scholarly journals Controlling Ice Nucleation during Lyophilization: Process Optimization of Vacuum-Induced Surface Freezing

Processes ◽  
2020 ◽  
Vol 8 (10) ◽  
pp. 1263 ◽  
Author(s):  
Andrea Allmendinger ◽  
Yuen Li Butt ◽  
Raphael Mietzner ◽  
Felix Schmidt ◽  
Joerg Luemkemann ◽  
...  
Keyword(s):  
Process Optimization ◽  
Storage Stability ◽  
Drug Product ◽  
Ice Nucleation ◽  
Freezing Process ◽  
Present Communication ◽  
Drying Time ◽  
Freeze Dried ◽  
Model Protein ◽  
Surface Freezing

Biopharmaceuticals are often lyophilized to improve their storage stability. Controlling ice nucleation during the freezing step of the lyophilization process is desired to increase homogeneity of product properties across a drug product batch and shorten the primary drying time. The present communication summarizes the process optimization of the freezing process when using vacuum-induced surface freezing to control ice nucleation, in particular for amorphous samples. We characterized freeze-dried samples for solid state properties, and compared these to uncontrolled nucleated samples using bovine serum albumin (BSA) as a model protein. Freezing parameters were optimized to obtain complete nucleation, adequate cake resistance during the subsequent lyophilization cycle, and elegant cakes. We highlight the challenges associated with vacuum-induced surface freezing and propose optimized freezing parameters to control ice nucleation, enabling manufacturing of amorphous samples.

scholarly journals Influence of Freezing Parameters on the Formation of Internal Porous Structure and Its Impact on Freeze-Drying Kinetics

Processes ◽  
2021 ◽  
Vol 9 (8) ◽  
pp. 1273
Author(s):  
Patrick Levin ◽  
Vincent Meunier ◽  
Ulrich Kessler ◽  
Stefan Heinrich
Keyword(s):  
Internal Structure ◽  
Freeze Drying ◽  
Crystal Size ◽  
Single Layer ◽  
Drying Kinetics ◽  
Freezing Process ◽  
Drying Time ◽  
Air Blast ◽  
Temperature Cycles ◽  
Freeze Dried

The main objective of this study was firstly to investigate the influence of freezing process parameters on the formation of the internal structure of frozen coffee granules. It was investigated how these frozen internal structures affect the drying kinetics during freeze-drying. A design of experiment study was carried out using the response surface method to quantify the influence of the freezing step that occurs in a scraped surface heat exchanger (SSHE). Therefore, the coffee extract at a concentration of 30% w/w is entering the SSHE as a liquid and gets partially crystallized up to a weight-based ice content of 0.364. During this step, the influence of factors like cooling temperature, scraper rotation speed and temperature cycles on ice crystal structure was investigated. In a second freezing step, the influence of freezing rates during hardening of the product by air-blast freezing is investigated, where the freezing rate is significantly affected by the cake thickness. The produced frozen granules were freeze-dried in single layer experiments. During drying the influence of internal structure on the drying kinetics was investigated. Results show that all factors have a significant impact on structure parameters for 30% w/w coffee solutions. A lower degree of supercooling during freezing in an SSHE, a higher number of temperature cycles (2 to 8 times) and lower freezing rates during hardening (2 °C/min to 10 °C/min) were leading to increased crystal size. This increase accelerates the primary drying rate and decreases the total drying time. A higher number of temperature cycles leads to a significant increase of crystal size and therefore larger pore size at the end of the primary drying. Furthermore, in combination with temperature cycles in the SSHE, it was found that high freezing rates during air blast freezing generally lead to a second nucleation step of ice crystals.

scholarly journals The Quality of Red Bell Pepper Subjected to Freeze-Drying Preceded by Traditional and Novel Pretreatment

Foods ◽  
2021 ◽  
Vol 10 (2) ◽  
pp. 226
Author(s):  
Katarzyna Rybak ◽  
Artur Wiktor ◽  
Dorota Witrowa-Rajchert ◽  
Oleksii Parniakov ◽  
Małgorzata Nowacka
Keyword(s):  
Freeze Drying ◽  
Bell Pepper ◽  
Total Phenolic ◽  
Thermal Methods ◽  
Drying Time ◽  
Freeze Dried ◽  
Dehydration Processes ◽  
Vacuum Freezing ◽  
Better Than

It has been demonstrated previously in the literature that utilization of PEF or a combination of a pulsed electric field (PEF) and ultrasounds (US) can facilitate dehydration processes and improve the quality of dried products even better than the application of thermal methods such as blanching. The aim of the study was to evaluate the quality of red bell pepper subjected to freeze-drying preceded by blanching or PEF or US treatment applied in a single and combined mode. Furthermore, the freeze-drying was preceded by shock freezing or vacuum freezing performed inside the freeze-dryer as a result of pressure drop during the first stage of freeze-drying. All of the analyzed technological variants enhanced the drying kinetics when compared to the intact material. Freeze-dried bell pepper subjected to non-thermal pretreatment exhibited higher vitamin C, total phenolic and carotenoids content than blanched material despite the fact that blanching reduced drying time the most compared to all other analyzed methods.

Storage stability of freeze–dried Lactobacillus acidophilus (La-5) in relation to water activity and presence of oxygen and ascorbate

Cryobiology ◽  
2009 ◽  
Vol 58 (2) ◽  
pp. 175-180 ◽  
Author(s):  
Lone Kurtmann ◽  
Charlotte U. Carlsen ◽  
Jens Risbo ◽  
Leif H. Skibsted
Keyword(s):  
Water Activity ◽  
Lactobacillus Acidophilus ◽  
Storage Stability ◽  
Freeze Dried

scholarly journals Effect of Hot-Water Blanching Pretreatment on Drying Characteristics and Product Qualities for the Novel Integrated Freeze-Drying of Apple Slices

2018 ◽  
Vol 2018 ◽  
pp. 1-12 ◽  
Author(s):  
Hai-ou Wang ◽  
Qing-quan Fu ◽  
Shou-jiang Chen ◽  
Zhi-chao Hu ◽  
Huan-xiong Xie
Keyword(s):  
Electron Microscopy ◽  
Freeze Drying ◽  
Hot Water ◽  
The Novel ◽  
Rehydration Ratio ◽  
Drying Time ◽  
Drying Characteristics ◽  
Promising Alternative ◽  
Freeze Dried ◽  
Apple Slices

The effect of hot-water blanching (HWB) on drying characteristics and product qualities of dried apple slices with the novel integrated freeze-drying (NIFD) process was investigated by comparing with 3 different FD methods. Compared with the NIFD process without HWB pretreatment (VF-FD), the NIFD process with HWB pretreatment (HWB-VF-FD) resulted in a significantly higher mass loss and more sufficient freezing in vacuum-frozen samples, significantly higher rehydration ratio (RR), higher shrinkage ratio (SR), smaller Vitamin C (VC) content and lower hardness and better apparent shape in freeze-dried samples, and fewer change to the color of the dried or rehydrated samples (p<0.05). Compared with the conventional FD process with HWB pretreatment (HWB-PF-FD), HWB-VF-FD cost significantly less processing time and FD time and obtained significantly higher RR (p<0.05), almost the equivalent SR, VC content, and hardness, and similar appearance in dried samples. The microstructure of apple cell tissues was analyzed by transmission electron microscopy and scanning electron microscopy to interpret the above differences in drying characteristics and product qualities. The results suggested that the NIFD process of apple slices with HWB pretreatment was a promising alternative method to decrease drying time, achieve similar product quality, and simplify the process steps of the conventional FD technology.

Storage stability of freeze-dried, spray-dried and drum-dried skim milk powders evaluated by available lysine

LWT ◽  
2016 ◽  
Vol 73 ◽  
pp. 675-682 ◽  
Author(s):  
Kataneh Aalaei ◽  
Marilyn Rayner ◽  
Ingegerd Sjöholm
Keyword(s):  
Storage Stability ◽  
Skim Milk ◽  
Freeze Dried ◽  
Available Lysine ◽  
Spray Dried

Freeze dried probiotic carrot juice powder for better storage stability of probiotic

2021 ◽  
Author(s):  
Dwivedi Rishabh ◽  
Ajith Athira ◽  
Radhakrishnan Preetha ◽  
G. Nagamaniammai
Keyword(s):  
Storage Stability ◽  
Carrot Juice ◽  
Freeze Dried

scholarly journals Fortified and freeze-dried kiwi fruit (Actinidia deliciosa): quality and sensory assessment

2020 ◽  
Vol 23 ◽  
Author(s):  
Niladri Chakraborty ◽  
Rajat Chakraborty ◽  
Asit Kumar Saha
Keyword(s):  
Moisture Content ◽  
Freeze Drying ◽  
Raw Materials ◽  
Food Product ◽  
Rice Flour ◽  
Actinidia Deliciosa ◽  
Crude Fibre ◽  
Kiwi Fruit ◽  
Drying Time ◽  
Freeze Dried

Abstract Kiwi fruit (Actinidia deliciosa) (KF) is one of the best fruits available due to its large amount of nutrients. Despite its many health benefits, there are no previous reports on its preparation in other readily ingestible forms. The objective of the present study was to make a new food product from KF. The KF pulp was fortified and blended with several raw materials (such as rice flour and oat flour) using a stepwise short time addition and mixing methodology since this avoids unwanted biochemical and chemical reactions. The blended and reduced moisture KF paste was freeze-dried on a round silver coated steel plate (RSCSP), supplying the heat of sublimation using a newly designed cubic heater. The freeze-drying (FD) time was 4.5 h and the drying kinetics were studied using four established models. The effective moisture diffusivity (Deff) during FD (at 50 °C) was 1.532 x 10-6 m2/s and the activation energy (E) estimated for the FD was 28.35 kJ/mol. The freeze-dried sample was ground and placed under vacuum to reduce the weathering effects. The quality of the stored product was evaluated using the proximate analysis, physicochemical analysis and a sensory evaluation using a hedonic scale. The raw, fresh KF had a moisture content of 85.07% and the final freeze-dried product one of 3%. The carbohydrate, total sugar, protein, fat, total ash, crude fibre and vitamin C contents of the final product increased by 563%, 400%, 355%, 386%, 672%, 106%, and 117% respectively. Of the 66 panelists, the % consumer acceptances for the different attributes were: sweetness (68.18%), sourness (90.91%), saltiness (100%), bitterness (100%), flavour (95.45%), texture (77.27%) and overall acceptability (81.82%). Using conventional freeze-drying (CFD) for blended KF pulp without fortification, with the same RSCSP and the same cubic heater for sublimation, the drying time was found to be 7 h to reach the same final moisture content of 3%.

scholarly journals Analysis of isothermal and cooling rate dependent immersion freezing by a unifying stochastic ice nucleation model

2015 ◽  
Vol 15 (9) ◽  
pp. 13109-13166
Author(s):  
P. A. Alpert ◽  
D. A. Knopf
Keyword(s):  
Cooling Rate ◽  
Surface Area ◽  
Ice Nucleation ◽  
Rate Dependence ◽  
Nucleation Theory ◽  
Freezing Process ◽  
Nucleation Kinetics ◽  
Rate Dependent ◽  
Immersion Freezing ◽  
The Impact

Abstract. Immersion freezing is an important ice nucleation pathway involved in the formation of cirrus and mixed-phase clouds. Laboratory immersion freezing experiments are necessary to determine the range in temperature (T) and relative humidity (RH) at which ice nucleation occurs and to quantify the associated nucleation kinetics. Typically, isothermal (applying a constant temperature) and cooling rate dependent immersion freezing experiments are conducted. In these experiments it is usually assumed that the droplets containing ice nuclei (IN) all have the same IN surface area (ISA), however the validity of this assumption or the impact it may have on analysis and interpretation of the experimental data is rarely questioned. A stochastic immersion freezing model based on first principles of statistics is presented, which accounts for variable ISA per droplet and uses physically observable parameters including the total number of droplets (Ntot) and the heterogeneous ice nucleation rate coefficient, Jhet(T). This model is applied to address if (i) a time and ISA dependent stochastic immersion freezing process can explain laboratory immersion freezing data for different experimental methods and (ii) the assumption that all droplets contain identical ISA is a valid conjecture with subsequent consequences for analysis and interpretation of immersion freezing. The simple stochastic model can reproduce the observed time and surface area dependence in immersion freezing experiments for a variety of methods such as: droplets on a cold-stage exposed to air or surrounded by an oil matrix, wind and acoustically levitated droplets, droplets in a continuous flow diffusion chamber (CFDC), the Leipzig aerosol cloud interaction simulator (LACIS), and the aerosol interaction and dynamics in the atmosphere (AIDA) cloud chamber. Observed time dependent isothermal frozen fractions exhibiting non-exponential behavior with time can be readily explained by this model considering varying ISA. An apparent cooling rate dependence ofJhet is explained by assuming identical ISA in each droplet. When accounting for ISA variability, the cooling rate dependence of ice nucleation kinetics vanishes as expected from classical nucleation theory. The model simulations allow for a quantitative experimental uncertainty analysis for parameters Ntot, T, RH, and the ISA variability. In an idealized cloud parcel model applying variability in ISAs for each droplet, the model predicts enhanced immersion freezing temperatures and greater ice crystal production compared to a case when ISAs are uniform in each droplet. The implications of our results for experimental analysis and interpretation of the immersion freezing process are discussed.

Osmotic dehydration assisted impregnation of Lactobacillus rhamnosus in banana and effect of water activity on the storage stability of probiotic in the freeze-dried product

LWT ◽  
2018 ◽  
Vol 92 ◽  
pp. 490-496 ◽  
Author(s):  
M.P. Rascón ◽  
K. Huerta-Vera ◽  
L.A. Pascual-Pineda ◽  
A. Contreras-Oliva ◽  
E. Flores-Andrade ◽  
...  
Keyword(s):  
Water Activity ◽  
Storage Stability ◽  
Osmotic Dehydration ◽  
Lactobacillus Rhamnosus ◽  
Effect Of Water ◽  
Freeze Dried
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