Redistribution of Protein Biological Activity in a Freeze-Dried Cake

Lactate dehydrogenase (LDH) solutions were freeze dried in order to investigate the redistribution of the remaining LDH activity in the dried cake. D-Mannitol and a polysaccharide (κ-carrageenan, ι-carrageenan, or dextran) were mixed and used as stabilizers in freeze drying. It was found that the remaining LDH activity was significantly redistributed in the freeze-dried cake, and the enzyme concentration was not uniform along the axis of the dried cake due to variations in the freeze-drying conditions and stabilizer concentration. In some cases, active enzymes were highly localized in a specific portion of the dried cake. This was mainly due to the redistribution of the protein content. Further freeze-drying tests employing bovine serum albumin (BSA) and the above-mentioned polysaccharides showed that proteins (BSA) tended to accumulate in the lower portions of the dried cake, forming concentration gradients. Therefore, the concentration gradient in the freeze-dried cake was mainly due to the freezing process. This redistribution of protein content contributed considerably to the apparent redistribution of enzyme activity. The results suggest that a process that can control the redistribution of protein content in a freeze-dried cake would further improve the biological activity of freeze-dried proteins.     

Properties and Stability of Spray-Dried and Freeze-Dried Microcapsules Co-Encapsulated with Fish Oil,Phytosterol Esters,and Limonene

The objectives of this study were to investigate the properties and stability of microcapsules containing fish oil co-encapsulated with phytosterol ester and limonene, prepared by spray-drying and freeze-drying methods. Whey protein isolate and soluble corn fiber were used as wall materials in the encapsulation process. The properties of microcapsules, including structure, glass transition, volatile/non-volatiles retention, microencapsulation efficiency, oxidation stability, color measurement, and sensory profiles, were evaluated after drying and during a seven-day accelerated storage trial. The finding reveals that drying methods have an effect on the retention of volatile fraction and the physical structure of the wall matrix consisted of WPI and SCF, consequently influencing the storage stability of the powders. Significantly higher retention of volatile fraction (p < 0.05) and lower surface oil were found in the spray-dried samples, resulting in the higher microencapsulation efficiency. However, samples dehydrated by both methods have good redispersion properties, showing no statistical significance (p > 0.05). The oxidation of the encapsulated oils was comparable for both spray- and freeze-dried samples during the seven-day accelerated storage trial but the loss of limonene flavor was significantly higher in the freeze-dried samples (p < 0.05). Sensory evaluation indicated that the addition of limonene could mask the unpleasant fishy odor in the co-encapsulated microcapsules. Overall, freeze drying did not produce powders with superior properties and did not show better protection towards the core materials than spray drying.     

Effect of Ultrasonically Induced Nucleation on the Drying Kinetics and Physical Properties of Freeze-Dried Strawberry

Power ultrasound has proved to be very useful in controlling crystallization processes since sonication can enhance both the nucleation rate and crystal growth rate by producing fresh and/or more nucleation sites. Therefore, in this study, power ultrasound was applied to control the freezing step of freeze-dried strawberry. The results showed that when power ultrasound was applied at different temperatures, it increased the nucleation temperature and shortened the characteristic freezing time. The application of power ultrasound in the freezing step increased the drying time in subsequently freeze-dried strawberry samples. This longer drying time was found to be due to increased resistance to moisture diffusion due to the formation of a network of small pores caused by sublimation of small ice crystals induced by the power ultrasound. Scanning electron microscopic images revealed that the freeze-dried sample frozen by ultrasound-assisted freezing (UAFD) had finer cellular structure compared to those frozen in other freezing conditions. UAFD samples had better textural hardness, while the rehydration capacity was lower compared to those of NRFD and NIFD samples.     

Effect of Processing Conditions on Drying Kinetics and Particle Microstructure of Carrot

The drying of carrot particles (6 mm × 6 mm × 12 mm) was studied in a tunnel dryer; a vacuum-freeze dryer, either with or without infrared radiation; a pulsed fluidized-bed dryer assisted by microwave radiation; and combinations of these methods. The effect of two freezing rates (quick freezing in liquid nitrogen and slow freezing in a household freezer) was also studied.

The drying kinetics for these drying methods were determined and modeled, and the dried products were subjected to texture (hardness), color, and rehydration analysis, as well as 2D and 3D image analysis of pictures from scanning electron microscope.

The combination of freeze drying with other dehydration techniques reduces the drying time by 6–70%, although, in general, the structural damage increases with respect to freeze drying alone. The hybrid drying systems did not show significant differences in drying times either for quick- or slow-frozen samples. The combination of freeze drying followed by conventional drying reduces the drying time between 23 and 40% on average.

The Page empirical model represents adequately the entire drying process for combined methods, with specific parameters for each drying zone. The values of effective diffusivity calculated with the simplified constant diffusivity model agree with those reported in the literature.     

Influence of Chemical Composition and Structure on Sorption Properties of Freeze-Dried Pumpkin

The aim of this study was to investigate the influence of chemical composition and material structure on sorption properties of freeze-dried pumpkin. The chemical composition and material structure were changed by osmotic dehydration, blanching, freezing, and temperature of the freeze-drying process. Freeze-dried pumpkin obtained from nonpretreated pumpkin had the best sorption properties, whereas osmotic dehydration significantly decreased the water vapor adsorption ability of the investigated samples. Studies on the influence of different freezing methods on water vapor sorption showed that a combination method of freezing resulted in the best sorption properties. When the temperature of freeze drying was increased, the water vapor adsorption ability of the freeze-dried pumpkin also increased.     

Effect of Drying Methods on Odorous Compounds and Antioxidative Activity of Gelatin Hydrolysate Produced by Protease from B. amyloliquefaciens H11

Gelatin hydrolysates with antioxidative activity produced by protease from Bacillus amyloliquefaciens H11 with different hydrolysis times were prepared. Alpha-amino group content and antioxidative activities increased with increasing hydrolysis time (p < 0.05). When gelatin hydrolysate prepared with hydrolysis time of 3 h (GH-3H) was subjected to freeze drying and spray drying, the powder obtained from spray drying showed a decrease in antioxidant activity as measured by DPPH and ABTS radical scavenging activities, ferric-reducing antioxidant power, and metal chelating activity. Spray-dried gelatin hydrolysate (GH-3H-SD) showed higher whiteness with lower fishy odor and off-odor associated with fermentation. This was concomitant with the decreases in several odorous compounds in the sample, except for nonanal, which was higher in comparison with the powder obtained by freeze drying. Thus, spray drying could be an effective drying method to improve color and reduce undesirable odor of gelatin hydrolysate.     

羟基磷灰石明胶复合材料的研究进展

主要是介绍羟基磷灰石明胶复合材料的研究进展。分析了羟基磷灰石明胶物理复合方法和化学复合方法。及该系统在其他方面的应用．最后对羟基磷灰石明胶复合材料的发展进行了展望。     

Experimental Investigation of the Recovery of Soaked Paper Using Evaporative Freeze Drying

The aim of this article is to develop an experiment and a procedure to investigate the restoration of water-damaged paper and archival materials using freeze drying in order to allow a reproducible test and comparison of the influence of different operating conditions on drying time and restored paper quality. Firstly, a reproducible method for the preparation of soaked samples simulating water-damaged paper has been developed. Then, the samples have been freeze-dried in a laboratory-scale apparatus that allowed monitoring the temperature as well as the weight of the samples. The technique of evaporative freezing, which reduces the drying time required, has been used in this case. An innovative procedure for the visualization of the progress of the drying process has been validated, thus allowing the validation of a simple phenomenological model of the time evolution of the ice core volume; in addition, data on the residual moisture of the dried paper sheets in different zones have been given. Finally, optimization of this particular drying process by using simple or more sophisticated approaches has been discussed.     

Optimal Control of the Primary Drying Stage of Freeze Drying of Solutions in Vials Using Variational Calculus

Abstract

The problem of operating freeze drying of pharmaceutical products in vials placed in trays of a freeze dryer to remove free water (in frozen state) at a minimum time was formulated as an optimal control problem. Two different types of freeze dryer designs were considered. In type I freeze dryer design, upper and lower plate temperatures were controlled together, while in type II freeze dryer design, upper and lower plate temperatures were controlled independently. The heat input to the material being dried and the drying chamber pressure were considered as control variables. Constraints were placed on the system state variables by the melting and scorch temperatures during primary drying stage. Necessary conditions of optimality for the primary drying stage of freeze drying process in vials are derived and presented. Furthermore, an approach for constructing the optimal control policies that would minimize the drying time for the primary drying stage was given. In order to analyze optimal control policy for the primary drying stage of the freeze-drying process in vials, a rigorous multi-dimensional unsteady state mathematical model was used. The theoretical approach presented in this work was applied in the freeze drying of skim milk. Significant reductions in the drying times of primary drying stage of freeze drying process in vials were obtained, as compared to the drying times obtained from conventional operational policies.     

Optimal Control of the Primary Drying Stage of Freeze Drying of Solutions in Vials Using Variational Calculus

The problem of operating freeze drying of pharmaceutical products in vials placed in trays of a freeze dryer to remove free water (in frozen state) at a minimum time was formulated as an optimal control problem. Two different types of freeze dryer designs were considered. In type I freeze dryer design, upper and lower plate temperatures were controlled together, while in type II freeze dryer design, upper and lower plate temperatures were controlled independently. The heat input to the material being dried and the drying chamber pressure were considered as control variables. Constraints were placed on the system state variables by the melting and scorch temperatures during primary drying stage. Necessary conditions of optimality for the primary drying stage of freeze drying process in vials are derived and presented. Furthermore, an approach for constructing the optimal control policies that would minimize the drying time for the primary drying stage was given. In order to analyze optimal control policy for the primary drying stage of the freeze-drying process in vials, a rigorous multi-dimensional unsteady state mathematical model was used. The theoretical approach presented in this work was applied in the freeze drying of skim milk. Significant reductions in the drying times of primary drying stage of freeze drying process in vials were obtained, as compared to the drying times obtained from conventional operational policies.     

How to Meet the Freeze Drying Standard in Combined Drying Processes: Pre and Finish Drying of Carrot Dice

Freeze-drying (FD) processes are well known to produce high-quality consumer products. Major problems are long drying times, high investment costs, and resulting maintenance and operating costs that make FD a very costly process. In this study, the potential of air drying (AD) and microwave vacuum drying (MVD) is tested to reduce freeze-drying times and make better utilization of the investment by combining FD with alternative lower cost drying processes using a pre or finish drying step while preserving the qualwity of the final product. Using carrot dice as a sample product, predrying did not lead to the desired qualities and reduction in drying time, whereas finish drying produced promising results. FD/MVD was 40% faster than pure FD and achieved freeze-drying standards regarding volume retention, shape, color, and rehydration. The good performance of microwave vacuum finish drying can directly be traced back to a time effect that is possibly linked to a characteristic collapse time of the cellular matrix. In order to use this effect, a stable skeleton must have developed at the point of process changeover, changeover has to be immediate, and finish drying has to be quick.     

Effect of Cryoprotectant and Freeze-Drying Process on the Stability of W/O/W Emulsions

In order to protect a hydrophilic drug and to prolong its further delivery, the formulation of multiple emulsions could be worthy. However, the double emulsions are not stable, their structure can change, leading to the formation of a single emulsion as the destruction of the system, and the drug can release easily from the globules in liquid state. The freeze-drying technology could be used to produce dry emulsion, the powder form being much more stable. The aim of this work was to study the influence of a cryoprotectant and a freeze-drying process on the stability of W/O/W emulsions. Samples were frozen at two different freezing rate (ν _f  = 0.55°C/min and 1.25°C/min) and successively dried at two different sublimation temperature (T _s  = ? 10°C and ? 20°C). The particle size distributions were measured by granulometer and UV spectrophotometer was performed to investigate the leakage of internal constituent. The glass transition temperature (T _g ) of the double emulsions was analyzed by DSC. The particle sizes became even smaller after freeze drying, except when κ-carrageenan is used as a cryoprotectant. In that case, the particles became aggregated after freeze drying, whatever the process conditions. The mean size is considerably reduced when the globules are diluted at low concentration in glucose and trehalose solution. When the concentration is increased, the size distribution is not significantly affected. The leakage of the internal aqueous phase to the external one during freeze drying was measured as an indicator of the structure stability. It is affected by the nature of the cryoprotectant and the conditions of the freeze-drying process. The leakage of the internal phase was smaller when cycle III (ν _f  = 1.25°C/min, T _s  = ? 10°C) was processed. From our experiments, we suppose that the water transfer from the inner phase to the outer aqueous phase results in the diminution of the globules size in double emulsion. The T _g of the double emulsions diluted with trehalose and glucose were determined at ? 33.8°C and ? 47.1°C. In contrast, the T _g of double emulsion with κ-carrageenan and HES did not appear.     

Effect of Cryoprotectant and Freeze-Drying Process on the Stability of W/O/W Emulsions

In order to protect a hydrophilic drug and to prolong its further delivery, the formulation of multiple emulsions could be worthy. However, the double emulsions are not stable, their structure can change, leading to the formation of a single emulsion as the destruction of the system, and the drug can release easily from the globules in liquid state. The freeze-drying technology could be used to produce dry emulsion, the powder form being much more stable. The aim of this work was to study the influence of a cryoprotectant and a freeze-drying process on the stability of W/O/W emulsions. Samples were frozen at two different freezing rate (ν_f = 0.55°C/min and 1.25°C/min) and successively dried at two different sublimation temperature (T_s = - 10°C and - 20°C). The particle size distributions were measured by granulometer and UV spectrophotometer was performed to investigate the leakage of internal constituent. The glass transition temperature (T_g) of the double emulsions was analyzed by DSC. The particle sizes became even smaller after freeze drying, except when κ-carrageenan is used as a cryoprotectant. In that case, the particles became aggregated after freeze drying, whatever the process conditions. The mean size is considerably reduced when the globules are diluted at low concentration in glucose and trehalose solution. When the concentration is increased, the size distribution is not significantly affected. The leakage of the internal aqueous phase to the external one during freeze drying was measured as an indicator of the structure stability. It is affected by the nature of the cryoprotectant and the conditions of the freeze-drying process. The leakage of the internal phase was smaller when cycle III (ν_f = 1.25°C/min, T_s = - 10°C) was processed. From our experiments, we suppose that the water transfer from the inner phase to the outer aqueous phase results in the diminution of the globules size in double emulsion. The T_g of the double emulsions diluted with trehalose and glucose were determined at - 33.8°C and - 47.1°C. In contrast, the T_g of double emulsion with κ-carrageenan and HES did not appear.     

Efficient Immobilization of Lecitase in Gelatin Hydrogel and Degumming of Rice Bran Oil Using a Spinning Basket Reactor

Immobilization of Lecitase (Phospholipase A1) in gelatin hydrogel and its stability is studied with a view to utilizing the immobilized enzyme for degumming rice bran oil. Excellent retention of enzyme activity (>80%) is observed in hydrogel containing 43.5% gelatin crosslinked with glutaraldehyde. Compared to the free enzyme which has a broad pH-activity profile (6.5–8.0), the activity of the immobilized enzyme is strongly dependent on pH and has a pH-optimum of pH 7.5. The optimum temperature of enzyme activity increases from 37 to 50 °C. Compared to the free enzyme which loses all its activity in 72 h at 50 °C, the immobilized enzyme retains its activity in full. The immobilized enzyme has been used efficiently in a spinning basket bioreactor for the degumming of rice bran oil with 6 recycles without loss of enzyme activity. The phosphorus content of the oil decreases from 400 ppm to 50–70 ppm in each cycle. After charcoal treatment and dewaxing, a second enzymatic treatment brings down the phosphorus content to <5 ppm.     

Optimal Control of the Secondary Drying Stage of Freeze Drying of Solutions in Vials Using Variational Calculus

Abstract:

The problem of operating freeze drying of pharmaceutical products in vials loaded on trays of freeze dryer to obtain a desired final bound water content in minimum time is formulated as an optimal control problem. Two different types of freeze dryer designs were considered. In the type I freeze dryer design, upper and lower plate temperatures were controlled together, while in the type II freeze dryer design, upper and lower plate temperatures were controlled independently. The heat input to the material being dried and the drying chamber pressure were considered as control variables. Only the scorch temperature was considered as a constraint on the system state variables during the secondary drying stage, because all the free water content (frozen water) is removed from the solid matrix during the primary drying stage of freeze drying. Necessary conditions of optimality for the secondary drying stage of freeze drying process in vials were derived and presented by using rigorous multidimensional unsteady-state mathematical models. The theoretical approach presented in this work was applied in the freeze drying of skim milk. Significant reductions in drying times of the secondary drying stage of the freeze drying process in vials were observed and more uniform bound water and temperature distributions in the material being dried were obtained compared to the conventional operational policies.     

Drying of Seabuckthorn (Hippophae rhamnoides L.) Berry: Impact of Dehydration Methods on Kinetics and Quality

Convective hot air drying and freeze drying were investigated as potential dehydration processes to obtain powders of seabuckthorn fruit pulp. Halved seabuckthorn fruits were placed in a hot air dryer and dried at 1 m/s and at 50 or 60°C or freeze dried at less than 30 mTorr and at 20 or 50°C shelf plate temperature. An initial characterization of the seabuckthorn pulp (moisture, pH, soluble solid content, vitamins C and E, total phenolics, and carotenoids) was performed. Water loss, total phenolic compounds, total carotenoids, and vitamin C were determined at different processing times. Vitamin E was determined before and at the end of drying.

Freeze-drying kinetics were faster than air drying, probably due to lower moisture diffusion in the compact, sugary, and oily structure of the air-dried tissue. The temperature had an important impact on hot air–drying and freeze-drying kinetics. Drying method and processing times affected the remaining phenolic, carotenoid, and vitamin contents of seabuckthorn berries. Freeze drying was revealed as a superior method to obtain seabuckthorn powders because of the lower residual moisture content, the ease of grinding, as well as the better nutritional retention.     

Studies on the Mechanical Properties of Gelatin and Its Blends with Vinyltrimethoxysilane: Effect of Gamma Radiation

Gelatin films were prepared by casting. Tensile strength (TS), elongation at break (Eb) and tensile modulus (TM) of the gelatin films were found to be 56 MPa, 6.1% and 1.14 GPa, respectively. Effect of gamma radiation (Co-60) on the mechanical properties of the gelatin films was studied. Vinyltrimethoxysilane (VTMS) was added to the gelatin during casting varying 1–7% by weight and found to increase the TS and TM significantly. Then the films were irradiated and found further increase of TS and TM. Water uptake of the gelatin films and 5% VTMS containing gelatin films were also evaluated.     

Drying of Foamed Biological Materials: Opportunities and Challenges

An overview is provided on hot air drying of foamed materials in a thin layer (foam-mat drying), foam-spray drying, microwave-assisted drying of liquid foams, as well as microwave drying of frozen foams with and without dielectric solid inserts, used as complementary heat sources. In particular, the mechanisms of heat and moisture transport during the drying of foams are identified. The effects of foam characteristics (e.g., foam density and stability) and drying conditions (temperature, air velocity) on drying kinetics and product quality are examined, and the differences between the drying of non-foamed and foamed materials are discussed.     

Drying of Foamed Biological Materials: Opportunities and Challenges

An overview is provided on hot air drying of foamed materials in a thin layer (foam-mat drying), foam-spray drying, microwave-assisted drying of liquid foams, as well as microwave drying of frozen foams with and without dielectric solid inserts, used as complementary heat sources. In particular, the mechanisms of heat and moisture transport during the drying of foams are identified. The effects of foam characteristics (e.g., foam density and stability) and drying conditions (temperature, air velocity) on drying kinetics and product quality are examined, and the differences between the drying of non-foamed and foamed materials are discussed.     

荷电杂化膜浓缩明胶水溶液的初步研究:pH值对明胶截留率的影响

本文探讨荷正电有机-无机杂化膜浓缩明胶水溶液,明胶水溶液pH值对明胶截留率的影响。实验结果表明,随着pH值上升,截留率下降;对同一pH值含有不同量强碱基团的荷正电有机-无机杂化膜,明胶截留率取决于明胶大分子与膜表面之间静电作用和憎水作用的综合效应。