared with that of the subcultured strain. The effects of KNO 3 as a bioluminescence stimulant were observed on the pure inducers and groundwater samples. The stimulation rates varied according to the type of inducers and samples, ranging from 2.2 to 20.5 times (for pure inducers) and from 1.1 to 11 times (for groundwater samples) the total bioluminescence of the control. No considerable correlations were observed between the bioluminescence intensity of the freeze-dried strain and the inducer concentrations in the samples (R 2  < 0.1344). However, samples without a high methyl tertiary butyl ether (MTBE) level and those from the gas station leakage site showed reasonable correlations with the bioluminescence activity with R 2 values of 0.3551 and 0.4131, respectively. These results highlight the potential of using freeze-dried bioluminescent bacteria as a rapid, simple, and portable tool for the preliminary biomonitoring of specific pollutants at contaminated sites.

Suitability of canine herpesvirus as a vector for oral bait vaccination of foxes.

PubMed

Reubel, Gerhard H; Wright, John; Pekin, Jenny; French, Nigel; Strive, Tanja

2006-05-31

Studies were conducted to evaluate the feasibility of using canine herpesvirus (CHV) as a vaccine vector for bait-delivered oral vaccination of wild foxes. To test the viability of CHV in baits, CHV was freeze-dried, incorporated into different baits, stored, and the remaining viral infectivity tested in cell culture after varying periods of time at different storage temperatures. Experimental baits (mouse carcasses) and commercial baits (FOXOFF and PROBAIT) were prepared with either liquid or freeze-dried CHV and tested in two fox trials for their capacity to induce CHV-specific antibodies following oral baiting. Freeze-drying and storage temperatures below 0 degrees C had a stabilizing effect to virus infectivity. When stored at -20 degrees C, freeze-dried CHV retained its full infectivity for up to 3 months in PROBAIT baits, the remaining infectivity in FOXOFF baits was 100-fold less. Oral baiting with CHV induced antiviral serum antibodies in all vaccinated foxes (20/20). None of the vaccinated foxes became ill or shed infectious virus into the environment although viral DNA was detected in body secretions as evaluated by PCR. The results indicate that CHV can be freeze-dried and stored over extended periods of time without loosing much of its infectivity. This is the first report of CHV being used for oral bait vaccination of foxes. It appears that CHV is well suited for use as a recombinant vector for wild canids.

Bioavailability of House Dust Mite Allergens in Sublingual Allergy Tablets Is Highly Dependent on the Formulation.

PubMed

Ohashi-Doi, Katsuyo; Kito, Hirokazu; Du, Weibin; Nakazawa, Hiroshi; Ipsen, Henrik; Gudmann, Pernille; Lund, Kaare

2017-01-01

In sublingual immunotherapy (SLIT), the immune system is addressed by solubilized allergen that interacts with immunocompetent cells of the oral mucosa, the efficiency of which is governed by 2 main factors of SLIT allergen bioavailability: the allergen concentration and the mucosal contact time. Recently, 3 house dust mite (HDM) SLIT tablets were developed that differ with regard to allergen content, nominal strength (maintenance doses: 6 SQ-HDM/10,000 Japanese Allergen Units [JAU], 12 SQ-HDM/ 20,000 JAU, and 300 IR/57,000 JAU), and formulation (freeze-dried/compressed). Here, the importance of the SLIT tablet formulation for HDM major allergen bioavailability is examined. The HDM major allergen content, tablet disintegration times, and allergen release kinetics were determined. Dissolution kinetics (allergen concentration vs. time) of Der f 1, Der p 1, and Der 2 were measured. Area under the curve (AUC) was used as a surrogate parameter for allergen bioavailability. The release of HDM major allergens from the freeze-dried tablets was complete after 30 s, while only partial release was achieved with the compressed tablets, even after prolonged dissolution. At 1 min, i.e., the recommended sublingual holding time for the freeze-dried tablets, the allergen bioavailability (AUC) of the compressed 300 IR/57,000 JAU tablet was 4.7-fold (Der f 1), 10.8-fold (Der p 1), and 23.6-fold (Der 2) lower than that of the freeze-dried 12 SQ-HDM/20,000 JAU tablet and similar to (Der f 1) and 5.3-fold (Der p 1) and 12.5-fold (Der 2) lower than that of the freeze-dried 6 SQ-HDM/10,000 JAU tablet. SLIT tablet allergen bioavailability depends highly on the tablet formulation. Only the fast-dissolving freeze-dried tablets provide maximal delivery of soluble allergens and achieve allergen concentrations that reflect the nominal tablet strengths within the recommended sublingual holding time. © 2017 S. Karger AG, Basel.

Stability of buffer-free freeze-dried formulations: A feasibility study of a monoclonal antibody at high protein concentrations.

PubMed

Garidel, Patrick; Pevestorf, Benjamin; Bahrenburg, Sven

2015-11-01

We studied the stability of freeze-dried therapeutic protein formulations over a range of initial concentrations (from 40 to 160 mg/mL) and employed a variety of formulation strategies (including buffer-free freeze dried formulations, or BF-FDF). Highly concentrated, buffer-free liquid formulations of therapeutic monoclonal antibodies (mAbs) have been shown to be a viable alternative to conventionally buffered preparations. We considered whether it is feasible to use the buffer-free strategy in freeze-dried formulations, as an answer to some of the known drawbacks of conventional buffers. We therefore conducted an accelerated stability study (24 weeks at 40 °C) to assess the feasibility of stabilizing freeze-dried formulations without "classical" buffer components. Factors monitored included pH stability, protein integrity, and protein aggregation. Because the protein solutions are inherently self-buffering, and the system's buffer capacity scales with protein concentration, we included highly concentrated buffer-free freeze-dried formulations in the study. The tested formulations ranged from "fully formulated" (containing both conventional buffer and disaccharide stabilizers) to "buffer-free" (including formulations with only disaccharide lyoprotectant stabilizers) to "excipient-free" (with neither added buffers nor stabilizers). We evaluated the impacts of varying concentrations, buffering schemes, pHs, and lyoprotectant additives. At the end of 24 weeks, no change in pH was observed in any of the buffer-free formulations. Unbuffered formulations were found to have shorter reconstitution times and lower opalescence than buffered formulations. Protein stability was assessed by visual inspection, sub-visible particle analysis, protein monomer content, charge variants analysis, and hydrophobic interaction chromatography. All of these measures found the stability of buffer-free formulations that included a disaccharide stabilizer comparable to buffer-based formulations, especially at protein concentrations up to and including 115 mg/mL. Copyright © 2015 Elsevier B.V. All rights reserved.

Effects of Different Drying Methods and Storage Time on Free Radical Scavenging Activity and Total Phenolic Content of Cosmos Caudatus.

PubMed

Mediani, Ahmed; Abas, Faridah; Tan, Chin Ping; Khatib, Alfi

2014-05-07

The present study was conducted to determine the effect of air (AD), oven (OD) and freeze drying (FD) on the free radical scavenging activity and total phenolic content (TPC) of Cosmos caudatus and the effect of storage time by the comparison with a fresh sample (FS). Among the three drying methods that were used, AD resulted in the highest free radical scavenging activity against 1,1-diphenyl-2-picrylhydrazyl (DPPH) (IC50 = 0.0223 mg/mL) and total phenolic content (27.4 g GAE/100 g), whereas OD produced the lowest scavenging activity and TPC value. After three months of storage, the dried samples showed a high and consistent free radical scavenging activity when compared to stored fresh material. The drying methods could preserve the quality of C. caudatus during storage and the stability of its bioactive components can be maintained.

Effects of Different Drying Methods and Storage Time on Free Radical Scavenging Activity and Total Phenolic Content of Cosmos caudatus

PubMed Central

Mediani, Ahmed; Abas, Faridah; Tan, Chin Ping; Khatib, Alfi

2014-01-01

The present study was conducted to determine the effect of air (AD), oven (OD) and freeze drying (FD) on the free radical scavenging activity and total phenolic content (TPC) of Cosmos caudatus and the effect of storage time by the comparison with a fresh sample (FS). Among the three drying methods that were used, AD resulted in the highest free radical scavenging activity against 1,1-diphenyl-2-picrylhydrazyl (DPPH) (IC50 = 0.0223 mg/mL) and total phenolic content (27.4 g GAE/100 g), whereas OD produced the lowest scavenging activity and TPC value. After three months of storage, the dried samples showed a high and consistent free radical scavenging activity when compared to stored fresh material. The drying methods could preserve the quality of C. caudatus during storage and the stability of its bioactive components can be maintained. PMID:26784876

Annatto Polymeric Microparticles: Natural Product Encapsulation by the Emulsion-Solvent Evaporation Method

ERIC Educational Resources Information Center

Teixeira, Zaine; Duran, Nelson; Guterres, Silvia S.

2008-01-01

In this experiment, the extract from annatto seeds was encapsulated in poly(3-hydroxybutyrate-co-3-hydroxyvalerate) (PHBV) particles by the emulsion-solvent evaporation method. The particles were washed and centrifuged to remove excess stabilizer and then freeze-dried. The main compound of annatto seeds, bixin, has antioxidant properties as well…

Analysis of the moisture evaporation process during vacuum freeze-drying of koumiss and shubat

NASA Astrophysics Data System (ADS)

Shingisov, Azret Utebaevich; Alibekov, Ravshanbek Sultanbekovich

2017-05-01

The equation for the calculating of a moisture evaporation rate in the vacuum freeze-drying, wherein as a driving force instead of the generally accepted in the drying theory of Δt temperature difference, Δp pressure difference, Δc concentration difference, a difference of water activity in the product and the relative air humidity (a_{{w}} - \\varphi) is suggested. By using the proposed equation, the processes of vacuum freeze-drying of koumiss and shubat were analyzed, and it was found two drying periods: constant and falling. On the first drying period, a moisture evaporation rate of koumiss is j = 2.75 × 10-3 kg/(m2 h) and of shubat is j = 2.37 × 10-3 kg/(m2 h). On the second period, values decrease for koumiss from j = 2.65 × 10-3 kg/(m2 h) to j = 1.60 × 10-3 kg/(m2 h), and for shubat from j = 2.25 × 10-3 kg/(m2 h) to j = 1.62 × 10-3 kg/(m2 h). Specific humidity for koumiss is ueq = 0.61 kg/kg and for shubat is ueq = 0.58 kg/kg. The comparative analyze of the experimental data of the moisture evaporation rate versus the theoretical calculation shows that the approximation reliability is R2 = 0.99. Consequently, the proposed equation is useful for the analyzing a moisture evaporation rate during a vacuum freeze-drying of dairy products, including cultured milk foods.

Technological Development of Brewing in Domestic Refrigerator Using Freeze-Dried Raw Materials

PubMed Central

2017-01-01

Summary Development of a novel directly marketable beer brewed at low temperature in a domestic refrigerator combined with yeast immobilization technology is presented in this study. Separately, freeze-dried wort and immobilized cells of the cryotolerant yeast strain Saccharomyces cerevisiae AXAZ-1 on tubular cellulose were used in low-temperature fermentation (2, 5 and 7 °C). The positive effect of tubular cellulose during low-temperature brewing was examined, revealing that freeze-dried immobilized yeast cells on tubular cellulose significantly reduced the fermentation rates in contrast to freeze-dried free cells, although they are recommended for home-made beer production. Immobilization also enhanced the yeast resistance at low-temperature fermentation, reducing the minimum brewing temperature value from 5 to 2 °C. In the case of high-quality beer production, the effect of temperature and initial sugar concentration on the fermentation kinetics were assessed. Sensory enrichment of the produced beer was confirmed by the analysis of the final products, revealing a low diacetyl concentration, together with improved polyphenol content, aroma profile and clarity. The proposed process for beer production in a domestic refrigerator can easily be commercialized and applied by dissolving the content of two separate packages in tap water; one package containing dried wort and the other dried immobilized cells on tubular cellulose suspended in tap water. PMID:29089847

Production and processing of Metarhizium anisopliae var. acridum submerged conidia for locust and grasshopper control.

PubMed

Kassa, Adane; Stephan, Dietrich; Vidal, Stefan; Zimmermann, Gisbert

2004-01-01

Currently, mycopesticide development for locust and grasshopper control depends on aerial conidia or submerged spores of entomopathogenic fungi. In our study, the production of submerged conidia of Metarhizium anisopliae var. acridum (IMI 330189) was investigated in a liquid medium containing 3% biomalt and 1% yeast extract (BH-medium). The effects of freeze and spray drying techniques on the quality of submerged conidia were determined. The influence of different additives on the viability of fresh submerged conidia and their suitability for oil flowable concentrate formulation development was assessed. In a BH medium maintained at 180 rev min(-1), at 30 degrees C for 72 h, IMI 330189 produced a green pigmented biomass of submerged conidia whereas in Adámek medium it produced a yellowish biomass of submerged spores. The spore concentration was high in both media; however, the size of the spores produced in the BH medium was significantly lower than those produced in Adámek medium (P < 0.001). Submerged conidia can be effectively dried using either freeze or spray drying techniques. The viability and speed of germination were significantly affected by the drying and pulverizing process (P < 0.001). The initial viability was significantly higher for spray-dried submerged conidia than for freeze-dried spores. Pulverizing of freeze-dried submerged conidia reduced the speed of germination and the viability by 63-95%. Dried submerged conidia can be stored over 45 wk at low temperatures (< 10 degrees) without suffering a significant loss in viability. Furthermore, we have identified carriers that are suitable for oil flowable concentrate formulation development.

The effect of excipients on the stability and aerosol performance of salmon calcitonin dry powder inhalers prepared via the spray freeze drying process.

PubMed

Poursina, Narges; Vatanara, Alireza; Rouini, Mohammad Reza; Gilani, Kambiz; Najafabadi, Abdolhossein Rouholamini

2016-06-01

Spray freeze drying was developed to produce dry powders suitable for applications such as inhalation delivery. In the current study, the spray freeze drying technique was employed to produce inhalable salmon calcitonin microparticles. Effects of the carrier type, concentration of hydroxyl propyl-β-cyclodextrin and the presence of Tween 80 on the chemical and structural stability, as well as on the aerosol performance of the particles were investigated. The results indicated that hydroxyl propyl-β-cyclodextrin had the most important effect on the chemical stability of the powder and strongly increased its stability by increasing its concentration in the formulation. Chemically stable formulations (over 90 % recovery) were selected for further examinations. Fluorescence spectroscopy and circular dichroism suggested that the formulations were structurally stable. Aerosol performance showed that the Tween-free powders produced higher fine particle fraction values than the formulations containing Tween (53.7 vs. 41.92 % for trehalose content and 52.85 vs. 43.06 % for maltose content).

Encapsulation of antioxidant phenolic compounds extracted from spent coffee grounds by freeze-drying and spray-drying using different coating materials.

PubMed

Ballesteros, Lina F; Ramirez, Monica J; Orrego, Carlos E; Teixeira, José A; Mussatto, Solange I

2017-12-15

Freeze-drying and spray-drying techniques were evaluated for encapsulation of phenolic compounds (PC) extracted from spent coffee grounds. Additionally, the use of maltodextrin, gum arabic and a mixture of these components (ratio 1:1) as wall material to retain the PC and preserve their antioxidant activity was also assessed. The contents of PC and flavonoids (FLA), as well as the antioxidant activity of the encapsulated samples were determined in order to verify the efficiency of each studied condition. Additional analyses for characterization of the samples were also performed. Both the technique and the coating material greatly influenced the encapsulation of antioxidant PC. The best results were achieved when PC were encapsulated by freeze-drying using maltodextrin as wall material. Under these conditions, the amount of PC and FLA retained in the encapsulated sample corresponded to 62% and 73%, respectively, and 73-86% of the antioxidant activity present in the original extract was preserved. Copyright © 2017 Elsevier Ltd. All rights reserved.

Development of a Mini-Freeze Dryer for Material-Sparing Laboratory Processing with Representative Product Temperature History.

PubMed

Obeidat, Wasfy M; Sahni, Ekneet; Kessler, William; Pikal, Michael

2018-02-01

The goal of the work described in this publication was to evaluate a new, small, material-sparing freeze dryer, denoted as the "mini-freeze dryer or mini-FD", capable of reproducing the product temperature history of larger freeze dryers, thereby facilitating scale-up. The mini-FD wall temperatures can be controlled to mimic loading procedures and dryer process characteristics of larger dryers. The mini-FD is equipped with a tunable diode laser absorption spectroscopy (TDLAS) water vapor mass flow monitor and with other advanced process analytical technology (PAT) sensors. Drying experiments were performed to demonstrate scalability to larger freeze dryers, including the determination of vial heat transfer coefficients, K v . Product temperature histories during K v runs were evaluated and compared with those obtained with a commercial laboratory-scale freeze dryer (LyoStar II) for sucrose and mannitol product formulations. When the mini-FD wall temperature was set at the LyoStar II band temperature (- 20°C) to mimic lab dryer edge vials, edge vial drying in the mini-FD possessed an average K v within 5% of those obtained during drying in the LyoStar II. When the wall temperature of the mini-FD was set equal to the central vial product temperature, edge vials behaved as center vials, possessing a K v value within 5% of those measured in the LyoStar II. During both K v runs and complete product freeze drying runs, the temperature-time profiles for the average edge vials and central vial in the mini-FD agreed well with the average edge and average central vials of the LyoStar II.

Effect of temperature and relative humidity on stability following simulated gastro-intestinal digestion of microcapsules of Bordo grape skin phenolic extract produced with different carrier agents.

PubMed

Kuck, Luiza Siede; Wesolowski, Júlia Lerina; Noreña, Caciano Pelayo Zapata

2017-09-01

The stability of microparticles of Bordo grape skin aqueous extract, produced by spray-drying and freeze-drying using polydextrose (5%) and partially hydrolyzed guar gum (5%), was evaluated under accelerated conditions (75 and 90% relative humidity, at 35, 45, and 55°C for 35days) and simulated gastrointestinal digestion. The temperature had a significant effect on the reduction of phenolics content, with retentions varying from 82.5 to 93.5%. The retention of total monomer anthocyanins were in the range of 3.9-42.3%. The antioxidant activity had a final retention of 38.5-59.5%. In the simulated gastrointestinal digestion, a maximum release was observed for the phenolic compounds in the intestinal phase (90.6% for the spray-dried powder and 94.9% for the freeze-dried powder), as well as the antioxidant activity (69.4% for the spray-dried powder and 67.8% for the freeze-dried powder). However, a reduction of monomeric anthocyanins was observed in the intestinal phase. Copyright © 2017 Elsevier Ltd. All rights reserved.

Comparison of different drying methods on Chinese ginger (Zingiber officinale Roscoe): Changes in volatiles, chemical profile, antioxidant properties, and microstructure.

PubMed

An, Kejing; Zhao, Dandan; Wang, Zhengfu; Wu, Jijun; Xu, Yujuan; Xiao, Gengsheng

2016-04-15

Nowadays, food industry is facing challenges in preserving better quality of fruit and vegetable products after processing. Recently, many attentions have been drawn to ginger rhizome processing due to its numerous health promoting properties. In our study, ginger rhizome slices were subjected to air-drying (AD), freeze drying (FD), infrared drying (IR), microwave drying (MD) and intermittent microwave & convective drying (IM&CD). Quality attributes of the dried samples were compared in terms of volatile compounds, 6, 8, 10-gingerols, 6-shogaol, antioxidant activities and microstructure. Results showed that AD and IR were good drying methods to preserve volatiles. FD, IR and IM&CD led to higher retention of gingerols, TPC, TFC and better antioxidant activities. However, FD and IR had relative high energy consumption and drying time. Therefore, considering about the quality retention and energy consumption, IM&CD would be very promising for thermo sensitive material. Copyright © 2015 Elsevier Ltd. All rights reserved.

Chemical composition, antioxidant capacity, and sensory quality of dried jujube fruits as affected by cultivar and drying method.

PubMed

Wojdyło, Aneta; Figiel, Adam; Legua, Pilar; Lech, Krzysztof; Carbonell-Barrachina, Ángel A; Hernández, Francisca

2016-09-15

The aim of this study was to determine the effect of different dying methods, such as convective drying (CD: 50, 60, 70 °C), vacuum-microwave drying (VMD: 120, 480, 480-120 W), a combination of convective pre-drying and vacuum-microwave finish drying [(CPD (60 °C)-VMFD (480-120 W)], and freeze-drying (FD) on key quality parameters of dried jujube fruits (cv. "GAL", "MSI", and "PSI"). The parameters studied included bioactive compounds (flavan-3-ols and flavonols, identified by LC-PDA-MS, and vitamin C), antioxidant capacity (ABTS and FRAP), and sensory attributes (e.g. hardness, jujube-ID, and sweetness). The best quality of the dried product (high contents of bioactive compounds and high intensity of key sensory attributes) was found in fruits treated by FD and VMD 480-120 W. The best cultivars were "PSI" and "GAL" from the point of view of bioactive content and sensory quality, respectively. Copyright © 2016 Elsevier Ltd. All rights reserved.

Physicochemical properties of whole fruit plum powders obtained using different drying technologies.

PubMed

Michalska, Anna; Wojdyło, Aneta; Lech, Krzysztof; Łysiak, Grzegorz P; Figiel, Adam

2016-09-15

Physicochemical quality parameters of plum powders obtained by applying conventional drying methods and their combination devised to process plums were evaluated. The effect of freeze-drying (FD), vacuum drying (VD), convective drying (CD), microwave-vacuum drying (MVD) and combination of convective pre-drying and microwave finish-drying (CPD-MVFD) affected physical (bulk density, porosity, colour, solubility) and chemical (polyphenolic compounds determined by UPLC and antioxidant capacity by TEAC ABTS and FRAP methods) properties of plum powders. The MVD at 1.2 W g(-1) and a novel combination for plum powders production - CPD-MVFD at 70 °C/1.2 W g(-1) allowed the best preservation of phenolic compounds and increased the efficiency of production. Results obtained support the use of MVD and its combination for better quality of dried plum products. The study proved that the determination of the browning index and HMF level (formed via Maillard reaction) might be good tool for monitoring the thermal processing of plum powders. Copyright © 2016 Elsevier Ltd. All rights reserved.

Microwave-Osmotic/Microwave-Vacuum Drying of Whole Cranberries: Comparison with Other Methods.

PubMed

Wray, Derek; Ramaswamy, Hosahalli S

2015-12-01

A novel drying method for frozen-thawed whole cranberries was developed by combining microwave osmotic dehydration under continuous flow medium spray (MWODS) conditions with microwave vacuum finish-drying. A central composite rotatable design was used to vary temperature (33 to 67 °C), osmotic solution concentration (33 to 67 °B), contact time (5 to 55 min), and flow rate (2.1 to 4.1 L/min) in order to the determine the effects of MWODS input parameters on quality of the dried berry. Quality indices monitored included colorimetric and textural data in addition to anthocyanin retention and cellular structure. Overall it was found that the MWODS-MWV process was able to produce dried cranberries with quality comparable to freeze dried samples in much shorter time. Additionally, cranberries dried via the novel process exhibited much higher quality than those dried via either vacuum or convective air drying in terms of color, anthocyanin content, and cellular structure. © 2015 Institute of Food Technologists®

Development of a Soluplus budesonide freeze-dried powder for nasal drug delivery.

PubMed

Pozzoli, Michele; Traini, Daniela; Young, Paul M; Sukkar, Maria B; Sonvico, Fabio

2017-09-01

The aim of this work was to develop an amorphous solid dispersions/solutions (ASD) of a poorly soluble drug, budesonide (BUD) with a novel polymer Soluplus ® (BASF, Germany) using a freeze-drying technique, in order to improve dissolution and absorption through the nasal route. The small volume of fluid present in the nasal cavity limits the absorption of a poorly soluble drug. Budesonide is a corticosteroid, practically insoluble and normally administered as a suspension-based nasal spray. The formulation was prepared through freeze-drying of polymer-drug solution. The formulation was assessed for its physicochemical (specific surface area, calorimetric analysis and X-ray powder diffraction), release properties and aerodynamic properties as well as transport in vitro using RPMI 2650 nasal cells, in order to elucidate the efficacy of the Soluplus-BUD formulation. The freeze-dried Soluplus-BUD formulation (LYO) showed a porous structure with a specific surface area of 1.4334 ± 0.0178 m 2 /g. The calorimetric analysis confirmed an interaction between BUD and Soluplus and X-ray powder diffraction the amorphous status of the drug. The freeze-dried formulation (LYO) showed faster release compared to both water-based suspension and dry powder commercial products. Furthermore, a LYO formulation, bulked with calcium carbonate (LYO-Ca), showed suitable aerodynamic characteristics for nasal drug delivery. The permeation across RPMI 2650 nasal cell model was higher compared to a commercial water-based BUD suspension. Soluplus has been shown to be a promising polymer for the formulation of BUD amorphous solid suspension/solution. This opens up opportunities to develop new formulations of poorly soluble drug for nasal delivery.

Cold tolerance and freeze-induced glucose accumulation in three terrestrial slugs.

PubMed

Slotsbo, Stine; Hansen, Lars Monrad; Jordaens, Kurt; Backeljau, Thierry; Malmendal, Anders; Nielsen, Niels Chr; Holmstrup, Martin

2012-04-01

Cold tolerance and metabolic responses to freezing of three slug species common in Scandinavia (Arion ater, Arion rufus and Arion lusitanicus) are reported. Autumn collected slugs were cold acclimated in the laboratory and subjected to freezing conditions simulating likely winter temperatures in their habitat. Slugs spontaneously froze at about -4 °C when cooled under dry conditions, but freezing of body fluids was readily induced at -1 °C when in contact with external ice crystals. All three species survived freezing for 2 days at -1 °C, and some A. rufus and A. lusitanicus also survived freezing at -2 °C. (1)H NMR spectroscopy revealed that freezing of body fluids resulted in accumulation of lactate, succinate and glucose. Accumulation of lactate and succinate indicates that ATP production occurred via fermentative pathways, which is likely a result of oxygen depletion in frozen tissues. Glucose increased from about 6 to 22 μg/mg dry tissue upon freezing in A. rufus, but less so in A. ater and A. lusitanicus. Glucose may thus act as a cryoprotectant in these slugs, although the concentrations are not as high as reported for other freeze tolerant invertebrates. Copyright © 2012 Elsevier Inc. All rights reserved.

Pre-cure freezing affects proteolysis in dry-cured hams.

PubMed

Bañón, S; Cayuela, J M; Granados, M V; Garrido, M D

1999-01-01

Several parameters (sodium chloride, moisture, intramuscular fat, total nitrogen, non-protein nitrogen, white precipitates, free tyrosine, L* a* b* values and acceptability) related with proteolysis during the curing were compared in dry-cured hams manufactured from refrigerated and frozen/thawed raw material. Pre-cure freezing increased the proteolysis levels significantly (p<0.05) in the zones of the ham where water losses and absorption of salt is slowest. Frozen hams present a high incidence of white precipitates, formed mainly by tyrosine crystals. The colour and acceptability scores are similar in frozen and refrigerated hams. The previous freezing and thawing process accentuates the water losses, salt absorption and proteolysis of the cured meat, although it does not significantly affect the sensory quality of the dry-cured ham.

Valorization of postharvest sweet cherry discard for the development of dehydrated fruit ingredients: compositional, physical, and mechanical properties.

PubMed

Franceschinis, Lorena; Sette, Paula; Salvatori, Daniela; Schebor, Carolina

2018-04-20

Sweet cherries are an excellent source of phenolic compounds, which may contribute to a healthy diet. The objective of this work was to generate dehydrated ingredients from postharvest discard of sweet cherries. Four dried ingredients were obtained from fresh sweet cherry discard (Lapins var.) using an osmotic dehydration pretreatment and freeze drying or air drying. The ingredients showed an important phenolic contribution (2.8-6.6 g gallic acid kg -1 of product) and preserved the natural color of the fruit to a great extent. Freeze-dried ingredients were less hygroscopic than air-dried ones, and presented with a softer texture. All the ingredients were in a supercooled state at room temperature (T g range: -23.0 to -18.8 °C). Sugar infusion pretreatment caused a decrease in water sorption capacity and molecular mobility; it also reduced the initial rehydration rate. Relevant differences in nutritional and structural characteristics of the ingredients were observed depending on the processing method used. These ingredients could be incorporated into different processed foods, such as snacks, cereal mixtures, cereal bars, and bakery and confectionery products. Air-dried control ingredients presented better nutritional qualities and air-dried sweet cherries with sugar infusion pretreatment could be appropriate ingredients for applications where sweet flavor and slow rehydration rate are required. © 2018 Society of Chemical Industry. © 2018 Society of Chemical Industry.

A rapid method for concentrating sedimentary organic matter for vitrinite reflectance analysis.

USGS Publications Warehouse

Barker, C.E.

1982-01-01

The tecnique discussed in this paper utilizes crushing, high-speed blending, and ultrasonic treatment to mechanically disaggregate rock and release the sedimentary organic matter (OM) in a suitable heavy liquid. This new method can provide freeze-dried concentrated OM in approximately 8 to 24 hours (longer time is necessary for removing carbonate). Under optimal conditions, it is possible to concentrate the OM and prepare a hardened epoxy microscope slide in about 24 hours. Subsequent grinding, polishing, and drying allows microscopic examination of the organic concentrate the next day.-from Author

Temperature Dependence of Positron Annihilation in beta-Cyclodextrin and beta-Cyclodextrin Complexes

NASA Astrophysics Data System (ADS)

Hu, Y.; Hsu Hadley, F. H., Jr.; Trinh, T.

1996-11-01

The effects of temperature on positron annihilation in beta-cyclodextrin and beta-cyclodextrin complexed with benzyl salicylate, benzyl acetate, ethyl salicylate, geraniol, linalool and nerol were studied. Samples were prepared by slurry, air-dried and freeze-dried methods. Lifetime spectra were measured as a function of temperature for each sample. Comparison of the annihilation rate and intensity of the longer-lived component showed that positronium formation was affected by guest molecules, preparation methods and temperature variations. Results can be used to explain beta-cyclodextrin complex formation with different guest molecules.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sundaramurthi, Prakash; Patapoff, Thomas W.; Suryanarayanan, Raj

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 frozenmore » 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.« less

Lyophilization process design space.

PubMed

Patel, Sajal Manubhai; Pikal, Michael J

2013-11-01

The application of key elements of quality by design (QbD), such as risk assessment, process analytical technology, and design space, is discussed widely as it relates to freeze-drying process design and development. However, this commentary focuses on constructing the Design and Control Space, particularly for the primary drying step of the freeze-drying process. Also, practical applications and considerations of claiming a process Design Space under the QbD paradigm have been discussed. © 2013 Wiley Periodicals, Inc. and the American Pharmacists Association.

[Production and characteristics of bacteria-labeled talc dust for experimental air hygiene studies].

PubMed

Ohgke, H; Oldenburg, B; Gropengiesser, R; Herbst, M

1983-04-01

Freeze-drying of suspensions of Micrococcus luteus together with talc yields bacteria-labelled dust. This material can be used in experimental air hygiene. Loss of viability due to drying in air during experiments can be expected to be negligible. A wide range of particle diameters (1 to greater than 23 micron) is available. Scanning electron microscopy shows the bacteria sticking on talc particles after freeze-drying (Fig. 3a + b). Viable counts of the material decreased very slowly on storage.

Development of a nanosuspension for iv administration: From miniscale screening to a freeze dried formulation.

PubMed

Frank, Kerstin J; Boeck, Georg

2016-05-25

The aim was to develop a nanosuspension of the poorly soluble BI XX. The nanosuspension is intended for intravenous (iv) administration in preclinical studies and should not cause any unwanted side effects. Thus, only stabilizers that are accepted for iv application should be used and isotonicity, euhydria and the absence of living microorganisms were targeted. Suspensions were prepared in a ball-mill (mixing mill MM 400 from Retsch). There were various vials used as containers; HPLC-vials were used for the small scale screening of stabilizers and injection vials for preparation of larger quantities of the nanosuspensions. Particle size distribution was analyzed by laser diffraction measurement (Mastersizer 2000). Lyophilization was used for processing of the suspensions (Christ freeze dryer). Stable nanosuspensions (d90 remained <1μm up to 7days) were prepared with several FDA-accepted stabilizers. Freeze drying was evaluated for one formulation containing 2% of the API, 0.5% of arginine and 4% of mannitol. The particle size distribution before freeze drying and after re-dispersion was comparable. After milling for 2h, no living microorganisms were detected in the nanosuspension. Various FDA accepted excipients were identified which resulted in stable nanosuspensions of BI XX. The most stable formulation was successfully freeze dried. It was proven that milling in the ball-mill decreases the presence of living microorganisms. Copyright © 2016. Published by Elsevier B.V.

Oligosaccharide-based Surfactant/Citric Acid Buffer System Stabilizes Lactate Dehydrogenase during Freeze-drying and Storage without the Addition of Natural Sugar.

PubMed

Ogawa, Shigesaburo; Kawai, Ryuichiro; Koga, Maito; Asakura, Kouichi; Takahashi, Isao; Osanai, Shuichi

2016-06-01

Experiments were conducted to assess the maintenance effects of oligosaccharide-based surfactants on the enzymatic activity of a model protein, lactate dehydrogenase (LDH), during freeze-drying and room temperature storage using the citric acid buffer system. Oligosaccharide-based surfactants, which exhibit a high glass transition temperature (Tg), promoted the eminent retention of enzymatic activity during these protocols, whereas monosaccharide-based surfactants with a low Tg displayed poor performance at high concentration, albeit much better than that of Tween 80 at middle concentration. The increase in the alkyl chain length did not exert positive effects as observed for the maintenance effect during freeze-thawing, but an amphiphilic nature and a glass forming ability were crucial for the effective stabilization at a low excipient concentration during freeze-drying. Even a low oligosaccharide-based surfactant content (0.1 mg mL(-1)) could maintain LDH activity during freeze-drying, but a high surfactant content (1.0 mg mL(-1)) was required to prevent buffer precipitation and retain high LDH activity on storage. Regarding storage, glass formation restricted molecular mobility in the lyophilized matrix, and LDH activity was effectively retained. The present results describe a strategy based on the glass-forming ability of surfactant-type excipients that affords a natural sugar-free formulation or an alternative use for polysorbate-type surfactants.

A method for trace element determination of single Daphnia specimens using total reflection X-ray fluorescence spectrometry

NASA Astrophysics Data System (ADS)

Mages, Margarete; Woelfl, Stefan; v. Tümpling jun, Wolf

2001-11-01

Two new preparation techniques for total-reflection X-ray fluorescence (TXRF) element determination of single freshwater crustacean specimens (dry weight: 3-40 μg ind -1) have been developed and tested using Daphnia pulex from a deep, oligotrophic freshwater lake located in southern Chile. Dry method: Specimens were washed with 0.2 μm filtered lake water and frozen in liquid nitrogen. The freeze-dried Daphnia specimens were weighed using an ultra-fine microbalance and placed on quartz glass carriers for TXRF analysis. Wet method: Specimens were washed with 0.2 μm filtered lake water and placed on quartz glass carriers for TXRF analysis and dried in air. The dry weight was determined using the previously established body length-dry weight relationship. Method validation for both the dry and the wet preparation method in combination with TXRF spectrometry for the element determination in small single freshwater crustaceans showed that both methods can be used for routine investigations. There were no significant differences between the dry and the wet methods concerning the elements Ca, K, Fe, Zn, Br, P, Cu, but the determination of Mn, S and Sr revealed significant differences between the two methods. It seems that the dry method yields more precise results, but the wet method is easier to handle in the field when samples cannot be fixed with liquid nitrogen.

Influence of drying method on steviol glycosides and antioxidants in Stevia rebaudiana leaves.

PubMed

Periche, Angela; Castelló, María Luisa; Heredia, Ana; Escriche, Isabel

2015-04-01

The application of different drying conditions (hot air drying at 100 °C and 180 °C, freeze drying and shade drying) on steviol glycosides (stevioside, dulcoside A, rebaudioside A and rebaudioside C) and antioxidants in Stevia leaves was evaluated. Stevioside, the major glycoside found in fresh leaves (81.2mg/g), suffered an important reduction in all cases, although shade drying was the least aggressive treatment. Considering the antioxidant parameters (total phenols, flavonoids and total antioxidants), the most suitable drying method was hot air at 180 °C, since it substantially increased all of them (76.8 mg gallic acid, 45.1mg catechin and 126 mg Trolox, all equivalent/g Stevia, respectively), with respect to those present in fresh leaves (44.4, 2.5 and 52.9 mg equivalent/g). Therefore, the ideal method for drying Stevia leaves depends on their final use (sweetener or antioxidant), although, hot air at 180 °C is the most recommendable if only one treatment has to be chosen. Copyright © 2014 Elsevier Ltd. All rights reserved.

Mechanical performance and thermal stability of glass fiber reinforced silica aerogel composites based on co-precursor method by freeze drying

NASA Astrophysics Data System (ADS)

Zhou, Ting; Cheng, Xudong; Pan, Yuelei; Li, Congcong; Gong, Lunlun; Zhang, Heping

2018-04-01

In order to maintain the integrity, glass fiber (GF) reinforced silica aerogel composites were synthesized using methltrimethoxysilane (MTMS) and water glass co-precursor by freeze drying method. The composites were characterized by scanning electron microscopy, Brunauer-Emmett-Teller analysis, uniaxial compressive test, three-point bending test, thermal conductivity analysis, contact angle test, TG-DSC analysis. It was found that the molar ratio of MTMS/water glass could significantly affect the properties of composites. The bulk density and thermal conductivity first decreased and then increased with the increasing molar ratio. The composites showed remarkable mechanical strength and flexibility compared with pure silica aerogel. Moreover, when the molar ratio is 1.8, the composites showed high specific surface area (870.9 m2/g), high contact angle (150°), great thermal stability (560 °C) and low thermal conductivity (0.0248 W/m·K). These outstanding properties indicate that GF/aerogels have broad prospects in the field of thermal insulation.

Role of precursors on greening in crushed garlic (Allium sativum) bulbs, and its control with freeze-dried onion powder.

PubMed

Cho, Jungeun; Lee, Eun Jin; Yoo, Kil Sun; Lee, Seung Koo

2012-01-30

Lachrymatory factor (LF) synthase in onion bulbs reacts with S-1-propenyl-L-cysteine sulfoxide (1-PeCSO), a key compound in garlic greening. In this study, freeze-dried onion powder containing LF synthase was used in treatments to control garlic greening. Prior to the use of freeze-dried onion powder to treat greening garlic bulbs, model reactions were conducted to confirm the reactivity of 1-PeCSO in onion bulbs to garlic greening. While pink pigments were generated from 1-PeCSO, green pigments were produced from the combination of 1-PeCSO and S-2-propenyl-L-cysteine sulfoxide (2-PeCSO). However, pigments were formed in the systems containing 1-PeCSO, amino acid and alliinase. Even non-greening garlic bulbs stored at 20 °C turned green with the reaction of 200 g L(-1) 1-PeCSO; therefore 1-PeCSO isolated from onion bulbs had the same role as 1-PeCSO in garlic bulbs in terms of greening. Onion bulbs turned green after the addition of 600 g L(-1) 2-PeCSO. The addition of freeze-dried onion powder inhibited garlic greening, and treatment with 15 g kg(-1) onion powder gave the best storage stability of crushed garlic bulbs. The addition of freeze-dried onion powder inhibited the greening in crushed garlic bulbs, and treatment with 15 g kg(-1) onion powder gave the best storage stability of crushed garlic bulbs. Copyright © 2011 Society of Chemical Industry.

Correlation of laboratory and production freeze drying cycles.

PubMed

Kuu, Wei Y; Hardwick, Lisa M; Akers, Michael J

2005-09-30

The purpose of this study was to develop the correlation of cycle parameters between a laboratory and a production freeze-dryer. With the established correlation, key cycle parameters obtained using a laboratory dryer may be converted to those for a production dryer with minimal experimental efforts. In order to develop the correlation, it was important to consider the contributions from the following freeze-drying components: (1) the dryer, (2) the vial, and (3) the formulation. The critical parameters for the dryer are the shelf heat transfer coefficient and shelf surface radiation emissivity. The critical parameters for the vial are the vial bottom heat transfer coefficients (the contact parameter Kcs and separation distance lv), and vial top heat transfer coefficient. The critical parameter of the formulation is the dry layer mass transfer coefficient. The above heat and mass transfer coefficients were determined by freeze-drying experiments in conjunction with mathematical modeling. With the obtained heat and mass transfer coefficients, the maximum product temperature, Tbmax, during primary drying was simulated using a primary drying subroutine as a function of the shelf temperature and chamber pressure. The required shelf temperature and chamber pressure, in order to perform a successful cycle run without product collapse, were then simulated based on the resulting values of Tbmax. The established correlation approach was demonstrated by the primary drying of the model formulation 5% mannitol solution. The cycle runs were performed using a LyoStar dryer as the laboratory dryer and a BOC Edwards dryer as the production dryer. The determined normalized dried layer mass transfer resistance for 5% mannitol is expressed as RpN=0.7313+17.19l, where l is the receding dry layer thickness. After demonstrating the correlation approach using the model formulation 5% mannitol, a practical comparison study was performed for the actual product, the lactate dehydrogenase (LDH) formulation. The determined normalized dried layer mass transfer resistance for the LDH formulation is expressed as RpN=4.344+10.85l. The operational templates Tbmax and primary drying time were also generated by simulation. The cycle run for the LDH formulation using the Edwards production dryer verified that the cycle developed in a laboratory freeze-dryer was transferable at the production scale.

A new method for long-term storage of titred microbial standard solutions suitable for microbiologic quality control activities of pharmaceutical companies.

PubMed

Chiellini, Carolina; Mocali, Stefano; Fani, Renato; Ferro, Iolanda; Bruschi, Serenella; Pinzani, Alessandro

2016-08-01

Commercially available lyophilized microbial standards are expensive and subject to reduction in cell viability due to freeze-drying stress. Here we introduce an inexpensive and straightforward method for in-house microbial standard preparation and cryoconservation that preserves constant cell titre and cell viability over 14 months.

A Comparison between Use of Spray and Freeze Drying Techniques for Preparation of Solid Self-Microemulsifying Formulation of Valsartan and In Vitro and In Vivo Evaluation

PubMed Central

Singh, Sanjay Kumar; Vuddanda, Parameswara Rao; Singh, Sanjay; Srivastava, Anand Kumar

2013-01-01

The objective of the present study was to develop self micro emulsifying formulation (SMEF) of valsartan to improve its oral bioavailability. The formulations were screened on the basis of solubility, stability, emulsification efficiency, particle size and zeta potential. The optimized liquid SMEF contains valsartan (20% w/w), Capmul MCM C8 (16% w/w), Tween 80 (42.66% w/w) and PEG 400 (21.33% w/w) as drug, oil, surfactant and co-surfactant, respectively. Further, Liquid SMEF was adsorbed on Aerosol 200 by spray and freeze drying methods in the ratio of 2 : 1 and transformed into free flowing powder. Both the optimized liquid and solid SMEF had the particle size <200 nm with rapid reconstitution properties. Both drying methods are equally capable for producing stable solid SMEF and immediate release of drug in in vitro and in vivo conditions. However, the solid SMEF produced by spray drying method showed high flowability and compressibility. The solid state characterization employing the FTIR, DSC and XRD studies indicated insignificant interaction of drug with lipid and adsorbed excipient. The relative bioavailability of solid SMEF was approximately 1.5 to 3.0 folds higher than marketed formulation and pure drug. Thus, the developed solid SMEF illustrates an alternative delivery of valsartan as compared to existing formulations with improved bioavailability. PMID:23971048

Basic Principles of Lyophilization, Part 1.

PubMed

Akers, Michael J

2015-01-01

The achievement of a high-quality lyophilized (freeze-dried) dosage form involves the combination of optimal formulation design and optimal freeze-dry cycle design. This 2-part article describes how this can be done. Part 1 discusses the basic principles and procedures of lyophilization up to a discussion on the different stages of lyophilization. The stages of lyophilization are discussed in part 2.

Freeze drying-assisted synthesis of Pt@reduced graphene oxide nanocomposites as excellent hydrogen sensor

NASA Astrophysics Data System (ADS)

Lu, Xiaojing; Song, Xinjie; Gu, Cuiping; Ren, Haibo; Sun, Yufeng; Huang, Jiarui

2018-05-01

Quick and efficient detection of low concentrations of hydrogen remains a challenge because of the stability of hydrogen. A sensor based on reduced oxide graphene functionalized with Pt nanoparticles is successfully fabricated using a freeze-drying method followed by heat treatment. The structure and morphology of the Pt@rGO nanocomposites are well analyzed by X-ray diffraction, field emission scanning electron microscopy, transmission electron microscopy, Raman spectroscopy, and X-ray photoelectron spectroscopy. The as-prepared Pt@rGO nanocomposites show excellent hydrogen gas sensing properties at a low working temperature of 50 °C. The sensitivity toward 0.5% hydrogen is 8%. The response and recovery times of the sensor exposed to 0.5% hydrogen are 63 and 104 s, respectively. The gas-sensing mechanism of Pt@rGO sensor is also discussed.

Polymer formulations for gettering hydrogen

DOEpatents

Shepodd, Timothy J.; Even, Jr., William R.

2000-01-01

A novel method for preparing a hydrogenation composition comprising organic polymer molecules having carbon--carbon double bonds, for removing hydrogen from the atmosphere within enclosed spaces and particularly from atmospheres within enclosed spaces that contain air, water vapor, oxygen, carbon dioxide or ammonia. The organic polymers molecules containing carbon--carbon double bonds throughout their structures, preferably polybutadiene, polyisoprene and derivatives thereof, intimately mixed with an insoluble noble metal catalyst composition. High molecular weight polymers may be added to the organic polymer/catalyst mixture in order to improve their high temperature performance. The hydrogenation composition is prepared by dispersing the polymers in a suitable solvent, forming thereby a solution suspension, flash-freezing droplets of the solution in a liquid cryogen, freeze-drying the frozen droplets to remove frozen solvent incorporated in the droplets, and recovering the dried powder thus formed.

Impact behaviour of freeze-dried and fresh pomelo (Citrus maxima) peel: influence of the hydration state

PubMed Central

Thielen, Marc; Speck, Thomas; Seidel, Robin

2015-01-01

Pomelos (Citrus maxima) are known for their thick peel which—inter alia—serves as energy dissipator when fruits impact on the ground after being shed. It protects the fruit from splitting open and thus enables the contained seeds to stay germinable and to potentially be dispersed by animal vectors. The main part of the peel consists of a parenchymatous tissue that can be interpreted from a materials point of view as open pored foam whose struts are pressurized and filled with liquid. In order to investigate the influence of the water content on the energy dissipation capacity, drop weight tests were conducted with fresh and with freeze-dried peel samples. Based on the coefficient of restitution it was found that freeze-drying markedly reduces the relative energy dissipation capacity of the peel. Measuring the transmitted force during impact furthermore indicated a transition from a uniform collapse of the foam-like tissue to a progressive collapse due to water extraction. Representing the peel by a Maxwell model illustrates that freeze-drying not only drastically reduces the damping function of the dashpots but also stiffens the springs of the model. PMID:26543566

Postharvest Ultrasound-Assisted Freeze-Thaw Pretreatment Improves the Drying Efficiency, Physicochemical Properties, and Macamide Biosynthesis of Maca (Lepidium meyenii).

PubMed

Chen, Jin-Jin; Gong, Peng-Fei; Liu, Yi-Lan; Liu, Bo-Yan; Eggert, Dawn; Guo, Yuan-Heng; Zhao, Ming-Xia; Zhao, Qing-Sheng; Zhao, Bing

2018-04-01

A novel technique of ultrasound-assisted freeze-thaw pretreatment (UFP) was developed to improve the drying efficiency of maca and bioactive amide synthesis in maca. The optimal UFP conditions are ultrasonic processing 90 min at 30 °C with 6 freeze-thaw cycles. Samples with freeze-thaw pretreatment (FP), ultrasound pretreatment (UP), and UFP were prepared for further comparative study. A no pretreatment (NP) sample was included as a control. The results showed that UFP improved the drying efficiency of maca slices, showing the highest effective moisture diffusivity (1.75 × 10 -9 m 2 /s). This result was further supported by low-field nuclear magnetic resonance (LF-NMR) analysis and scanning electron microscopy (SEM). The rehydration capacity and protein content of maca slices were improved by UFP. More importantly, contents of bioactive macamides and their biosynthetic precursors were increased in 2.5- and 10-fold, respectively. In conclusion, UFP is an efficient technique to improve drying efficiency, physicochemical properties, and bioactive macamides of maca, which can be applied in the industrial manufacture of maca products. © 2018 Institute of Food Technologists®.

Cancer prevention with freeze-dried berries and berry components.

PubMed

Stoner, Gary D; Wang, Li-Shu; Zikri, Nancy; Chen, Tong; Hecht, Stephen S; Huang, Chuanshu; Sardo, Christine; Lechner, John F

2007-10-01

Our laboratory is developing a food-based approach to the prevention of esophageal and colon cancer utilizing freeze-dried berries and berry extracts. Dietary freeze-dried berries were shown to inhibit chemically induced cancer of the rodent esophagus by 30-60% and of the colon by up to 80%. The berries are effective at both the initiation and promotion/progression stages of tumor development. Berries inhibit tumor initiation events by influencing carcinogen metabolism, resulting in reduced levels of carcinogen-induced DNA damage. They inhibit promotion/progression events by reducing the growth rate of pre-malignant cells, promoting apoptosis, reducing parameters of tissue inflammation and inhibiting angiogenesis. On a molecular level, berries modulate the expression of genes involved with proliferation, apoptosis, inflammation and angiogenesis. We have recently initiated clinical trials; results from a toxicity study indicated that freeze-dried black raspberries are well tolerated in humans when administered orally for 7 days at a dose of 45 g per day. Several Phase IIa clinical trials are underway in patients at high risk for esophagus and colon cancer; i.e., Barrett's esophagus, esophageal dysplasia and colonic polyps, to determine if berries will modulate various histological and molecular biomarkers of development of these diseases.

Cancer Prevention with Freeze-dried Berries and Berry Components

PubMed Central

Stoner, Gary D.; Wang, Li-Shu; Zikri, Nancy; Chen, Tong; S. Hecht, Stephen; Huang, Chuanshu; Sardo, Christine; Lechner, John F.

2007-01-01

Our laboratory is developing a food-based approach to the prevention of esophageal and colon cancer utilizing freeze-dried berries and berry extracts. Dietary freeze-dried berries were shown to inhibit chemically-induced cancer of the rodent esophagus by 30-60% and of the colon by up- to 80%. The berries are effective at both the initiation and promotion/progression stages of tumor development. Berries inhibit tumor initiation events by influencing carcinogen metabolism, resulting in reduced levels of carcinogen-induced DNA damage. They inhibit promotion/progression events by reducing the growth rate of premalignant cells, promoting apoptosis, reducing parameters of tissue inflammation and inhibiting angiogenesis. On a molecular level, berries modulate the expression of genes involved with proliferation, apoptosis, inflammation and angiogenesis. We have recently initiated clinical trials; results from a toxicity study indicated that freeze-dried black raspberries are well tolerated in humans when administered orally for 7 days at a dose of 45 grams per day. Several Phase IIa clinical trials are underway in patients at high risk for esophagus and colon cancer; i.e., Barrett’s esophagus, esophageal dysplasia and colonic polyps, to determine if berries will modulate various histological and molecular biomarkers of development of these diseases. PMID:17574861

Pulverization of coffee silverskin extract as a source of antioxidant

NASA Astrophysics Data System (ADS)

Tan, S.; Kusumocahyo, S. P.; Widiputri, D. I.

2016-11-01

Coffee silverskin (CS) is waste from coffee roasting process that has a value as source of antioxidant. In this research, two types of variant coffee Robusta and Arabica CS were extracted for their phenolic content, flavonoid content, and antioxidant activity. The extraction was done at 40°C for 60 minutes using hydroalcoholic solvent. The phenolic, flavonoid content, and antioxidant activity of Robusta CS extract were 816.75 ± 63.24 mg GAE/L and 32.82 ± 2.47 mg QE/L, and 54.80% inhibition respectively, while for Arabica CS extract were 473.51 ± 56.70 mg GAE/L, 18.58 ± 2.47 mg QE/L, and 26.30% inhibition respectively. Thus, the Robusta coffee silverskin extract has higher value of total phenolic content, flavonoid content, and antioxidant activity than Arabica coffee silverskin extract. To produce high antioxidant powder of CS extract, the effect of drying method (freeze drying and spray drying) affecting the phenolic content, flavonoid content, and antioxidant activity was evaluated. The effect of evaporation prior to both drying processes was also evaluated. Evaporation caused up to 23% of total phenolic content degradation. Spray drying resulted in dried CS extract with degradation of total phenolic content up to 17%. On the other hand, freeze drying resulted no major degradation of total phenolic content. However, the coffee silverskin extract can be directly spray dried without evaporation resulting in higher amount of phenolic content in the powder than the one which was evaporated first.

Aripiprazole-Cyclodextrin Binary Systems for Dissolution Enhancement: Effect of Preparation Technique, Cyclodextrin Type and Molar Ratio

PubMed Central

M. Badr-Eldin, Shaimaa; A. Ahmed, Tarek; R Ismail, Hatem

2013-01-01

Objective(s): The aim of this work was to investigate the effect of the natural and the chemically modified form of cyclodextrins namely; β-cyclodextrin (β-CD) and hydroxypropyl-β-cyclodextrin (HP-β-CD) respectively on the solubility and dissolution rate of aripiprazole; an antipsychotic medication showing poor aqueous solubility. Materials and Methods: Phase solubility of aripiprazole with the studied CDs and the complexation efficiency values (CE) which reflect the solubilizing power of the CDs towards the drug was performed. Solid binary systems of aripiprazole with CDs were prepared by kneading, microwave irradiation and freeze-drying techniques at 1:1 and 1:2 (drug to CD) molar ratios. Drug-CD physical mixtures were also prepared in the same molar ratios for comparison. The dissolution of aripiprazole-binary systems was carried out to select the most appropriate CD type, molar ratio and preparation technique. Results: Phase solubility study indicated formation of higher order complexes and the complexation efficiency values was higher for HP-β-CD compared to β-CD. Drug dissolution study revealed that aripiprazole dissolution was increased upon increasing the CD molar ratio and, the freeze-drying technique was superior to the other studied methods especially when combined with the HP-β-CD. The cyclodextrin type, preparation technique and molar ratio exhibited statistically significant effect on the drug dissolution at P≤ 0.05. Conclusion: The freeze-dried system prepared at molar ratio 1:2 (drug: CD) can be considered as efficient tool for enhancing aripiprazole dissolution with the possibility of improving its bioavailability. PMID:24570827

The intrinsically disordered protein LEA7 from Arabidopsis thaliana protects the isolated enzyme lactate dehydrogenase and enzymes in a soluble leaf proteome during freezing and drying.

PubMed

Popova, Antoaneta V; Rausch, Saskia; Hundertmark, Michaela; Gibon, Yves; Hincha, Dirk K

2015-10-01

The accumulation of Late Embryogenesis Abundant (LEA) proteins in plants is associated with tolerance against stresses such as freezing and desiccation. Two main functions have been attributed to LEA proteins: membrane stabilization and enzyme protection. We have hypothesized previously that LEA7 from Arabidopsis thaliana may stabilize membranes because it interacts with liposomes in the dry state. Here we show that LEA7, contrary to this expectation, did not stabilize liposomes during drying and rehydration. Instead, it partially preserved the activity of the enzyme lactate dehydrogenase (LDH) during drying and freezing. Fourier-transform infrared (FTIR) spectroscopy showed no evidence of aggregation of LDH in the dry or rehydrated state under conditions that lead to complete loss of activity. To approximate the complex influence of intracellular conditions on the protective effects of a LEA protein in a convenient in-vitro assay, we measured the activity of two Arabidopsis enzymes (glucose-6-P dehydrogenase and ADP-glucose pyrophosphorylase) in total soluble leaf protein extract (Arabidopsis soluble proteome, ASP) after drying and rehydration or freezing and thawing. LEA7 partially preserved the activity of both enzymes under these conditions, suggesting its role as an enzyme protectant in vivo. Further FTIR analyses indicated the partial reversibility of protein aggregation in the dry ASP during rehydration. Similarly, aggregation in the dry ASP was strongly reduced by LEA7. In addition, mixtures of LEA7 with sucrose or verbascose reduced aggregation more than the single additives, presumably through the effects of the protein on the H-bonding network of the sugar glasses. Copyright © 2015 Elsevier B.V. All rights reserved.

In vitro and in vivo evaluation of a sublingual fentanyl wafer formulation

PubMed Central

Lim, Stephen CB; Paech, Michael J; Sunderland, Bruce; Liu, Yandi

2013-01-01

Background The objective of this study was to prepare a novel fentanyl wafer formulation by a freeze-drying method, and to evaluate its in vitro and in vivo release characteristics, including its bioavailability via the sublingual route. Methods The wafer formulation was prepared by freeze-drying an aqueous dispersion of fentanyl containing sodium carboxymethylcellulose and amylogum as matrix formers. Uniformity of weight, friability, and dissolution testing of the fentanyl wafer was achieved using standard methods, and the residual moisture content was measured. The fentanyl wafer was also examined using scanning electron microscopy and x-ray diffraction. The absolute bioavailability of the fentanyl wafer was evaluated in 11 opioid-naïve adult female patients using a randomized crossover design. Results In vitro release showed that almost 90% of the fentanyl dissolved in one minute. In vivo, the first detectable plasma fentanyl concentration was observed after 3.5 minutes and the peak plasma concentration between 61.5 and 67 minutes. The median absolute bioavailability was 53.0%. Conclusion These results indicate that this wafer has potential as an alternative sublingual fentanyl formulation. PMID:23596347

Mutual Influence of Mannitol and Trehalose on Crystallization Behavior in Frozen Solutions.

PubMed

Jena, Sampreeti; Suryanarayanan, Raj; Aksan, Alptekin

2016-06-01

Phase separation of trehalose during freeze-drying could render it ineffective as a lyoprotectant. The bulking agent, mannitol, on the other hand, should crystallize readily upon freezing. It is therefore imperative to understand the mutual interaction of these sugars during freezing to ensure preservation of the API during freeze-drying. We investigated the effect of mannitol to trehalose ratio (R) on the crystallization behavior of both solutes using Differential Scanning Calorimetry, X-Ray Crystallography and FTIR Spectrosopy during controlled freezing and annealing. When R = 1, crystallization of both mannitol (as hemihydrate) and trehalose (as α-anhydrate) were observed. When R ≥ 1, extent of mannitol crystallization was directly proportional to the value of R. When R < 1, trehalose completely suppressed mannitol crystallization. At R > 1, the freeze concentrate was heterogeneous and characterized by two glass transitions - the lower temperature transition (Tg") attributed to systems containing "extra" unfrozen water. When heated above Tg", crystallization of mannitol and the associated unfrozen water resulted in Tg' (glass transition temperature of the freeze-concentrate). R and not the total solute concentration, dictates the composition of the freeze concentrate as well as the physical stability of the excipients.

The control of ice crystal growth and effect on porous structure of konjac glucomannan-based aerogels.

PubMed

Ni, Xuewen; Ke, Fan; Xiao, Man; Wu, Kao; Kuang, Ying; Corke, Harold; Jiang, Fatang

2016-11-01

Konjac glucomannan (KGM)-based aerogels were prepared using a combination of sol-gel and freeze-drying methods. Preparation conditions were chosen to control ice crystal growth and aerogel structure formation. The ice crystals formed during pre-freezing were observed by low temperature polarizing microscopy, and images of aerogel pores were obtained by scanning electron microscopy. The size of ice crystals were calculated and size distribution maps were drawn, and similarly for aerogel pores. Results showed that ice crystal growth and aerogel pore sizes may be controlled by varying pre-freezing temperatures, KGM concentration and glyceryl monostearate concentration. The impact of pre-freezing temperatures on ice crystal growth was explained as combining ice crystal growth rate with nucleation rate, while the impacts of KGM and glyceryl monostearate concentration on ice crystal growth were interpreted based on their influences on sol network structure. Copyright © 2016 Elsevier B.V. All rights reserved.

Formulation and Stabilization of Francisella tularensis Live Vaccine Strain

PubMed Central

OHTAKE, SATOSHI; MARTIN, RUSSELL A.; SAXENA, ATUL; LECHUGA-BALLESTEROS, DAVID; SANTIAGO, ARACELI E; BARRY, EILEEN M.; TRUONG-LE, VU

2012-01-01

Francisella tularensis live vaccine strain (F. tularensis LVS), a promising vaccine candidate for protection against F. tularensis exposure, is a particularly thermolabile vaccine and difficult to stabilize sufficiently for storage under refrigerated conditions. Our preliminary data show that F. tularensis LVS can be stabilized in the dried state using foam drying, a modified freeze drying method, with sugar-based formulations. The process was conducted under mild drying conditions, which resulted in a good titer retention following processing. The inclusion of osmolytes in the growth media resulted in an acceleration of growth kinetics, although no change in osmotolerance was observed. The optimized F. tularensis formulation, which contained trehalose, gelatin, and Pluronic F68 demonstrated stability for approximately 1.5 weeks at 37°C (i.e., time required for the vaccine to decrease in potency by 1 log10 colony forming unit) and for 12 weeks at 25°C. At refrigerator storage condition (4°C), stabilized F. tularensis LVS vaccine exhibited no activity loss for at least 12 weeks. This stabilization method utilizes conventional freeze dryers and pharmaceutically approved stabilizers, and thus can be readily implemented at many manufacturing sites for large-scale production of stabilized vaccines. The improved heat stability of the F. tularensis LVS could mitigate risks of vaccine potency loss during long-term storage, shipping, and distribution. PMID:21491457

Space Food

NASA Technical Reports Server (NTRS)

1994-01-01

In planning for the long duration Apollo missions, NASA conducted extensive research into space food. One of the techniques developed was freeze drying. Action Products commercialized this technique, concentrating on snack food including the first freeze-dried ice cream. The foods are cooked, quickly frozen and then slowly heated in a vacuum chamber to remove the ice crystals formed by the freezing process. The final product retains 98 percent of its nutrition and weighs only 20 percent of its original weight. Action snacks are sold at museums, NASA facilities and are exported to a number of foreign countries. Sales run to several million dollars annually.

Mechanistic modelling of infrared mediated energy transfer during the primary drying step of a continuous freeze-drying process.

PubMed

Van Bockstal, Pieter-Jan; Mortier, Séverine Thérèse F C; De Meyer, Laurens; Corver, Jos; Vervaet, Chris; Nopens, Ingmar; De Beer, Thomas

2017-05-01

Conventional pharmaceutical freeze-drying is an inefficient and expensive batch-wise process, associated with several disadvantages leading to an uncontrolled end product variability. The proposed continuous alternative, based on spinning the vials during freezing and on optimal energy supply during drying, strongly increases process efficiency and improves product quality (uniformity). The heat transfer during continuous drying of the spin frozen vials is provided via non-contact infrared (IR) radiation. The energy transfer to the spin frozen vials should be optimised to maximise the drying efficiency while avoiding cake collapse. Therefore, a mechanistic model was developed which allows computing the optimal, dynamic IR heater temperature in function of the primary drying progress and which, hence, also allows predicting the primary drying endpoint based on the applied dynamic IR heater temperature. The model was validated by drying spin frozen vials containing the model formulation (3.9mL in 10R vials) according to the computed IR heater temperature profile. In total, 6 validation experiments were conducted. The primary drying endpoint was experimentally determined via in-line near-infrared (NIR) spectroscopy and compared with the endpoint predicted by the model (50min). The mean ratio of the experimental drying time to the predicted value was 0.91, indicating a good agreement between the model predictions and the experimental data. The end product had an elegant product appearance (visual inspection) and an acceptable residual moisture content (Karl Fischer). Copyright © 2017 Elsevier B.V. All rights reserved.

Effect of species, pretreatments, and drying methods on the functional and pasting properties of high-quality yam flour.

PubMed

Wahab, Bashirat A; Adebowale, Abdul-Rasaq A; Sanni, Silifat A; Sobukola, Olajide P; Obadina, Adewale O; Kajihausa, Olatundun E; Adegunwa, Mojisola O; Sanni, Lateef O; Tomlins, Keith

2016-01-01

The study investigated the functional properties of HQYF (high-quality yam flour) from tubers of four dioscorea species. The tubers were processed into HQYF using two pretreatments (potassium metabisulphite: 0.28%, 15 min; blanching: 70°C, 15 min) and drying methods (cabinet: 60°C, 48 h; sun drying: 3 days). Significant differences (P < 0.05) were observed in pasting characteristics of flours among the four species. The drying method significantly affected only the peak viscosity. The interactive effect of species, pretreatment, and drying methods on the functional properties was significant (P < 0.05) except for emulsification capacity, angle of repose, and least gelation concentration. The significant variation observed in most of the functional properties of the HQYF could contribute significantly to breeding programs of the yam species for diverse food applications. The pastes of flour from Dioscorea dumetorum pretreated with potassium metabisulphite and dried under a cabinet dryer were stable compared to other samples, hence will have better applications in products requiring lower retrogradation during freeze/thaw cycles.

A comprehensive laboratory study on the immersion freezing behavior of illite NX particles. A comparison of 17 ice nucleation measurement techniques

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hiranuma, Naruki; Augustin-Bauditz, Stefanie; Bingemer, Heinz

Immersion freezing is the most relevant heterogeneous ice nucleation mechanism through which ice crystals are formed in mixed-phase clouds. In recent years, an increasing number of laboratory experiments utilizing a variety of instruments have examined immersion freezing activity of atmospherically relevant ice-nucleating particles. However, an intercomparison of these laboratory results is a difficult task because investigators have used different ice nucleation (IN) measurement methods to produce these results. A remaining challenge is to explore the sensitivity and accuracy of these techniques and to understand how the IN results are potentially influenced or biased by experimental parameters associated with these techniques.more » Within the framework of INUIT (Ice Nuclei Research Unit), we distributed an illite-rich sample (illite NX) as a representative surrogate for atmospheric mineral dust particles to investigators to perform immersion freezing experiments using different IN measurement methods and to obtain IN data as a function of particle concentration, temperature ( T), cooling rate and nucleation time. A total of 17 measurement methods were involved in the data intercomparison. Experiments with seven instruments started with the test sample pre-suspended in water before cooling, while 10 other instruments employed water vapor condensation onto dry-dispersed particles followed by immersion freezing. The resulting comprehensive immersion freezing data set was evaluated using the ice nucleation active surface-site density, n s, to develop a representative n s( T) spectrum that spans a wide temperature range (-37 °C < T < -11 °C) and covers 9 orders of magnitude in n s. In general, the 17 immersion freezing measurement techniques deviate, within a range of about 8 °C in terms of temperature, by 3 orders of magnitude with respect to n s. In addition, we show evidence that the immersion freezing efficiency expressed in n s of illite NX particles is relatively independent of droplet size, particle mass in suspension, particle size and cooling rate during freezing. A strong temperature dependence and weak time and size dependence of the immersion freezing efficiency of illite-rich clay mineral particles enabled the n s parameterization solely as a function of temperature. We also characterized the n s( T) spectra and identified a section with a steep slope between -20 and -27 °C, where a large fraction of active sites of our test dust may trigger immersion freezing. This slope was followed by a region with a gentler slope at temperatures below -27 °C. While the agreement between different instruments was reasonable below ~ -27 °C, there seemed to be a different trend in the temperature-dependent ice nucleation activity from the suspension and dry-dispersed particle measurements for this mineral dust, in particular at higher temperatures. For instance, the ice nucleation activity expressed in n s was smaller for the average of the wet suspended samples and higher for the average of the dry-dispersed aerosol samples between about -27 and -18 °C. Only instruments making measurements with wet suspended samples were able to measure ice nucleation above -18 °C. A possible explanation for the deviation between -27 and -18 °C is discussed. Multiple exponential distribution fits in both linear and log space for both specific surface area-based n s( T) and geometric surface area-based n s( T) are provided. These new fits, constrained by using identical reference samples, will help to compare IN measurement methods that are not included in the present study and IN data from future IN instruments.« less

A comprehensive laboratory study on the immersion freezing behavior of illite NX particles. A comparison of 17 ice nucleation measurement techniques

DOE PAGES

Hiranuma, Naruki; Augustin-Bauditz, Stefanie; Bingemer, Heinz; ...

2015-03-06

Immersion freezing is the most relevant heterogeneous ice nucleation mechanism through which ice crystals are formed in mixed-phase clouds. In recent years, an increasing number of laboratory experiments utilizing a variety of instruments have examined immersion freezing activity of atmospherically relevant ice-nucleating particles. However, an intercomparison of these laboratory results is a difficult task because investigators have used different ice nucleation (IN) measurement methods to produce these results. A remaining challenge is to explore the sensitivity and accuracy of these techniques and to understand how the IN results are potentially influenced or biased by experimental parameters associated with these techniques.more » Within the framework of INUIT (Ice Nuclei Research Unit), we distributed an illite-rich sample (illite NX) as a representative surrogate for atmospheric mineral dust particles to investigators to perform immersion freezing experiments using different IN measurement methods and to obtain IN data as a function of particle concentration, temperature ( T), cooling rate and nucleation time. A total of 17 measurement methods were involved in the data intercomparison. Experiments with seven instruments started with the test sample pre-suspended in water before cooling, while 10 other instruments employed water vapor condensation onto dry-dispersed particles followed by immersion freezing. The resulting comprehensive immersion freezing data set was evaluated using the ice nucleation active surface-site density, n s, to develop a representative n s( T) spectrum that spans a wide temperature range (-37 °C < T < -11 °C) and covers 9 orders of magnitude in n s. In general, the 17 immersion freezing measurement techniques deviate, within a range of about 8 °C in terms of temperature, by 3 orders of magnitude with respect to n s. In addition, we show evidence that the immersion freezing efficiency expressed in n s of illite NX particles is relatively independent of droplet size, particle mass in suspension, particle size and cooling rate during freezing. A strong temperature dependence and weak time and size dependence of the immersion freezing efficiency of illite-rich clay mineral particles enabled the n s parameterization solely as a function of temperature. We also characterized the n s( T) spectra and identified a section with a steep slope between -20 and -27 °C, where a large fraction of active sites of our test dust may trigger immersion freezing. This slope was followed by a region with a gentler slope at temperatures below -27 °C. While the agreement between different instruments was reasonable below ~ -27 °C, there seemed to be a different trend in the temperature-dependent ice nucleation activity from the suspension and dry-dispersed particle measurements for this mineral dust, in particular at higher temperatures. For instance, the ice nucleation activity expressed in n s was smaller for the average of the wet suspended samples and higher for the average of the dry-dispersed aerosol samples between about -27 and -18 °C. Only instruments making measurements with wet suspended samples were able to measure ice nucleation above -18 °C. A possible explanation for the deviation between -27 and -18 °C is discussed. Multiple exponential distribution fits in both linear and log space for both specific surface area-based n s( T) and geometric surface area-based n s( T) are provided. These new fits, constrained by using identical reference samples, will help to compare IN measurement methods that are not included in the present study and IN data from future IN instruments.« less

Characterisation of crystalline-amorphous blends of sucrose with terahertz-pulsed spectroscopy: the development of a prediction technique for estimating the degree of crystallinity with partial least squares regression.

PubMed

Ermolina, I; Darkwah, J; Smith, G

2014-04-01

The control of the amorphous and crystalline states of drugs and excipients is important in many instances of product formulation, manufacture, and packaging, such as the formulation of certain (freeze-dried) fast melt tablets. This study examines the use of terahertz-pulsed spectroscopy (TPS) coupled with two different data analytical methods as an off-line tool (in the first instance) for assessing the degree of crystallinity in a binary mixture of amorphous and polycrystalline sucrose. The terahertz spectrum of sucrose was recorded in the wave number range between 3 and 100 cm(-1) for both the pure crystalline form and for a mixture of the crystalline and amorphous (freeze-dried) form. The THz spectra of crystalline sucrose showed distinct absorption bands at ∼48, ∼55, and ∼60 cm(-1) while all these features were absent in the amorphous sucrose. Calibration models were constructed based on (1) peak area analysis and (2) partial least square regression analysis, with the latter giving the best LOD and LOQ of 0.76% and 2.3%, respectively. The potential for using THz spectroscopy, as a quantitative in-line tool for percent crystallinity in a range of complex systems such as conventional tablets and freeze-dried formulations, is suggested in this study.

On the Design of a Fuzzy Logic-Based Control System for Freeze-Drying Processes.

PubMed

Fissore, Davide

2016-12-01

This article is focused on the design of a fuzzy logic-based control system to optimize a drug freeze-drying process. The goal of the system is to keep product temperature as close as possible to the threshold value of the formulation being processed, without trespassing it, in such a way that product quality is not jeopardized and the sublimation flux is maximized. The method involves the measurement of product temperature and a set of rules that have been obtained through process simulation with the goal to obtain a unique set of rules for products with very different characteristics. Input variables are the difference between the temperature of the product and the threshold value, the difference between the temperature of the heating fluid and that of the product, and the rate of change of product temperature. The output variables are the variation of the temperature of the heating fluid and the pressure in the drying chamber. The effect of the starting value of the input variables and of the control interval has been investigated, thus resulting in the optimal configuration of the control system. Experimental investigation carried out in a pilot-scale freeze-dryer has been carried out to validate the proposed system. Copyright © 2016 American Pharmacists Association®. Published by Elsevier Inc. All rights reserved.

Beef, chicken and lamb fatty acid analysis--a simplified direct bimethylation procedure using freeze-dried material.

PubMed

Lee, M R F; Tweed, J K S; Kim, E J; Scollan, N D

2012-12-01

When fractionation of meat lipids is not required, procedures such as saponification can be used to extract total fatty acids, reducing reliance on toxic organic compounds. However, saponification of muscle fatty acids is laborious, and requires extended heating times, and a second methylation step to convert the extracted fatty acids to fatty acid methyl esters prior to gas chromatography. Therefore the development of a more rapid direct methylation procedure would be of merit. The use of freeze-dried material for analysis is common and allows for greater homogenisation of the sample. The present study investigated the potential of using freeze-dried muscle samples and a direct bimethylation to analyse total fatty acids of meat (beef, chicken and lamb) in comparison with a saponification procedure followed by bimethylation. Both methods compared favourably for all major fatty acids measured. There was a minor difference in relation to the C18:1 trans 10 isomer with a greater (P<0.05) recovery with saponification. However, numerically the difference was small and likely as a result of approaching the limits of isomer identification by single column gas chromatography. Differences (P<0.001) between species were found for all fatty acids measured with no interaction effects. The described technique offers a simplified, quick and reliable alternative to saponification to analyse total fatty acids from muscle samples. Copyright © 2012 Elsevier Ltd. All rights reserved.

Antimicrobial eugenol nanoemulsion prepared by gum arabic and lecithin and evaluation of drying technologies.

PubMed

Hu, Qiaobin; Gerhard, Hannah; Upadhyaya, Indu; Venkitanarayanan, Kumar; Luo, Yangchao

2016-06-01

The purpose of present work was to develop eugenol oil nanoemulsions using gum arabic and lecithin as food grade natural emulsifiers, and study their antimicrobial activity. In addition, our study also evaluated different drying techniques (spray drying and freeze drying) on the morphology and redispersibility of nanoemulsion powders. The optimal fabrication method, physicochemical and structural characterization, stability, and antimicrobial activity were investigated. Results showed that nanoemusions with a particle size of 103.6±7.5nm were obtained by mixing aqueous phase (0.5% gum arabic, 0.5% lecithin, w/v) and eugenol oil (1.25%, w/v), which was premixed with ethanol (as a co-surfactant), followed by high speed homogenization process. The molecular interactions among emulsifiers and eugenol were evidenced by Fourier transform infrared spectroscopy. Buchi B-90 Nano Spray Dryer was evaluated as a powerful tool to obtain ultrafine spherical powders with a size of less than 500nm, compared to flake-like aggregation obtained by freeze-drying. The dried powders exhibited excellent re-dispersibility in water and maintained their physicochemical properties after re-hydration. The nanoemulsions did not adversely affect the antimicrobial activity of eugenol against Listeria monocytogenes and Salmonella Enteritidis. Therefore, the nanoemulsions have the potential to be applied in the food industry as a food preservative or sanitizer. Copyright © 2016 Elsevier B.V. All rights reserved.

The Effect of Freeze-Drying on the Nutrient, Polyphenol, and Oxidant Levels of Breast Milk.

PubMed

Cortez, Mariela Valentina; Soria, Elio Andrés

2016-12-01

Human milk banks need to extend the suitability of milk for breastfeeding, and for this technological advances are required. Our aim was to establish the capacity of freeze-drying to conserve milk properties without further oxidative deterioration. One hundred sixteen healthy women participated from the city of Cordoba (Argentina). Proteins, glucose, triglycerides, polyphenols, and markers (nitrites, superoxide anion, hydroperoxides, lipoperoxides, and γ-glutamyl transpeptidase) were measured in their fresh milk. Samples were then separated for three treatments as follows: freezing and conservation for 6 months at -80°C (F: positive control); freeze-drying for 24 hours at ≤-70°C and ≤1.33 Pa and conservation for 6 months at 4°C (FD: treatment of interest); and freeze-drying for 24 hours at ≤-70°C and ≤1.33 Pa and conservation for 6 months at -80°C (FD+F). Next, analyses were repeated and compared by ANOVA and Tukey tests. Fresh milk showed these values per L as follows: proteins: 12.62 ± 2.51 g, glucose: 4.44 ± 0.25 g, triglycerides: 34.26 ± 0.59 g, polyphenols: 53.27 ± 8.67 mg, nitrites: 62.40 ± 19.09 mg, superoxide: 3,721.02 ± 198.80 OD, hydroperoxides: 7,343.76 ± 294.53 OD, lipoperoxides: 7,349.72 ± 398.72 OD, and γ-glutamyl transpeptidase: 4.66 ± 0.55 IU. Glucose was decreased after F treatment (p < 0.05), all variables were conserved by FD and were not improved by the FD + F combination. Freeze-drying achieved suitable conservation and may improve bank functioning, by protecting nutritional properties, polyphenol-related functionality, and oxidative integrity of human milk through a 1-day treatment with easy maintenance.

Reverse freeze casting: a new method for fabricating highly porous titanium scaffolds with aligned large pores.

PubMed

Yook, Se-Won; Jung, Hyun-Do; Park, Chang-Hoon; Shin, Kwan-Ha; Koh, Young-Hag; Estrin, Yuri; Kim, Hyoun-Ee

2012-07-01

Highly porous titanium with aligned large pores up to 500 μm in size, which is suitable for scaffold applications, was successfully fabricated using the reverse freeze casting method. In this process we have newly developed, the Ti powders migrated spontaneously along the pre-aligned camphene boundaries at a temperature of 45.5°C and formed a titanium-camphene mixture with an aligned structure; this was followed by freeze drying and sintering. As the casting time increased from 24 to 48 h, the initial columnar structures turned into lamellar structures, with the porosity decreasing from 69 to 51%. This reduction in porosity caused the compressive yield strength to increase from 121 to 302 MPa, with an elastic modulus of the samples being in the range of 2-5 GPa. In addition, it was demonstrated that reverse freeze casting can also be successfully applied to various other raw powders, suggesting that the method developed in this work opens up new avenues for the production of a range of porous metallic and ceramic scaffolds with highly aligned pores. Copyright © 2012 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

ESR detection procedure of irradiated papaya containing high water content

NASA Astrophysics Data System (ADS)

Kikuchi, Masahiro; Shimoyama, Yuhei; Ukai, Mitsuko; Kobayashi, Yasuhiko

2011-05-01

ESR signals were recorded from irradiated papaya at liquid nitrogen temperature (77 K), and freeze-dried irradiated papaya at room temperature (295 K). Two side peaks from the flesh at the liquid nitrogen temperature indicated a linear dose response for 3-14 days after the γ-irradiation. The line shapes recorded from the freeze-dried specimens were sharper than those at liquid nitrogen temperature.

A simple, field-friendly technique for cryopreserving semen from Asian elephants (Elephas maximus).

PubMed

Arnold, Danielle M; Gray, Charlie; Roth, Terri L; Mitchell, Sebastian; Graham, Laura H

2017-07-01

The specific objectives of the present study were to investigate the effects of manual seeding, differing freeze and thaw rates as well as storage for 24h at 4°C prior to cryopreservation on post-thaw sperm quality in Asian elephants. Extended semen was cooled in an equitainer to 4°C, frozen in liquid nitrogen vapour at various rates with and without manual seeding or in a dry shipper and thawed at 37, 50 and 75°C. There was a significant effect of freeze rate on post-thaw motility (P<0.0001) and acrosomal integrity (P<0.005). The faster freeze rates in the dry shipper and at 1cm or 2cm above liquid nitrogen consistently provided better cryopreservation than slower freezing rates. Thaw temperature had no effect on post-thaw semen quality but there was an interaction between freeze and thaw rates with higher thaw rates resulting in superior post-thaw semen quality in straws frozen at fast rates. Storage of samples prior to freezing had a detrimental effect on post-thaw semen quality. In summary, our results indicate cooling extended semen in an equitainer and cryopreserving it by placing straws directly in a dry shipper is a simple technique for effectively cryopreserving Asian elephant semen in the field or zoo. Copyright © 2017 Elsevier B.V. All rights reserved.

Effect of Controlled Ice Nucleation on Stability of Lactate Dehydrogenase During Freeze-Drying.

PubMed

Fang, Rui; Tanaka, Kazunari; Mudhivarthi, Vamsi; Bogner, Robin H; Pikal, Michael J

2018-03-01

Several controlled ice nucleation techniques have been developed to increase the efficiency of the freeze-drying process as well as to improve the quality of pharmaceutical products. Owing to the reduction in ice surface area, these techniques have the potential to reduce the degradation of proteins labile during freezing. The objective of this study was to evaluate the effect of ice nucleation temperature on the in-process stability of lactate dehydrogenase (LDH). LDH in potassium phosphate buffer was nucleated at -4°C, -8°C, and -12°C using ControLyo™ or allowed to nucleate spontaneously. Both the enzymatic activity and tetramer recovery after freeze-thawing linearly correlated with product ice nucleation temperature (n = 24). Controlled nucleation also significantly improved batch homogeneity as reflected by reduced inter-vial variation in activity and tetramer recovery. With the correlation established in the laboratory, the degradation of protein in manufacturing arising from ice nucleation temperature differences can be quantitatively predicted. The results show that controlled nucleation reduced the degradation of LDH during the freezing process, but this does not necessarily translate to vastly superior stability during the entire freeze-drying process. The capability of improving batch homogeneity provides potential advantages in scaling-up from lab to manufacturing scale. Copyright © 2018 American Pharmacists Association®. Published by Elsevier Inc. All rights reserved.

The influence of phosphorylation and freezing temperature on the mechanical properties of hydroxyapatite/chitosan composite as bone scaffold biomaterial

NASA Astrophysics Data System (ADS)

Albab, Muh Fadhil; Giovani, Nicholas; Yuwono, Akhmad Herman; Sofyan, Nofrijon; Ramahdita, Ghiska; Whulanza, Yudan

2018-02-01

Biomaterials composite of hydroxyapatite/chitosan is a preeminent material for medical applications including bone scaffold. To improve its mechanical properties, the chitosan as the matrix needs to be modified with particular chemical agents. One of the methods is phosphorylation of chitosan by using orthophosphoric acid prior to the biomaterials fabrication. In the current study, biomaterials with the weight composition of 70% hydroxyapatite (HA) and 30% phosphorylated chitosan have been fabricated using thermally induced phase separation (TIPS) method with freezing temperature variation of -20, -30, -40 and -80°C prior to three day-freeze drying. The results obtained by this work showed that the highest compression modulus of 376.9 kPa, highest compressive strength of 38.4 kPa and biggest pore size of 48.24 µm were achieved in the freezing temperature of -20°C. In comparison to non-phosphorylated chitosan/hydroxyapatite, the modification of chitosan using orthophosphoric acid in this work has been found to increase the compressive strength of composite up to 5.5 times.

Impact of Ice Morphology on Design Space of Pharmaceutical Freeze-Drying.

PubMed

Goshima, Hiroshika; Do, Gabsoo; Nakagawa, Kyuya

2016-06-01

It has been known that the sublimation kinetics of a freeze-drying product is affected by its internal ice crystal microstructures. This article demonstrates the impact of the ice morphologies of a frozen formulation in a vial on the design space for the primary drying of a pharmaceutical freeze-drying process. Cross-sectional images of frozen sucrose-bovine serum albumin aqueous solutions were optically observed and digital pictures were acquired. Binary images were obtained from the optical data to extract the geometrical parameters (i.e., ice crystal size and tortuosity) that relate to the mass-transfer resistance of water vapor during the primary drying step. A mathematical model was used to simulate the primary drying kinetics and provided the design space for the process. The simulation results predicted that the geometrical parameters of frozen solutions significantly affect the design space, with large and less tortuous ice morphologies resulting in wide design spaces and vice versa. The optimal applicable drying conditions are influenced by the ice morphologies. Therefore, owing to the spatial distributions of the geometrical parameters of a product, the boundary curves of the design space are variable and could be tuned by controlling the ice morphologies. Copyright © 2016 American Pharmacists Association®. Published by Elsevier Inc. All rights reserved.

Freeze-dried Lactobacillus plantarum 299v increases iron absorption in young females—Double isotope sequential single-blind studies in menstruating women

PubMed Central

Önning, Gunilla; Hulthén, Lena

2017-01-01

Background The probiotic strain Lactobacillus plantarum 299v has earlier been shown to increase iron absorption when added to foods. However, it is not known if the same probiotic strain in a freeze-dried format included in a capsule increases the iron absorption. Objective The aim of this study was to test the hypotheses that non-heme iron absorption from a light meal is promoted by a simultaneous intake of freeze-dried Lactobacillus plantarum 299v (Lp299v, DSM 9843). Study design With a single blinded placebo controlled sequential design, iron absorption from a light breakfast meal administered with or without capsules containing 1010 cfu freeze-dried Lp299v was studied in healthy female volunteers of fertile age. The methodology used was a double isotope technique (59Fe and 55Fe). Two studies were performed using the same protocol. Results In study 1, the absorption of iron from a meal without Lp299v was found to be 17.4 ± 13.4%, and from an identical meal with Lp299v was found to be 22.4 ± 17.3% (mean ± SD). This difference was statistically significant (p = 0.040, n = 14). In study 2, the absorption of iron from a meal without Lp299v was found to be 20.9 ± 13.1%, and from an identical meal with Lp299v found to be 24.5 ± 12.0% (mean ± SD, n = 28), which again was statistically significant (p = 0.003). Conclusion Freeze-dried Lp299v enhances the absorption of iron when administered together with a meal with a high iron bioavailability. Trial registration ClinicalTrials.gov Identifier: NCT02131870 PMID:29236734

Application of Optical Coherence Tomography Freeze-Drying Microscopy for Designing Lyophilization Process and Its Impact on Process Efficiency and Product Quality.

PubMed

Korang-Yeboah, Maxwell; Srinivasan, Charudharshini; Siddiqui, Akhtar; Awotwe-Otoo, David; Cruz, Celia N; Muhammad, Ashraf

2018-01-01

Optical coherence tomography freeze-drying microscopy (OCT-FDM) is a novel technique that allows the three-dimensional imaging of a drug product during the entire lyophilization process. OCT-FDM consists of a single-vial freeze dryer (SVFD) affixed with an optical coherence tomography (OCT) imaging system. Unlike the conventional techniques, such as modulated differential scanning calorimetry (mDSC) and light transmission freeze-drying microscopy, used for predicting the product collapse temperature (Tc), the OCT-FDM approach seeks to mimic the actual product and process conditions during the lyophilization process. However, there is limited understanding on the application of this emerging technique to the design of the lyophilization process. In this study, we investigated the suitability of OCT-FDM technique in designing a lyophilization process. Moreover, we compared the product quality attributes of the resulting lyophilized product manufactured using Tc, a critical process control parameter, as determined by OCT-FDM versus as estimated by mDSC. OCT-FDM analysis revealed the absence of collapse even for the low protein concentration (5 mg/ml) and low solid content formulation (1%w/v) studied. This was confirmed by lab scale lyophilization. In addition, lyophilization cycles designed using Tc values obtained from OCT-FDM were more efficient with higher sublimation rate and mass flux than the conventional cycles, since drying was conducted at higher shelf temperature. Finally, the quality attributes of the products lyophilized using Tc determined by OCT-FDM and mDSC were similar, and product shrinkage and cracks were observed in all the batches of freeze-dried products irrespective of the technique employed in predicting Tc.

A Meta-analysis of Studies Comparing Outcomes of Diverse Acellular Dermal Matrices for Implant-Based Breast Reconstruction.

PubMed

Lee, Kyeong-Tae; Mun, Goo-Hyun

2017-07-01

The current diversity of the available acellular dermal matrix (ADM) materials for implant-based breast reconstruction raises the issue of whether there are any differences in postoperative outcomes according to the kind of ADM used. The present meta-analysis aimed to investigate whether choice of ADM products can affect outcomes. Studies that used multiple kinds of ADM products for implant-based breast reconstruction and compared outcomes between them were searched. Outcomes of interest were rates of postoperative complications: infection, seroma, mastectomy flap necrosis, reconstruction failure, and overall complications. A total of 17 studies met the selection criteria. There was only 1 randomized controlled trial, and the other 16 studies had retrospective designs. Comparison of FlexHD, DermaMatrix, and ready-to-use AlloDerm with freeze-dried AlloDerm was conducted in multiple studies and could be meta-analyzed, in which 12 studies participated. In the meta-analysis comparing FlexHD and freeze-dried AlloDerm, using the results of 6 studies, both products showed similar pooled risks for all kinds of complications. When comparing DermaMatrix and freeze-dried AlloDerm with the results from 4 studies, there were also no differences between the pooled risks of complications of the two. Similarly, the meta-analysis of 4 studies comparing ready-to-use and freeze-dried AlloDerm demonstrated that the pooled risks for the complications did not differ. This meta-analysis demonstrates that the 3 recently invented, human cadaveric skin-based products of FlexHD, DermaMatrix, and ready-to-use AlloDerm have similar risks of complications compared with those of freeze-dried AlloDerm, which has been used for longer. However, as most studies had low levels of evidence, further investigations are needed.

Effect of several food ingredients on radiation inactivation of Escherichia coli and Listeria monocytogenes inoculated into ground pork

NASA Astrophysics Data System (ADS)

Yun, Hyejeong; Lacroix, Monique; Jung, Samooel; Kim, Keehyuk; Lee, Ju Woon; Jo, Cheorun

2011-09-01

The objective of this study was to examine the effects of several food ingredients on the relative radiation sensitivity (RRS) of Escherichia coli and Listeria monocytogenes inoculated onto ground pork. Garlic, leek, onion, and ginger were prepared in 3 different forms; pressurized, freeze-dried, and 70% ethanol extracted. The prepared food ingredients were subdivided into 2 groups, non-irradiated and irradiated with 5 kGy of gamma irradiation, before addition to ground pork. The prepared food ingredients were added at concentrations of 1% and 5% (w/w) into radiation-sterilized ground pork and inoculated with E. coli and L. monocytogenes (10 6 CFU/mL). For E. coli inoculated pork, the most efficient ingredient was ethanol extracted leek (RRS=3.89), followed by freeze-dried ginger and leek (RRS=3.66 and 3.63, respectively) when used without pasteurization. However, when the food ingredients were irradiation-pasteurized, the freeze-dried ginger showed the highest RRS (4.10). When 5% natural materials were added, RRS was the highest for freeze-dried and ethanol extracted onion (4.44 and 4.65, respectively). For L. monocytogenes, the RRS was relatively lower than E. coli in general. The most efficient material was pressurized and freeze-dried onion (RRS=2.13 and 2.08, respectively) at a concentration of 1%. No increase in RRS was observed at increased concentration of food ingredients. These results suggest that the addition of particular food ingredients increased the efficiency of radiation-sterilization. However, changes in RRS were dependent on the species of microorganism as well as the form of the food ingredients.

Comparison of different drying methods on the physical properties, bioactive compounds and antioxidant activity of raspberry powders.

PubMed

Si, Xu; Chen, Qinqin; Bi, Jinfeng; Wu, Xinye; Yi, Jianyong; Zhou, Linyan; Li, Zhaolu

2016-04-01

Dehydration has been considered as one of the traditional but most effective techniques for perishable fruits. Raspberry powders obtained after dehydration can be added as ingredients into food formulations such as bakery and dairy products. In this study, raspberry powders obtained by hot air drying (HAD), infrared radiation drying (IRD), hot air and explosion puffing drying (HA-EPD), infrared radiation and microwave vacuum drying (IR-MVD) and freeze drying (FD) were compared on physical properties, bioactive compounds and antioxidant activity. Drying techniques affected the physical properties, bioactive compounds and antioxidant activity of raspberry powders greatly. FD led to significantly higher (P < 0.05) values of water solubility (45.26%), soluble solid (63.46%), hygroscopicity (18.06%), color parameters and anthocyanin retention (60.70%) of raspberry powder compared with other drying methods. However, thermal drying techniques, especially combined drying methods, were superior to FD in final total polyphenol content, total flavonoid content and antioxidant activity. The combined drying methods, especially IR-MVD, showed the highest total polyphenol content (123.22 g GAE kg(-1) dw) and total flavonoid content (0.30 g CAE kg(-1) dw). Additionally, IR-MVD performed better in antioxidant activity retention. Overall, combined drying methods, especially IR-MVD, were found to result in better quality of raspberry powders among the thermal drying techniques. IR-MVD could be recommended for use in the drying industry because of its advantages in time saving and nutrient retention. © 2015 Society of Chemical Industry.

Antioxidant capacities and anti-inflammatory effects of flavonoid compounds isolated from acai pulp (Euterpe oleracea Mart.)

USDA-ARS?s Scientific Manuscript database

Acai fruit (Euterpe oleracea Mart.) has been demonstrated to exhibit extremely high antioxidant capacity. Seven major flavonoids were isolated from freeze-dried acai pulp by various chromatographic methods. Their structures were elucidated as orientin (1), homoorientin (2), vitexin (3), luteolin (4)...

Antioxidant capacities of seven flavonoid compounds isolated from pulp of acai fruit (Euterpe oleracea)

USDA-ARS?s Scientific Manuscript database

The pulp of açai fruit (Euterpe oleracea Mart.) has been demonstrated to exhibit extremely high antioxidant capacity. Seven major flavonoids were isolated from freeze-dried acai pulp by various chromatographic methods. Their structures were elucidated as orientin (1), homoorientin (2), vitexin (3), ...

Particulate contamination from siliconized rubber closures for freeze drying.

PubMed

Gebhardt, U; Grumbridge, N A; Knoch, A

1996-01-01

It can be shown that siliconized closures for freeze drying may cause the opalescence and turbidity observed in freeze-dried products after reconstitution. Closures of different rubber composition show different intensities of turbidity when treated identically with the same quantity and type of silicone oil. Clear solutions are obtained after reconstitution if ETFE-coated closures are used instead of siliconized closures. Samples stored at 4 degrees C for up to 6 months show no change in the intensity of turbidity, while the turbidity of samples manufactured with siliconized closures and stored at higher temperatures increase with time. Samples with ETFE-coated closures show clear solutions when stored at 25 degrees C and 37 degrees C for up to 6 months and at 45 degrees C for 3 months. After 6 months only a very weak opalescence could be observed in these samples.

Freezing and fractionation: effects of preservation on carbon and nitrogen stable isotope ratios of some limnetic organisms.

PubMed

Wolf, J Marshall; Johnson, Brett; Silver, Douglas; Pate, William; Christianson, Kyle

2016-03-15

Stable isotopes of carbon and nitrogen have become important natural tracers for studying food-web structure and function. Considerable research has demonstrated that chemical preservatives and fixatives shift the isotopic ratios of aquatic organisms. Much less is known about the effects of freezing as a preservation method although this technique is commonly used. We conducted a controlled experiment to test the effects of freezing (-10 °C) and flash freezing (–79 °C) on the carbon and nitrogen isotope ratios of zooplankton (Cladocera), Mysis diluviana and Rainbow Trout (Oncorhynchus mykiss). Subsamples (~0.5 mg) of dried material were analyzed for percentage carbon, percentage nitrogen, and the relative abundance of stable carbon and nitrogen isotopes (δ13C and δ15N values) using a Carlo Erba NC2500 elemental analyzer interfaced to a ThermoFinnigan MAT Delta Plus isotope ratio mass spectrometer. The effects of freezing were taxon-dependent. Freezing had no effect on the isotopic or elemental values of Rainbow Trout muscle. Effects on the δ13C and δ15N values of zooplankton and Mysis were statistically significant but small relative to typical values of trophic fractionation. The treatment-control offsets had larger absolute values for Mysis (δ13C: ≤0.76 ± 0.41‰, δ15N: ≤0.37 ± 0.16‰) than for zooplankton (δ13C: ≤0.12 ± 0.06‰, δ15N: ≤0.30 ± 0.27‰). The effects of freezing were more variable for the δ13C values of Mysis, and more variable for the δ15N values of zooplankton. Generally, both freezing methods reduced the carbon content of zooplankton and Mysis, but freezing had a negative effect on the %N of zooplankton and a positive effect on the %N of Mysis. The species-dependencies and variability of freezing effects on aquatic organisms suggest that more research is needed to understand the mechanisms responsible for freezing-related fractionation before standardized protocols for freezing as a preservation method can be adopted.

Development of Biodegradable Polycation-Based Inhalable Dry Gene Powders by Spray Freeze Drying

PubMed Central

Okuda, Tomoyuki; Suzuki, Yumiko; Kobayashi, Yuko; Ishii, Takehiko; Uchida, Satoshi; Itaka, Keiji; Kataoka, Kazunori; Okamoto, Hirokazu

2015-01-01

In this study, two types of biodegradable polycation (PAsp(DET) homopolymer and PEG-PAsp(DET) copolymer) were applied as vectors for inhalable dry gene powders prepared by spray freeze drying (SFD). The prepared dry gene powders had spherical and porous structures with a 5~10-μm diameter, and the integrity of plasmid DNA could be maintained during powder production. Furthermore, it was clarified that PEG-PAsp(DET)-based dry gene powder could more sufficiently maintain both the physicochemical properties and in vitro gene transfection efficiencies of polyplexes reconstituted after powder production than PAsp(DET)-based dry gene powder. From an in vitro inhalation study using an Andersen cascade impactor, it was demonstrated that the addition of l-leucine could markedly improve the inhalation performance of dry powders prepared by SFD. Following pulmonary delivery to mice, both PAsp(DET)- and PEG-PAsp(DET)-based dry gene powders could achieve higher gene transfection efficiencies in the lungs compared with a chitosan-based dry gene powder previously reported by us. PMID:26343708

Optimization of resistant starch formation from high amylose corn starch by microwave irradiation treatments and characterization of starch preparations.

PubMed

Mutlu, Selime; Kahraman, Kevser; Öztürk, Serpil

2017-02-01

The effects of microwave irradiation on resistant starch (RS) formation and functional properties in high-amylose corn starch, Hylon VII, by applying microwave-storing cycles and drying processes were investigated. The Response Surface Methodology (RSM) was used to optimize the reaction conditions, microwave time (2-4min) and power (20-100%), for RS formation. The starch:water (1:10) mixtures were cooked and autoclaved and then different microwave-storing cycles and drying (oven or freeze drying) processes were applied. The RS contents of the samples increased with increasing microwave-storing cycle. The highest RS (43.4%) was obtained by oven drying after 3 cycles of microwave treatment at 20% power for 2min. The F, p (<0.05) and R 2 values indicated that the selected models were consistent. Linear equations were obtained for oven-dried samples applied by 1 and 3 cycles of microwave with regression coefficients of 0.65 and 0.62, respectively. Quadratic equation was obtained for freeze-dried samples applied by 3 cycles of microwave with a regression coefficient of 0.83. The solubility, water binding capacity (WBC) and RVA viscosity values of the microwave applied samples were higher than those of native Hylon VII. The WBC and viscosity values of the freeze-dried samples were higher than those of the oven-dried ones. Copyright © 2016 Elsevier B.V. All rights reserved.

Soil drying procedure affects the DNA quantification of Lactarius vinosus but does not change the fungal community composition.

PubMed

Castaño, Carles; Parladé, Javier; Pera, Joan; Martínez de Aragón, Juan; Alday, Josu G; Bonet, José Antonio

2016-11-01

Drying soil samples before DNA extraction is commonly used for specific fungal DNA quantification and metabarcoding studies, but the impact of different drying procedures on both the specific fungal DNA quantity and the fungal community composition has not been analyzed. We tested three different drying procedures (freeze-drying, oven-drying, and room temperature) on 12 different soil samples to determine (a) the soil mycelium biomass of the ectomycorrhizal species Lactarius vinosus using qPCR with a specifically designed TaqMan® probe and (b) the fungal community composition and diversity using the PacBio® RS II sequencing platform. Mycelium biomass of L. vinosus was significantly greater in the freeze-dried soil samples than in samples dried at oven and room temperature. However, drying procedures had no effect on fungal community composition or on fungal diversity. In addition, there were no significant differences in the proportions of fungi according to their functional roles (moulds vs. mycorrhizal species) in response to drying procedures. Only six out of 1139 operational taxonomic units (OTUs) had increased their relative proportions after soil drying at room temperature, with five of these OTUs classified as mould or yeast species. However, the magnitude of these changes was small, with an overall increase in relative abundance of these OTUs of approximately 2 %. These results suggest that DNA degradation may occur especially after drying soil samples at room temperature, but affecting equally nearly all fungi and therefore causing no significant differences in diversity and community composition. Despite the minimal effects caused by the drying procedures at the fungal community composition, freeze-drying resulted in higher concentrations of L. vinosus DNA and prevented potential colonization from opportunistic species.

The relevance of the amorphous state to pharmaceutical dosage forms: glassy drugs and freeze dried systems.

PubMed

Craig, D Q; Royall, P G; Kett, V L; Hopton, M L

1999-03-15

Many pharmaceuticals, either by accident or design, may exist in a total or partially amorphous state. Consequently, it is essential to have an understanding of the physico-chemical principles underpinning the behaviour of such systems. In this discussion, the nature of the glassy state will be described, with particular emphasis on the molecular processes associated with glass transitional behaviour and the use of thermal methods for characterising the glass transition temperature, Tg. The practicalities of such measurements, the significance of the accompanying relaxation endotherm and plasticization effects are considered. The advantages and difficulties associated with the use of amorphous drugs will be outlined, with discussion given regarding the problems associated with physical and chemical stability. Finally, the principles of freeze drying will be described, including discussion of the relevance of glass transitional behaviour to product stability. Copyright

Stability and cellular responses to fluorapatite-collagen composites.

PubMed

Yoon, Byung-Ho; Kim, Hae-Won; Lee, Su-Hee; Bae, Chang-Jun; Koh, Young-Hag; Kong, Young-Min; Kim, Hyoun-Ee

2005-06-01

Fluorapatite (FA)-collagen composites were synthesized via a biomimetic coprecipitation method in order to improve the structural stability and cellular responses. Different amounts of ammonium fluoride (NH4F), acting as a fluorine source for FA, were added to the precipitation of the composites. The precipitated composites were freeze-dried and isostatically pressed in a dense body. The added fluorine was incorporated nearly fully into the apatite structure (fluoridation), and a near stoichiometric FA-collagen composite was obtained with complete fluoridation. The freeze-dried composites had a typical biomimetic network, consisting of collagen fibers and precipitates of nano-sized apatite crystals. The human osteoblast-like cells on the FA-collagen composites exhibited significantly higher proliferation and differentiation (according to alkaline phosphatase activity) than those on the hydroxyapatite-collagen composite. These enhanced osteoblastic cell responses were attributed to the fluorine release and the reduced dissolution rate.

Freeze-drying synthesis of three-dimensional porous LiFePO4 modified with well-dispersed nitrogen-doped carbon nanotubes for high-performance lithium-ion batteries

NASA Astrophysics Data System (ADS)

Tu, Xiaofeng; Zhou, Yingke; Song, Yijie

2017-04-01

The three-dimensional porous LiFePO4 modified with uniformly dispersed nitrogen-doped carbon nanotubes has been successfully prepared by a freeze-drying method. The morphology and structure of the porous composites are characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS), and the electrochemical performances are evaluated using the constant current charge/discharge tests, cyclic voltammetry and electrochemical impedance spectroscopy. The nitrogen-doped carbon nanotubes are uniformly dispersed inside the porous LiFePO4 to construct a superior three-dimensional conductive network, which remarkably increases the electronic conductivity and accelerates the diffusion of lithium ion. The porous composite displays high specific capacity, good rate capability and excellent cycling stability, rendering it a promising positive electrode material for high-performance lithium-ion batteries.

Through-vial impedance spectroscopy of the mechanisms of annealing in the freeze-drying of maltodextrin: the impact of annealing hold time and temperature on the primary drying rate.

PubMed

Smith, Geoff; Arshad, Muhammad Sohail; Polygalov, Eugene; Ermolina, Irina

2014-06-01

The study aims to investigate the impact of annealing hold time and temperature on the primary drying rate/duration of a 10% (w/v) solution of maltodextrin with an emphasis on how the mechanisms of annealing might be understood from the in-vial measurements of the ice crystal growth and the glass transition. The electrical impedance of the solution within a modified glass vial was recorded between 10 and 10(6) Hz during freeze-drying cycles with varying annealing hold times (1-5 h) and temperatures. Primary drying times decreased by 7%, 27% and 34% (1.1, 4.3 and 5.5 h) with the inclusion of an annealing step at temperatures of -15°C, -10°C and -5°C, respectively. The glass transition was recorded at approximately -16°C during the re-heating and re-cooling steps, which is close to the glass transition (Tg ') reported for 10% (w/v) maltodextrin and therefore indicates that a maximum freeze concentration (∼86%, w/w, from the Gordon-Taylor equation) was achieved during first freezing, with no further ice being formed on annealing. This observation, coupled to the decrease in electrical resistance that was observed during the annealing hold time, suggests that the reduction in the drying time was because of improved connectivity of ice crystals because of Ostwald ripening rather than devitrification. © 2014 Wiley Periodicals, Inc. and the American Pharmacists Association.

Predicting glycogen concentration in the foot muscle of abalone using near infrared reflectance spectroscopy (NIRS).

PubMed

Fluckiger, Miriam; Brown, Malcolm R; Ward, Louise R; Moltschaniwskyj, Natalie A

2011-06-15

Near infrared reflectance spectroscopy (NIRS) was used to predict glycogen concentrations in the foot muscle of cultured abalone. NIR spectra of live, shucked and freeze-dried abalones were modelled against chemically measured glycogen data (range: 0.77-40.9% of dry weight (DW)) using partial least squares (PLS) regression. The calibration models were then used to predict glycogen concentrations of test abalone samples and model robustness was assessed from coefficient of determination of the validation (R2(val)) and standard error of prediction (SEP) values. The model for freeze-dried abalone gave the best prediction (R2(val) 0.97, SEP=1.71), making it suitable for quantifying glycogen. Models for live and shucked abalones had R2(val) of 0.86 and 0.90, and SEP of 3.46 and 3.07 respectively, making them suitable for producing estimations of glycogen concentration. As glycogen is a taste-active component associated with palatability in abalone, this study demonstrated the potential of NIRS as a rapid method to monitor the factors associated with abalone quality. Copyright © 2011 Elsevier Ltd. All rights reserved.

Controlling the physical form of mannitol in freeze-dried systems.

PubMed

Mehta, Mehak; Bhardwaj, Sunny P; Suryanarayanan, Raj

2013-10-01

A potential drawback with the use of mannitol as a bulking agent is its existence as mannitol hemihydrate (MHH; C₆H₁₄O₆·0.5H₂O) in the lyophile. Once formed during freeze-drying, MHH dehydration may require secondary drying under aggressive conditions which can be detrimental to the stability of thermolabile components. If MHH is retained in the lyophile, the water released by MHH dehydration during storage has the potential to cause product instability. We systematically identified the conditions under which anhydrous mannitol and MHH crystallized in frozen systems with the goal of preventing MHH formation during freeze-drying. When mannitol solutions were cooled, the temperature of solute crystallization was the determinant of the physical form of mannitol. Based on low temperature X-ray diffractometry (using both laboratory and synchrotron sources), MHH formation was observed when solute crystallization occurred at temperatures ≤ -20 °C, while anhydrous mannitol crystallized at temperatures ≤ -10 °C. The transition temperature (anhydrate - MHH) appears to be ∼-15 °C. The use of a freeze-dryer with controlled ice nucleation technology enabled anhydrous mannitol crystallization at ∼-5 °C. Thus, ice crystallization followed by annealing at temperatures ≤ -10 °C can be an effective strategy to prevent MHH formation. Copyright © 2013 Elsevier B.V. All rights reserved.

Fuzzy Logic-based expert system for evaluating cake quality of freeze-dried formulations.

PubMed

Trnka, Hjalte; Wu, Jian X; Van De Weert, Marco; Grohganz, Holger; Rantanen, Jukka

2013-12-01

Freeze-drying of peptide and protein-based pharmaceuticals is an increasingly important field of research. The diverse nature of these compounds, limited understanding of excipient functionality, and difficult-to-analyze quality attributes together with the increasing importance of the biosimilarity concept complicate the development phase of safe and cost-effective drug products. To streamline the development phase and to make high-throughput formulation screening possible, efficient solutions for analyzing critical quality attributes such as cake quality with minimal material consumption are needed. The aim of this study was to develop a fuzzy logic system based on image analysis (IA) for analyzing cake quality. Freeze-dried samples with different visual quality attributes were prepared in well plates. Imaging solutions together with image analytical routines were developed for extracting critical visual features such as the degree of cake collapse, glassiness, and color uniformity. On the basis of the IA outputs, a fuzzy logic system for analysis of these freeze-dried cakes was constructed. After this development phase, the system was tested with a new screening well plate. The developed fuzzy logic-based system was found to give comparable quality scores with visual evaluation, making high-throughput classification of cake quality possible. © 2013 Wiley Periodicals, Inc. and the American Pharmacists Association.

Effect of molecular weight and ratio of poly ethylene glycols' derivatives in combination with trehalose on stability of freeze-dried IgG.

PubMed

Mohammad Zadeh, Amir Hossein; Rouholamini Najafabadi, Abdolhosein; Vatanara, Alireza; Faghihi, Homa; Gilani, Kambiz

2017-12-01

The influence of poly ethylene glycol (PEG) at different molecular weights (MWs) and ratios was studied on the stability of freeze-dried immune globulin G (IgG). PEGs (600-4000 Dalton) at concentrations of 0.5 and 5% W/V were applied in the presence of 40 and 60% W/W of trehalose to prepare freeze-dried IgG formulations. Size-exclusion chromatography, infra-red spectroscopy, differential scanning calorimeter, and gel electrophoresis were performed to characterize lyophilized samples. Pure IgG demonstrated the highest aggregation of 5.77 ± 0.10% after process and 12.66 ± 0.50% as well as 44.69 ± 0.50% upon 1 and 2 months of storage at 45 °C, respectively. 5% W/V of PEGs 4000 in combination with 40% W/W trehalose, significantly suppressed aggregation, 0.05 ± 0.01%, with minimum aggregation rate constant of 0.32 (1/month). The integrity of IgG molecules and secondary conformation were properly preserved in all formulations comparing native IgG. It could be concluded that appropriate concentration and MW of PEGs, prominently augmented stabilizing effect of trehalose on freeze-dried antibody through inserting additional supportive mechanisms of actions.

Influence of osmotic dehydration pre-treatment and combined drying method on physico-chemical and sensory properties of pomegranate arils, cultivar Mollar de Elche.

PubMed

Cano-Lamadrid, Marina; Lech, Krzysztof; Michalska, Anna; Wasilewska, Malwina; Figiel, Adam; Wojdyło, Aneta; Carbonell-Barrachina, Ángel A

2017-10-01

"Mollar de Elche" is the most popular Spanish pomegranate cultivar (intense sweetness and easy-to-chew arils); however, arils have pale pink colour and flat sensory profile. "Mollar the Elche" arils first underwent an osmotic dehydration pre-treatment (OD) with concentrated juices: (i) chokeberry, (ii) apple, and/or (iii) pomegranate cultivar "Wonderful", to improve their antioxidant capacity, colour, and sensory profile complexity, and later the arils were dried by a combined method (convective pre-drying+vacuum microwave finish drying). The use of OD provided dried arils with characteristic sweetness, and improved colour and aromatic complexity. The recommended OD methods were those using (i) pomegranate, and (ii) pomegranate with chokeberry juices; they improved the total anthocyanin content (mean of 368mgkg -1 ), red colour (a ∗ coordinate 15.6), and antioxidant capacity (e.g. ABTS mean of 5.7mmolTrolox100g -1 ). However, further research is still needed because freeze-dried arils had the highest anthocyanin content. Copyright © 2017 Elsevier Ltd. All rights reserved.

Development of a Freeze-Dried, Heat-Stable Influenza Subunit Vaccine Formulation

PubMed Central

Flood, Alexander; Chen, Dexiang

2016-01-01

An influenza pandemic remains a major public health concern. A key strategy to prevent a pandemic is to stockpile and pre-position stable influenza vaccine to allow rapid deployment in response to an outbreak. However, most influenza vaccines today are formulated as liquids that are stable only within a temperature range of 2°C to 8°C and require use of a cold chain, making vaccine transportation, distribution, and storage complicated and expensive, particularly for developing countries. To support the National Strategy for Pandemic Influenza preparedness in the United States and internationally, we developed two lead dry formulations of stable H1N1 influenza subunit vaccines using freeze-drying technology. The stable formulations contain an excipient combination of a disaccharide, such as sucrose or trehalose, and glycine, in addition to a surfactant and phosphate buffer. The freeze-dried vaccines were shown to be safe and remained immunogenic in an in vivo study in mice. Moreover, the lead formulations demonstrated no significant loss of activity after 40 months at storage temperatures of 25°C and 37°C. This stability can be particularly attractive as it could eliminate the need to use a cold chain for vaccine deployment and facilitate integration of vaccine distribution with general drug distribution where appropriate. These freeze-dried thermostable influenza subunit vaccines could also reduce the frequency of vaccine stockpile turnover, offering a cost-effective option for pandemic preparedness. PMID:27851765

Development of a Freeze-Dried, Heat-Stable Influenza Subunit Vaccine Formulation.

PubMed

Flood, Alexander; Estrada, Marcus; McAdams, David; Ji, Yuhua; Chen, Dexiang

2016-01-01

An influenza pandemic remains a major public health concern. A key strategy to prevent a pandemic is to stockpile and pre-position stable influenza vaccine to allow rapid deployment in response to an outbreak. However, most influenza vaccines today are formulated as liquids that are stable only within a temperature range of 2°C to 8°C and require use of a cold chain, making vaccine transportation, distribution, and storage complicated and expensive, particularly for developing countries. To support the National Strategy for Pandemic Influenza preparedness in the United States and internationally, we developed two lead dry formulations of stable H1N1 influenza subunit vaccines using freeze-drying technology. The stable formulations contain an excipient combination of a disaccharide, such as sucrose or trehalose, and glycine, in addition to a surfactant and phosphate buffer. The freeze-dried vaccines were shown to be safe and remained immunogenic in an in vivo study in mice. Moreover, the lead formulations demonstrated no significant loss of activity after 40 months at storage temperatures of 25°C and 37°C. This stability can be particularly attractive as it could eliminate the need to use a cold chain for vaccine deployment and facilitate integration of vaccine distribution with general drug distribution where appropriate. These freeze-dried thermostable influenza subunit vaccines could also reduce the frequency of vaccine stockpile turnover, offering a cost-effective option for pandemic preparedness.

Preparative free-flow electrophoresis as a method of fractionation of natural organic materials

USGS Publications Warehouse

Leenheer, J.A.; Malcolm, R.L.

1973-01-01

Preparative free-flow electrophoresis was found to be an efficient method of conducting large-scale fractionations of the natural organic polyelectrolytes occurring in many surface waters and soils. The method of free-flow electrophoresis obviates, the problem of adsorption upon a supporting medium and permits the use of high potential gradients and currents because of an efficient cooling system. Separations were monitored by determining organic carbon concentration with a dissolved carbon analyzer, and color was measured by absorbance at 400 nanometers. Organic materials from waters and soils were purified by filtration, hydrogen exchange, and dialysis and were concentrated by freeze drying or freeze concentration. In electrophoretic fractionations of natural organic materials typically found in surface waters and soils, color was found to increase with the charge of the fraction.

A new method for reporting and interpreting textural composition of spawning gravel.

Treesearch

Fredrick B. Lotspeich; Fred H. Everest

1981-01-01

A new method has been developed for collecting, sorting, and interpreting gravel quality. Samples are collected with a tri-tube freeze-core device and dry-sorted by using sieves based on the Wentworth scale. An index to the quality of gravel is obtained by dividing geometric mean particle size by the sorting coefficient (a measure of the distribution of grain sizes) of...

Curcuminoid content of Curcuma longa L. and Curcuma xanthorrhiza rhizome based on drying method with NMR and HPLC-UVD

NASA Astrophysics Data System (ADS)

Hadi, S.; Artanti, A. N.; Rinanto, Y.; Wahyuni, D. S. C.

2018-04-01

Curcuminoid, consisting of curcumin, demethoxycurcumin and bis demethoxycurcumin, is the major compound in Curcuma longa L. and Curcuma xanthorrhiza rhizome. It has been known to have a potent antioxidants, anticancer, antibacteria activity. Those rhizomes needs to be dried beforehand which influenced the active compounds concentration. The present work was conducted to assess the curcuminoid content of C. longa L. and C. xanthorrhiza based on drying method with Nuclear Magnetic Resonance (NMR) and High Pressure Liquid Chromatography (HPLC)-UVD. Samples were collected and dried using freeze-drying and oven method. The latter is the common method applied in most drying method at herbal medicine preparation procedure. All samples were extracted using 96% ethanol and analyzed using NMR and HPLC-UVD. Curcuminoid as a bioactive compound in the sample exhibited no significant difference and weak significant difference in C. xanthorrhiza and C. longa L., respectively. HLPC-UVD as a reliable analytical method for the quantification is subsequently used to confirm of the data obtained by NMR. It resulted that curcuminoid content showed no significant difference in both samples. This replied that curcuminoids content in both samples were stable into heating process. These results are useful information for simplicia standardization method in pharmaceutical products regarding to preparation procedure.

Mesenchymal Tissue Response to Heterotopically Placed Demineralized Bone Powder Particles in the Rat

DTIC Science & Technology

1987-01-01

Press, Cambridge, England, pp. 329-356. Hurt, W. 1968. Freeze-dried bone homografts in periodontal lesions in dogs. J. Periodontology , JI89. Hynes, R...1974. Biodegradable ceramic in periodontal defects. Oral Surg., 11t344. Lindhe, J. 1983. Textbook of Clinical Periodontology . Philadelphia, Munskgaard... Periodontology , 58:129. Turner, D.W. and Mellonig, J. 1981. Antigenicity of freeze- dried bone allografts in periodontal osseous defects. J. Periodont. Res

[A case of orchitis following vaccination with freeze-dried live attenuated mumps vaccine].

PubMed

Suzuki, Masayasu; Takizawa, Akitoshi; Furuta, Akira; Yanada, Shuichi; Iwamuro, Shinya; Tashiro, Kazuya

2002-05-01

In Japan, freeze-dried live attenuated mumps vaccine has been used optionally since 1981. The effectiveness of mumps vaccination has been established by worldwide research since 1971. On the other hand, because of it's live activity several untoward effects have been reported. Vaccination-related mumps orchitis is a rare adverse effect of mumps vaccine. Only 9 cases of vaccination-related mumps orchitis have been reported in Japan. We describe a case of orchitis following mumps vaccination in adolescence. A 16 years-old male has admitted because of acute orchitis with high fever and painful swelling of right testis. The patient had received vaccination with freeze-dried live attenuated mumps vaccine 16 days before admission. After admission, the bed-rest had completely relieved the symptoms on 6th hospital day. The impaired testis has maintained normal size and consistency 6 months after discharge.

Release profile and stability evaluation of optimized chitosan/alginate nanoparticles as EGFR antisense vector

PubMed Central

Azizi, Ebrahim; Namazi, Alireza; Haririan, Ismaeil; Fouladdel, Shamileh; Khoshayand, Mohammad R; Shotorbani, Parisa Y; Nomani, Alireza; Gazori, Taraneh

2010-01-01

Chitosan/alginate nanoparticles which had been optimized in our previous study using two different N/P ratios were chosen and their ability to release epidermal growth factor receptor (EGFR) antisense was investigated. In addition, the stability of these nanoparticles in aqueous medium and after freeze-drying was investigated. In the case of both N/P ratios (5, 25), nanoparticles started releasing EGFR antisense as soon as they were exposed to the medium and the release lasted for approximately 50 hours. Nanoparticle size, shape, zeta potential, and release profile did not show any significant change after the freeze-drying process (followed by reswelling). The nanoparticles were reswellable again after freeze-drying in phosphate buffer with a pH of 7.4 over a period of six hours. Agarose gel electrophoresis of the nanoparticles with the two different N/P ratios showed that these nanoparticles could protect EGFR antisense molecules for six hours. PMID:20957167

Effects of ultrasonic pretreatments on quality, energy consumption and sterilization of barley grass in freeze drying.

PubMed

Cao, Xiaohuang; Zhang, Min; Mujumdar, Arun S; Zhong, Qifeng; Wang, Zhushang

2018-01-01

Barley grass is a plant resource for rehabilitation therapy. Its processing requires retaining nutrition well for rehabilitation cure of consumers. To meet the aim as well as low energy consumption and microbiological safety of products, ultrasonic treatments (UT) were applied to bathing materials at different power levels (10, 30, 45, 60W/L) for 10mins. After treatments, the bathed barley grass (100g) was freeze-dried under vacuum -0.09MPa with fixed power of 2W/g. Parameters of color, microbial colony, energy consumption, glass transition temperature, moisture content, water activity, taste substances, contents of flavonoid and chlorophyll were determined after drying. In contrast with no treatment case, UT (45W/L) decreased drying time by 14% and decreased energy consumption by 19%; UT (60W/L) decreased total microbial colonies by 33%. Also, UT (30W/L) yielded contents of flavonoid (9.2/kg) and chlorophyll (10.5g/kg) of dried sample; UT power (10W/L) yielded the highest L ∗ (51.5) and the lowest a ∗ (-9.3) value. Simultaneously, UT leads to a higher glass transition temperature (Tg), lower water activity and produces less sourness and bitterness of dried products. Ultra-sonication is an alternative to improve quality, flavor and energy consumption of barley grass in freeze drying. Copyright © 2017 Elsevier B.V. All rights reserved.

Preservation of Differentiation and Clonogenic Potential of Human Hematopoietic Stem and Progenitor Cells during Lyophilization and Ambient Storage

PubMed Central

Buchanan, Sandhya S.; Pyatt, David W.; Carpenter, John F.

2010-01-01

Progenitor cell therapies show great promise, but their potential for clinical applications requires improved storage and transportation. Desiccated cells stored at ambient temperature would provide economic and practical advantages over approaches employing cell freezing and subzero temperature storage. The objectives of this study were to assess a method for loading the stabilizing sugar, trehalose, into hematopoietic stem and progenitor cells (HPC) and to evaluate the effects of subsequent freeze-drying and storage at ambient temperature on differentiation and clonogenic potential. HPC were isolated from human umbilical cord blood and loaded with trehalose using an endogenous cell surface receptor, termed P2Z. Solution containing trehalose-loaded HPC was placed into vials, which were transferred to a tray freeze-dryer and removed during each step of the freeze-drying process to assess differentiation and clonogenic potential. Control groups for these experiments were freshly isolated HPC. Control cells formed 1450±230 CFU-GM, 430±140 BFU-E, and 50±40 CFU-GEMM per 50 µL. Compared to the values for the control cells, there was no statistical difference observed for cells removed at the end of the freezing step or at the end of primary drying. There was a gradual decrease in the number of CFU-GM and BFU-E for cells removed at different temperatures during secondary drying; however, there were no significant differences in the number of CFU-GEMM. To determine storage stability of lyophilized HPC, cells were stored for 4 weeks at 25°C in the dark. Cells reconstituted immediately after lyophilization produced 580±90 CFU-GM (∼40%, relative to unprocessed controls p<0.0001), 170±70 BFU-E (∼40%, p<0.0001), and 41±22 CFU-GEMM (∼82%, p = 0.4171), and cells reconstituted after 28 days at room temperature produced 513±170 CFU-GM (∼35%, relative to unprocessed controls, p<0.0001), 112±68 BFU-E (∼26%, p<0.0001), and 36±17 CFU-GEMM (∼82%, p = 0.2164) These studies are the first to document high level retention of CFU-GEMM following lyophilization and storage for 4 weeks at 25°C. This type of flexible storage stability would potentially permit the ability to ship and store HPC without the need for refrigeration. PMID:20824143