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Recent Developments in Freeze Drying of Foods
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DOI: 10.1016/B978-0-12-815781-7.00017-2
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From Waghmare, R.B., Perumal, A.B., Moses, J.A., Anandharamakrishnan, C., 2021. Recent
Developments in Freeze Drying of Foods. In: Knoerzer, K., Muthukumarappan, K. (Eds.),
Innovative Food Processing Technologies: A Comprehensive Review, vol. 3. Elsevier, pp.
82–99. https://doi.org/B978-0-12-815781-7.00017-2.
ISBN: 9780128157817
Copyright © 2021 Elsevier Inc. All rights reserved.
Elsevier
3.05 Recent Developments in Freeze Drying of Foods

Roji Balaji Waghmare, Anand Babu Perumal, JA Moses, and C Anandharamakrishnan, Computational Modeling and Nanoscale
Processing Unit, Indian Institute of Food Processing Technology (IIFPT), Ministry of Food Processing Industries, Government of
India, Thanjavur, Tamil Nadu, India
© 2021 Elsevier Inc. All rights reserved.
3.05.1 Introduction 82
3.05.2 Fundamental Principles of Freeze Drying 82
3.05.3 Changes in the Product During Lyophilization 83
3.05.4 Types of Freeze Drying Process 84
3.05.4.1 Vacuum Freeze Drying 84
3.05.4.2 Atmospheric Freeze Drying 85
3.05.4.3 Spray Freeze Drying 85
3.05.5 Combined Freeze Drying With Other Methods/Modification in Freeze Drying 86
3.05.5.1 Infrared-Assisted Freeze Drying 86
3.05.5.2 Microwave-Assisted Freeze Drying 89
3.05.5.3 Ultrasonic-Assisted Freeze Drying 89
3.05.5.4 Pulsed Electric Field-Assisted Freeze Drying 90
3.05.5.5 Osmotic Dehydration is a Low-Cost Pretreatment for Freeze Drying 91
3.05.6 Applications of Freeze drying 91
3.05.6.1 Fruit and Vegetable Products/Fresh Produce 91
3.05.6.2 Meat and Poultry 93
3.05.6.3 Seafood 93
3.05.6.4 Coffee 96
3.05.6.5 Other Applications 96
3.05.7 Conclusion and Future Perspectives 96
References 97
3.05.1 Introduction
Drying is perhaps the oldest method of preservation in the food industry (Maisnam et al., 2015). It hinders microbial deterioration
and enzyme activity, and consequently extends the shelf life of food products (de Bruijn et al., 2016). Dried products are more suit-
able for handling since their reduced volume helps to lower the packaging, transport, and storage costs (Prosapio and Norton,
2018). Rehydration capacity is the key parameter that measures the quality of a dried product. However, convective hot air-
dried products show moderate or low rehydration capacity, due to cellular and structural breakage taking place during the drying
process (Vega-Gálvez et al., 2015). Also, degradation of nutrients occurs during conventional drying, which results in quality loss of
food products. Hence, it is very important to design and study new drying equipment and drying techniques (Norton et al., 2014).
Among the various drying techniques, freeze drying or lyophilization has become one of the most important processes for the
preservation of food products. Freeze drying is based on sublimation of the solvent in a product. The solvent can be either water or
an organic solvent, which is crystallized at low temperatures and thereafter transforms directly from the solid state into the vapor
phase. Freeze drying is done at lower temperatures, consequently preserving the quality characteristics of food and also limiting the
damage suffered by thermolabile compounds (Martínez-Navarrete et al., 2019). Hence, the main objective of freeze drying is to
deliver a substance with extended shelf life where the quality of food is unaltered after reconstitution with water.
Freeze drying offers numerous advantages compared to conventional drying technology. The main advantages of freeze drying are
maintenance of morphological, biochemical, and original characteristics, high recovery of volatiles, and maintenance of the structure
and surface (Isleroglu et al., 2018; Ciurzy
nska and Lenart, 2011). Since freeze drying is performed at low temperatures, these products
present a lower risk for being labile to heat degradation. Therefore, freeze drying can be applicable for valuable materials that are heat
sensitive or samples sensitive to heat that cannot be treated using other processes involving high temperatures (Morais et al., 2016).
The purpose of this chapter is to review the recent developments in freeze drying. Recent applications of freeze drying in the food
processing area are also discussed.
3.05.2 Fundamental Principles of Freeze Drying
Freeze drying is a method of preservation with a core principle of removal of solvent from a liquid formulation. The freeze-drying
process, as shown in Fig. 1, usually falls into three phases: freezing, the primary drying phase, and the secondary drying phase.
82 Innovative Food Processing Technologies, Volume 3 https://doi.org/10.1016/B978-0-12-815781-7.00017-2
Innovative Food Processing Technologies, 2021, 82–99

Recent Developments in Freeze Drying of Foods 83
Figure 1 Freeze drying process, showing freezing, primary drying, and secondary drying. Reproduced with permission from Morais et al. (2016).
Copyright © 2016, Elsevier.
Within these three phases, the freeze-drying process includes five essential activities which are freezing, sublimation, desorption,
vacuum pumping, and vapor condensation (Liu et al., 2008). First, the liquid formulations are cooled to a low temperature and
the water present in the material is completely frozen. Then, at reduced pressure, the frozen solvent is heated and removed from
the solid state directly into the vapor phase, i.e., sublimation drying process (primary drying). This is followed by a desorption
process (secondary drying) for the removal of the unfrozen solvent. Hence, freezing and drying are the two equally significant major
processes that take place during a freeze-drying process (Tang and Pikal, 2004).
Freezing is the critical step in a freeze-drying process because this phase dominates ice crystal morphology and size distribution,
which thus impact various important parameters, such as drying rates, the extent of product crystallinity, specific surface area, and
reconstitutability of the dried product (Searles, 2001). During the freezing step, samples are placed into a special mold or a freeze-
dryer tank. The freezing process is comprised of three stages. The first stage is the cooling phase, in which the temperature of samples
is reduced by liquid nitrogen, mechanical refrigeration, or dry ice to the freezing point temperature and the temperature at which the
first ice nucleus appears is known as the ice nucleation temperature (Kasper et al., 2013).
The second phase is known as the phase-change stage, in which the first ice nucleus appears and ice crystal growth takes place.
Primary nucleation is an incredibly quick process that is characterized by the appearance of the first ice nuclease. The formation of
primary nucleation is extremely difficult to detect either by eye or on a cooling thermogram except for the beginning stage of the
secondary nucleation. Secondary nucleation quickly follows primary nucleation, and is characterized by the expansion of ice nucle-
ation sites. In the third phase of the solidification stage, the majority of the water is transferred into solid by forming a network of ice
crystals. In this phase, ice crystals grow to such a degree that no further development is feasible (Assegehegn et al., 2019).
3.05.3 Changes in the Product During Lyophilization
To develop the optimized lyophilization processes, a better understanding of stabilizing mechanisms during each step of the lyoph-
ilization process as well as in the solid state is essential. It is well recognized that freezing and drying are accompanied by different
stresses that influence protein stability during lyophilization. In recent times, the contribution of individual stress factors has been
examined in more detail. For example, Bhatnagar et al. (2008) described that ice formation as the critical factor for lactate dehydro-
genase (LDH) stability during freezing by independently examining the influence of temperature, ice formation, and freeze concen-
tration using a temperature-stage approach. Furthermore, Tang and Pikal (2005) found that proteins may be lyophilized well above
the glass transition temperature (Tg) without the requirement for vitrification, as protein unfolding kinetics are strongly coupled
with system viscosity, and therefore, protein unfolding is very slow on the timescale of lyophilization, even at temperatures well
above Tg. Luthra et al. (2007) illustrated that secondary drying is the critical step for LDH stability by distinguishing primary
and secondary drying stresses using a mini freeze-dryer. The detailed study of the stresses during secondary drying recognized
that LDH was considerably affected by drying temperature and duration and both direct excipient interaction and vitrification
are needed for complete protein stabilization (Luthra et al. 2007).
Based on widespread opinion, collapse, defined as loss of the product structure affected by viscous flow of the freeze-concentrate
during drying (Wang et al., 2004), is considered detrimental because of the loss of structure, increased residual moisture levels,
extended reconstitution times, and the adverse influence on protein stability (Tang and Pikal, 2004; Jiang and Nail, 1998).
Thus, better pharmaceutical freeze-drying practice requires maintaining the product temperature below Tg or a little higher collapse
temperature (Tc) of the product during primary drying (Fig. 2), although drying at higher temperatures could greatly speed up the
cost-intensive drying process and therefore reduce the overall process time and energy consumption (Tang and Pikal, 2004).

84 Recent Developments in Freeze Drying of Foods
Figure 2 Overview of the recent advances on increasing the product temperature without negatively affecting the product stability. Reproduced with
the permission from Kasper et al. (2013). Copyright © 2013, Elsevier.
Earlier, the protein stabilization in a sugar–glass matrix has been ascribed to a thermodynamic pattern according to which sugar
molecules stabilized the native protein conformation via ‘‘water replacement,’’ or to a kinetic mechanism, that is based on the fact
that degradation mechanisms in the vitrified, rigid sugar matrix will be restricted. The latter mechanisms, the ‘‘vitrification hypoth-
esis,’’ combined the stability of proteins or chemical mixtures to the universal mobility of the sugar glass matrix, which is then
referred to as structural relaxation or a-relaxation (Yoshioka and Aso, 2007). There is experimental evidence for both hypotheses,
however neither is capable of fully explaining and predicting stabilization in the glassy solid state (Wang et al., 2009; Pikal et al.,
2008).
Currently, the perception that the physical aging of an amorphous sample by thermal treatment, also known as annealing or
‘‘densification,’’ could enhance the permanence of an API was addressed in lyophilization development (Abdul-Fattah et al.,
2007). At this point, ‘‘annealing’’ is denoted as heating of an amorphous sample below its Tg for a particular period. While in
the annealing process, the glass will enter the ‘‘equilibrium glassy state’’ asymptotically causing a variation in the physical properties
of glass-like enthalpy, entropy, and volume (Hodge, 1995). Thus, structural relaxation times are augmented, universal mobility is
reduced, and therefore, to this point, the structural relaxation and reactivity are combined; reaction rates may be minimized upon
physical aging (Abdul-Fattah et al., 2007).
3.05.4 Types of Freeze Drying Process
Three different types of freeze-drying process are commonly employed for drying of food products: (1) vacuum freeze drying; (2)
atmospheric freeze drying; and (3) spray freeze drying.
3.05.4.1 Vacuum Freeze Drying

Vacuum freeze drying is a technique that has been widely used for producing dried food products in the food industry since the
1960s. In recent years, this technique has been extensively used for drying fruits, vegetables, coffee, milk, meat, and other
high-value food products. It is used throughout the world and is considered as the best processing technique for producing
high-quality dehydrated food products with minimal changes in texture, flavor, rehydration ability, and nutritional and chemical
compositions with other dried foods (Ma et al., 2018). Vacuum freeze drying consists of freezing components as well as a vacuum-
drying component and hence it gives the combined benefits of vacuum drying and freeze drying. Hence, in this way, it can preserve
the internal structure of particles and improve the rate of sublimation of water (Shi et al., 2012).
In the vacuum freeze-drying technique, the suspension is frozen under low temperature and the frozen water or solvent is
removed subsequently through sublimation. In vacuum freeze drying, simultaneous heat and mass transfer occur. Different
methods have been developed to increase the heat and mass transfer rates during the drying phase (Patil et al., 2010). Annealing
is the most effective method to increase ice crystal size, drying rate, and heat and mass transfer rate during the freeze-drying process
(Shi et al., 2012). In the annealing process frozen solvent is maintained above the final freezing temperature for a certain time (Lim
et al., 2018, Patil et al., 2010). Shi et al. (2012) found that the annealing process and the different cryoprotectants promote the
growth of ice crystals both inside and around the starch nanoparticles. It also influenced the residual moisture content, particle
size, and glass transition temperature of the starch nanoparticles.

Guo et al. (2019) investigated the effect of microbial transglutaminase (MTGase) on properties of gels prepared from vacuum
freeze-dried silver carp surimi. Vacuum freeze drying converts hydrated protein into solid protein without changing its gelling ability
(Danial, Seid, and Maryam, 2016). However, Guo et al. (2019) observed that the vacuum freeze drying partially denaturated the
surimi proteins, which decreases the gel texture. Heating at a temperature of 40 C and MTGase addition improves the gel texture of
the dried surimi. Hence, pretreatment in combination with vacuum freeze drying helps to produce surimi powder with an improved
gel texture. Vacuum freeze drying dehydrates grass carp (Ctenopharyngodon idella) fillets to achieve high-quality dried products with
good nutritional quality, texture, flavor, color, minimal shrinkage, and high porosity. Different approaches have been used to
predict the dehydrating mass loss percentage and rehydrating mass gain percentage (Ma et al., 2017).
3.05.4.2 Atmospheric Freeze Drying

Atmospheric freeze drying (AFD) combines freeze drying and convective drying. Freeze drying adds cost to energy usage as a high
vacuum is applied to the frozen samples to allow sublimation of the frozen solvent. However, frozen samples can be dried naturally
without providing a high vacuum. Therefore, the fundamental concept for creating atmospheric freeze drying is to reduce the energy
consumption compared with vacuum freeze drying while at the same time keeping high product quality. This process is feasible
when the partial pressure of water vapor in the drying chamber is lower than the water vapor pressure of the frozen sample. To
obtain this condition, cold and dry gas should be circulated through the frozen sample (Ishwarya et al., 2014). AFD products
show similar attributes of rehydration kinetics and hygroscopicity as vacuum freeze drying. However, in the case of apples, higher
levels of deterioration of antioxidant properties have been observed in comparison with vacuum freeze drying (Rahman and
Mujumdar, 2012; Taylor et al., 2010). Colucci et al. (2018) studied the effect of different drying process variables on the antioxidant
properties of eggplant (Solanum melongena L.) samples. It was found that the increase in drying temperature decreases ascorbic acid,
total phenolic content, and the antioxidant capacity of AFD eggplant samples. On the other hand, ultrasonic-assisted atmospheric
freeze drying helps to reduce the drying time and causes no significant change in the antioxidant content of the eggplant sample. A
schematic diagram of atmospheric spray freeze drying and its products is depicted in Fig. 3.
3.05.4.3 Spray Freeze Drying

Spray freeze drying (SFD) is a promising drying technique that yields powdered products with the combined attributes of spray
drying and freeze drying techniques (Anandharamakrishnan, 2019) (Fig. 4). SFD can be defined as a three-step process: (1) atom-
ization, the solution or suspension is atomized and the large volume of solution is broken down into small droplets which creates
a high surface to mass ratio; (2) solidification of the droplets (freezing), the atomized liquid foods are frozen in meeting with a cryo-
genic medium (usually liquid nitrogen); and (3) freeze drying, sublimation of the frozen particles at low temperature and pressure
(Vishali et al., 2019; Parthasarathi and Anandharamakrishnan, 2016).
The SFD process can be efficiently used for thermally sensitive compounds as this process is carried out at a lower temperature. In
recent years, SFD has had many applications in the microencapsulation of heat-sensitive probiotic microorganisms and compounds
Figure 3 Atmospheric spray freeze-drying equipment and its products. Reproduced with the permission from Borges Sebastião et al. (2017).
Copyright © 2017, Elsevier.

Figure 4 Schematic diagram of spray freeze drying. Reproduced with the permission from Wang et al. (2006). Copyright © 2006, Elsevier.
such as Lactobacillus plantarum, Lactobacillus paracasei, vitamin E, bovine serum albumin, docosahexaenoic acid, and fish oil (Rajam
and Anandharamakrishnan, 2015; Parthasarathi and Anandharamakrishnan, 2016; Isleroglu and Turker, 2019). Semyonov et al.
(2010) found that spray freeze drying was an effective method to encapsulate Lactobacillus paracasei using the maltodextrin–treha-
lose mixture as a matrix with final viabilities higher than 60%. Researchers also highlighted that the atomizer plays a very important
role in obtaining high-quality products as atomization directly affects the droplet size distribution of the spray. In the latest inno-
vation, ultrasonic-assisted spray-freeze drying (USFD) has been used to obtain controlled particle size and a shorter drying time
(Ishwarya et al. 2015; Isleroglu and Turker, 2019). USFD was used to prepare large, porous particles of mannitol, lysozyme, and
BSA protein and it was observed that the ultrasonic nozzles control the particle size and aerodynamic properties of SFD particles
(D’Addio et al., 2012).
For the process of atomization, two-fluid, three-fluid, four-fluid, and ultrasonic nozzles have been used. Among the different
kinds of nozzles used, the ultrasonic nozzle was reported to have good control over the particle size and four-fluid nozzles were
found to be appropriate for drugs with reduced aqueous solubility. Recently, four-fluid nozzles have been utilized for atomization
in SFD, as shown in Fig. 5 (Anandharamakrishnan, 2019). Two independent fluid feed streams are atomized by two separate
compressed air streams. With the streams coming in contact, the shock wave produces a mist of fine droplets at the collision focal
spot. These tiny droplets associate with liquid nitrogen and provide a more homogeneous temperature field for heat transfer which
promotes homogeneous nucleation and hence forms fine ice crystals.
The importance of SFD can be appreciated by the comparative studies done by Ishwarya and Anandharamakrishnan (2014).
They compared the physical parameters and aroma quality of coffee produced using SFD with those from FD and SD methods.
SFD helps to retain the characteristic low-boiling aromatic compounds of coffee, whereas these compounds were lost during the
initial stages of the FD and SD processes. Fig. 6 shows SEM images of SFD, SD, and FD coffee samples. These images clearly
show the difference in the product microstructure with the difference in drying methods. A spherical shape with a porous and rough
surface was observed in SFD coffee particles. However, spherical shape with a smooth surface and flaky structure were depicted in SD
and FD coffee samples.
3.05.5 Combined Freeze Drying With Other Methods/Modification in Freeze Drying
Although freeze drying is a well-accepted drying method, it is still expensive as it has high energy consumption because of its long
drying time which limits its applications on a wide range of products in the food industry (Wu et al., 2019a,b). To overcome the
shortcomings of freeze drying, new techniques are required to combine or modify the freeze-drying process to make it time- and
cost-effective.
3.05.5.1 Infrared-Assisted Freeze Drying

Infrared (IR) radiation represents thermal energy in the form of electromagnetic waves and surrounds that segment of the electro-
magnetic range that borders on visible light and microwaves. IR provides greater thermal efficiency and a rapid heating rate in

Figure 5 Four-fluid nozzle scheme. Reproduced with the permission from Anandharamakrishnan (2019). Copyright © 2019, Elsevier
Figure 6 Scanning electron micrographs of soluble coffee particles, (A) spray-freeze-dried, (B) spray-dried, and (C), freeze-dried. Reproduced with
the permission from Anandharamakrishnan (2019). Copyright © 2019, Elsevier.
comparison to conventional heating. Infrared-assisted freeze drying (IRAFD) effectively reduces the drying time and modifies the
properties of dried products. The freeze-drying time is the time required during the freeze-drying process, whereas the overall drying
time is the time needed for the IRAFD process. IR drying provides a higher drying rate and maintains better color in the final product
than other drying techniques and can be used as a predehydration technique before freeze drying (Krishnamurthy et al. 2008; Ciur-
zynska and Lenart, 2011).
IRAFD has found many applications for drying various food products such as strawberries (Shih et al., 2008), sweet potato (Lin
et al., 2005), Cordyceps militaris (Wu et al., 2019a,b), shiitake mushroom (Wang et al., 2015), banana snacks (Khampakool et al.,
2019), etc. Chakaborty et al. (2011) examined infrared-assisted freeze drying for the production of Aloe vera powders. The infrared-
assisted freeze drying of aloe vera showed a minimum moisture content of 3.49%, maximum wettability of 52.84 s, and maximum
yield percent of 3.87 through response surface methodology optimum conditions (Chakraborty et al., 2011).
Banana snack dehydration has been studied by combining a freeze-drying process with infrared radiation (Khampakool et al.,
2019). The study was performed using various IRAFD trials. As compared to freeze drying alone, continuous IRAFD markedly
reduced the drying time by up to 213 min, which saves more than 70% of the required time. In brief, the application of IR in freeze
drying of banana snacks indicates the potential of this technique to produce high-quality banana snacks with a significant reduction

Figure 7 Infrared-assisted freeze drying (IRAFD) system: (A) schematic diagram and (B) photo image. Reproduced with the permission from
Khampakool et al. (2019).
in time and energy during drying. Fig. 7 shows a schematic illustration and photo image of the IRAFD system. This consisted of the
following five major parts: vacuum pump, acrylic chamber, condenser and cold trap at 100 C, and near-infrared lamp. An electric
vitality meter was utilized for estimating the energy consumption of the condenser and pump. Voltage and current connected to the
IR light were estimated and recorded using the current sensor.
Wu et al. (2019a,b) developed an apparatus by replacing the electric heating plate with infrared lamps for freeze drying of
Cordyceps militaris. IRAFD and FD were compared at different drying temperatures of 40, 50, 60, and 70 C and it was observed
that the increase in drying temperature reduced the drying time and energy consumption significantly for both drying treatments.
IRAFD saves the total energy consumption compared to FD as it requires less drying time and the IR lamp uses minimal electrical
energy. Subsequently, these authors concluded that IRFD is a promising technique for acquiring high-quality dried products.

3.05.5.2 Microwave-Assisted Freeze Drying

Microwave (MW) drying is a technique based on electromagnetic waves that generate heat directly inside the product (Lenaerts
et al., 2018). MW radiation is a part of the electromagnetic spectrum ranging from 300 MHz to 300 GHz. As MW produces heat
inside the food product, it causes rapid internal heating. When microwave heating is coupled with freeze drying (MFD), the micro-
wave energy easily penetrates the ice and hence decreases the drying time by around 50%–75% in comparison to conventional FD
(Fan et al., 2012). Recent studies conducted on various food products such as button mushroom (Duan et al. 2016), restructured
mixed potato with apple chips (Huang et al., 2011), sea cucumber (Duan et al., 2010), and okra snacks (Jiang et al., 2017) showed
that MFD led to similar product quality compared to the FD process but at a reduced cost. Fan et al. (2012) evaluated the optimi-
zation of microwave freeze-drying conditions for the production of crude protein powders from Ginkgo biloba L. It is evident that
sample thickness has a direct relationship and microwave power has an indirect impact on the drying time. The drying time varied
curvilinearly and linearly with an increase in microwave power and sample thickness. These studies also proved that the drying time
of MFD is shorter than conventional FD. Therefore, MFD is a feasible alternative technique as it preserves the structure of the product
and also provides an economical drying process.
Despite its unique advantages, there are some difficulties in applications of the MFD technique at an industrial scale. The main
problem is associated with the fact that MFD technology causes nonuniform temperature distribution and corona discharge which
causes ice melting and overheating. Some scientists have attempted to solve these problems with the MFD technique. Wang et al.
(2013) designed microwave-assisted pulse fluidized bed freeze drying (MPFFD) to improve the drying uniformity of FD samples
and to obtain higher quality products (Fig. 8).
In recent years, the effect of MPFFD on the quality of dried Cordyceps militaris (Wu et al., 2019a,b) and stem lettuce slices (Wang
et al., 2013) has been studied. It was observed that the MPFFD samples dried more uniformly than the samples dried in a steady
spouted bed mode. The total drying time of Cordyceps militaris samples in MPFFD was reduced by 71.9% when compared to FD;
whereas for stem lettuce slices the drying time was reduced by more than 20% as compared with MFD. The color, crispness,
shrinkage, and antioxidant properties of C. militaris dried by MPFFD were quite similar to those of the FD samples. Hence, it
can be stated that MPFFD can be potentially used for providing high-quality products with high energy efficiency.
3.05.5.3 Ultrasonic-Assisted Freeze Drying

Ultrasonic waves refer to sound waves of frequency between 2 104 to 1 109 Hz. The ultrasonic mechanism is dependent on the
cavitation. Cavitation appears from ultrasonic conduct in a positive and negative alternating cycle. This cycle causes the formation
and contraction of a microbubble. The microbubble bursts when its frequency matches with the ultrasonic frequency and discharges
high energy and pressure. This disrupts the cell membrane and microstructure damage (Cao et al., 2018). Recently, various studies
have shown the potential advantages of ultrasound technologies in food processing. Ultrasonic spray-freeze drying (USFD) has
been used to produce partially purified microbial transglutaminase (mTGase) powder (Isleroglu et al., 2018); barley grass powder
(Cao et al., 2018), and liposomal dry powder (Ye et al., 2017). Colucci et al. (2018) also studied the influence of ultrasound-assisted
atmospheric freeze drying on the antioxidant properties of eggplant. The authors observed that ultrasound is effective in accelerating
the atmospheric freeze drying and improving the quality of eggplant. On the other hand, it was found that the increase in air velocity
and temperature during drying reduced the antioxidant potential of the dried samples.
The effect of USFD process parameters on enzymatic activity and particle size to produce partially purified microbial transglu-
taminase (mTGase) powder was investigated by Isleroglu et al. (2018). Ultrasonic atomization accelerates the freezing step of USFD.
It was found that the USFD process gives higher enzymatic activity, smaller particle size, and better morphology with reconstitution
when compared to freeze drying. USFD also better protects the samples at extreme pH levels and high temperatures as compared to
the freeze-drying process.
Figure 8 Schematic diagram of MPFFD. Reproduced with the permission from Wu et al. (2019a). Copyright © 2019, Elsevier.

Figure 9 Schematic diagram of ultrasonic-assisted spray freeze drying. Reproduced with the permission from Ye et al. (2017). Copyright © 2016,
Elsevier.
Fig. 9 shows the process and apparatus used for USFD as described by Ye et al. (2017). The USFD process consists of ultrasonic
atomization, rapid freezing, and lyophilization. In USFD, the ultrasonic spray nozzle atomizes liquid into fine droplets. The liquid
is atomized with high-frequency sound waves directly into liquid nitrogen, which rapidly freezes the atomized droplets. The ultra-
sonic nozzle sprays an aqueous formulation directly into liquid nitrogen, which rapidly freezes the atomized droplets. The frozen
particles are lyophilized, leaving behind a dry powder.
3.05.5.4 Pulsed Electric Field-Assisted Freeze Drying

Pulsed electric field (PEF) treatment depends on the application of short electrical pulses of high voltage to the product which is
placed between two electrodes. The polarization causes permeabilization of the cell membrane and accelerates heat and mass trans-
fer process. PEF is nonthermal microbial sterilization of microbial cells without causing undesirable changes in food tissues. Pulsed
electric field (PEF) causes permeabilization of cell membranes which results in nonthermal microbial sterilization of biological cells
(Toepfl and Knorr, 2008). Recently, the potential application of PEF treatment with freeze drying has been explored by some
authors on foods such as apple tissue (Parniakov et al., 2016), potato tissue (Wu and Zhang, 2014), and apples (Lammerskitten
et al., 2019).
Parniakov et al. (2016) studied the influence of PEF as a pretreatment at an electric field strength of E ¼ 800 V/cm on apple discs
in the processes of vacuum cooling and FD. Fig. 10 presents a schematic diagram of PEF-assisted freeze drying. Initially, the apple
samples were pretreated with PEF, and then they were subjected to vacuum cooling to decrease the temperature to subzero level for
freeze drying. PEF treatment influences the heat and mass processes during freezing and also accelerates the cooling and drying
process. The data from the capillary impregnation test show the presence of large pores, fast rate of moisture impregnation, and
greater rehydration capacity as compared to untreated samples. The PEF treatment shows the relative increase of the rehydration
capacity by 1.3.
Figure 10 Schematic diagram of PEF-assisted freeze drying with analysis. Reproduced with the permission from Parniakov et al. (2016). Copyright
© 2016, Elsevier.

3.05.5.5 Osmotic Dehydration is a Low-Cost Pretreatment for Freeze Drying

In osmotic dehydration (OD), equilibrium conditions are maintained on both sides of the membrane by evacuating water from
a lower solute concentration to a higher concentration. OD is a low-cost treatment that maintains the color, flavor, and nutritional
quality of food products by partially removing water. Osmotic dehydration and blanching pretreatments can be applied to freeze
drying to reduce its long processing time and energy demand (Prosapio and Norton, 2018). OD produces intermediate moisture
products which can be further dried using drying technique with reduced processing time (da Costa Ribeiro et al., 2016; Prosapio
and Norton, 2017).
Osmotic dehydration treatment with the FD process causes the incorporation of probiotics in banana slices with a microbial
content of 109 CFU/g and a stability of 20–28 days (Rascón et al., 2018). For osmotically dehydrated freeze-dried raspberries, higher
firmness and lower deformability in relation to air-dried samples were observed (Sette et al., 2016). Similarly, osmotic dehydration
pretreatment was applied to oven drying and freeze drying for strawberries (Prosapio and Norton, 2017). The application of OD
reduces the processing time and retains the food properties. Fig. 11 shows images of the cortex cells in fresh and rehydrated straw-
berries using a confocal scanning laser microscope. In Fig. 11A, cells of fresh strawberry are close to each other. Figs. 11B and C show
images of OD-treated samples and OD þ FD samples, respectively. In these figures, intact cells are visible, which indicates that the
process does not affect the microstructure of the samples. In contrast, in oven-dried samples (Fig. 11D), the microstructure of cells
was completely ruptured and the cells were difficult to identify. The cells of OD and oven-dried samples (Fig. 11E) were partially
broken. Therefore, the application of OD results in greater rehydration of samples. It can be stated that the OD pretreatment signif-
icantly reduces the processing time and retains the mechanical and structural properties of strawberries.
3.05.6 Applications of Freeze drying
Freeze drying is a promising technology that is used widely, especially for high-value food products. It has been widely used in the
production of fruits, vegetables, meat, fish, coffee, etc. Due to the high manufacturing costs, the use of freeze drying for commercial
food powder production remains limited mainly to instant coffee, high-end foodstuffs such as spices and herbs, extreme sports
foods, baby instant formulas, encapsulated food compounds, and microorganisms. Recently, the market for “natural” and “organic”
products has greatly increased, as well as consumers’ demands for healthy ingredients and foods with minimal processing and high
quality. The commercial production of freeze-dried powders from “organic” fruits and vegetables and nutraceutical products, that is,
isoflavones from soybean (Kao and Chen, 2007) or fucoxanthin-rich powder from algae (Mise et al., 2011), has already found its
place in the worldwide market and will significantly increase in the years to come. For the production of microorganisms in powder
form in the industry, freeze drying is the preferred drying technique since it causes the least cell viability loss when compared to
other drying methods (Morgan et al., 2006).
Ekdawi-Sever et al. (2003) showed that maintaining frozen samples at temperatures above Tg for a certain time increased ice
formation and decreased the final moisture content of freeze-dried samples, thus prolonging the storage time and stability of
freeze-dried powders. As freeze drying is widely recognized to be the best dehydration method in terms of powder final quality,
it is often used as a reference to test the performance of other drying methods. The application of nonconventional freeze-drying
technologies to produce food powders has mainly progressed in atmospheric, traditional, or spray-freeze drying. Claussen et al.
(2007) pointed out that the use of a heat pump system with environmentally friendly refrigerants, together with temperature
programs, may help in upgrading the final powder quality obtained by atmospheric freeze drying. Compared to the traditional
atmospheric freeze drying method, atmospheric spray-freeze drying presents improved heat and mass transfer, higher and homo-
geneous powder quality properties with increased retention of aroma, no “caking”, instant solubility, and wetting (Mumenthaler
and Leuenberger, 1991). By combining atmospheric spray-freeze drying with fluidization in countercurrent flow, Wang et al.
(2006) obtained loose and free-flowing carbohydrate powders in a reduced processing time. More recently, Rahman and Mujumdar
(2012) reported the potential for use of a vibrating bed atmospheric freeze dryer for cost-competitive drying of heat-sensitive mate-
rials like fruits and vegetables.
3.05.6.1 Fruit and Vegetable Products/Fresh Produce

Consumer interest in fresh produce is continuously increasing. However, maintaining the quality of fresh produce remains a critical
issue (Waghmare et al., 2013). The shelf life of fresh produce is limited due to its high water content and constrained availability
because of seasonality (Waghmare and Annapure, 2013; Martínez-Navarrete et al., 2019). Drying is one of the most common tech-
niques used to prolong the shelf life of fresh produce, in turn, allowing its consistent availability. Also, drying additionally involves
a decrease in the volume and weight of fresh produce, which promotes its transport and handling (Fazaeli et al., 2012). However,
bioactive compounds, thermolabile nutrients, such as vitamins or carotenoids, might be degraded during thermal processing and,
consequently, the fresh produce can lose its nutritional and health benefits. Therefore, freeze drying is a promising technique for
drying thermally sensitive products such as fresh produce (Djekic et al., 2018).
Freeze drying is a dehydration process that has a nominal effect on the quality of food products. Freeze drying is currently used in
several applications to process fresh produce. A recent study by Martínez-Navarrete et al. (2019) indicated that the added biopoly-
mers such as 5 g gum arabic and 1 g whey protein isolate per 100 g of mandarin juice with freeze drying increases its textural

Figure 11 Confocal microscope images of strawberry cells: (A) Nontreated sample. (B) FD sample. (C) Osmotic and FD sample. (D) Oven-dried
sample. (E) Osmotic and oven-dried sample. Reproduced with the permission from Prosapio and Norton (2017). Copyright © 2017, Elsevier.
properties. In addition, it reduces the processing time without affecting its sensory properties or vitamin content. Similarly,
Lammerskitten et al. (2019) investigated pulsed electric field and freeze drying for their effects on macro- and microscopic proper-
ties, color, total phenolic content, and the antioxidant activity by treating apples at various temperatures (set on 40 C and 60 C)
and pressures (0.1, 0.25 and 1 mbar). The electric field strength of 1.07 kV/cm and specific energy input of 0.5, 1, and 5 kJ/kg were
used in PEF. PEF pretreated samples showed an increase of total phenolic content by up to 47% compared to untreated samples.
However, antioxidant activity for PEF-treated apple was reduced by up to 60% in comparison to reference samples. These observa-
tions explain the need for optimizing such process combinations.

In studies on the stability of a microencapsulated strawberry flavor, three different drying techniques, spray drying, freeze drying,
and fluid bed, were compared (Pellicer et al., 2019). The mixtures were frozen at 80 C for 24 h with sequential lyophilization to
obtain a powder. The highest yield was obtained through the freeze-drying technique, whereas the spray-drying technique produced
the lowest moisture content powder. However, with respect to the stability of ethyl acetoacetate, benzyl alcohol, and fraistone, the
spray-drying technique showed the best results, followed by freeze drying and fluid bed. Some of the important recent findings in
this area are compiled in Table 1. Wang et al. (2007) studied the aroma encapsulation efficiency of banana powders produced by
belt drying, freeze drying, and vacuum drying, showing that freeze-dried banana powders had an optimum aroma, followed by
vacuum drying. The influence of hot-air and freeze-drying processes was evaluated to preserve and concentrate bioactive
compounds in sea buckthorn fruit powder (Araya-Farias et al., 2011). Surprisingly, sea buckthorn freeze-drying kinetics was
much faster than air drying, probably due to the composition of the fruit, which is rich both in oil and carbohydrates. The bioactive
compound retention was higher in freeze-dried samples than in hot-air dried ones, due to low temperatures and shorter exposure to
oxygen during the process.
3.05.6.2 Meat and Poultry

Meat and poultry products are extremely perishable due to the high amount of viable nutrients, water activity, and pH (Cantalejo
et al., 2016). The microbial contamination of meat can cause severe foodborne illness in consumers. Therefore, meat and poultry
safety is considered to be the essential factor for consumers (Van Wezemael et al., 2010). The use of freeze drying for meat and
poultry products has been studied extensively in recent years. Freeze drying preserves the natural color, flavor, taste, and nutritional
value of meat. This technique causes no damage to the protein in meat and retains the fat-soluble vitamins A and D (Ma et al.,
2018). Hence, freeze drying is a promising technique for the drying of food products that are extremely sensitive to heat and easily
oxidized.
Recently, several studies have been conducted on the effects of freeze drying on meat and meat products; however, few studies
have investigated the use of freeze drying on poultry. As is already known, vacuum freeze-dried meat has brighter color, higher nutri-
tional value, and is easy to digest (Kotwaliwale et al., 2007). Presently, some industries have started producing high-grade meat
products with rich nutrition using freeze-drying technology (Gao et al., 2017). Cantalejo et al. (2016) evaluated the combined
use of ozone and freeze drying on the total aerobic mesophilic bacteria (TAMB) and lactic acid bacteria (LAB) counts of broiler
chicken meat fillets. Reductions of 6.8 and 4.77 log CFU/g for TAMB and LAB counts were observed by combining ozone
(0.6 ppm for 10 min) and freeze-drying treatments as compared to nontreated samples, whereas 3.26 and 1.41 log reductions
were reported when compared with nonozonated freeze-dried meat. The authors indicated that the combined treatment would
be useful for enhancing the microbial properties and extending the shelf life of raw chicken breast meat up to 8 months at 21
1 C. In contrast, purely freeze-dried samples had a shelf life of 4 months only. Similarly, 0.4 ppm exposure of ozone to the sample
harmed its textural properties. Similarly, Zouaghi and Cantalejo (2016) indicated that three combined techniques (ozonation,
freeze drying, and modified atmosphere packaging) can be used successfully to deliver long-lasting and high-quality poultry meats.
The gas combination of 20% CO2/80% N2 presented the best preservation conditions for ozonated dried chicken breast fillets
stored at room temperature.
Salting is effective as a preservative method because it reduces the moisture content of meat and thus decreases microbial growth.
Yalçin and Şeker (2016) studied the influence of salt content, pressing, and moisture content on textural and microbiological
parameters of turkey breast meat. No Micrococcus/Staphylococcus count was observed in samples that were salted, pressed, and
partially freeze-dried throughout the storage period of 70 days. Total drying time was reduced to 7 hfrom 27 h in the freeze dryer
for a reduction of the moisture content of turkey breast meat to 40%.
Freeze drying has been used to improve the solubility, emulsion stability, water-holding capacity, and heat gel strength of egg
white protein. Some researchers analyzed drying treatment, solubility, gel property, and emulsification properties to evaluate the
freeze-drying processing of egg white protein. For example, Zhou et al. (2014) found that the drying time for egg white protein
was significantly reduced with the combined effect of freeze drying and microwave vacuum drying compared to freeze drying treat-
ment alone. Table 2 summarizes the key findings in the area of meat and poultry.
3.05.6.3 Seafood
Fish is an essential dietary component in various countries. Various studies are present on the drying and preservation of fish.
However, there are few reports on the freeze drying of fish. Freeze-drying technology has the potential to convert hydrated protein
into powder form without changing its gelling property because the low temperature during the drying process protects protein
from thermal denaturation (Dehnad et al., 2016).
The gelling property of surimi is affected by various factors such as the method of heating, surimi properties, and functional
additives (starch, hydrocolloids, enzymes, etc.) (Lanier et al., 2014). A study was recently conducted on the influence of heating
method and incorporation of microbial transglutaminase (MTGase) on properties of gels made from vacuum freeze-dried surimi
(Guo et al., 2019). The results showed that the gel texture of vacuum freeze-dried surimi partially declined during drying but the
improvement of gel texture was achieved by adding MTGase and using a setting temperature of 40 C. However, in the comparative
study of spray drying, freeze drying, and vacuum drying on various properties of gelatin from rohu swim bladder, the freeze-drying
treatment showed the highest gelatin yield followed by vacuum drying and spray drying (Kanwate et al., 2019). Table 3 presents

Table 1 Some current application researches of freeze drying for the preservation of fruits and vegetables.
Product Process Key highlights References
Apple Pulsed electric field-assisted vacuum freeze Preserved the shape of the samples without shrinking Parniakov et al. (2016)
drying Increased pore size by z 86 and rehydration capacity
by z 1.3
Cordyceps militaris Microwave-assisted pulse fluidized bed freeze MPFFD lowered the rehydration time and shrinkage of Wu et al. (2019a,b)
drying (MPFFD) dried samples
Preserved the color attributes, crispness, volatile
compounds, and antioxidant activities of dried
samples as compared to samples obtained using hot
air drying
Banana snacks IRAFD system þ FD Continuous IRAFD-2.7 kW/m2 saved electrical energy Khampakool et al. (2019)
consumption of up to 8.4 103 kJ
Decreased the drying time up to 213 min compared to
freeze drying
Button mushroom Freeze drying combined with microwave Increased total free amino acid content Pei et al. (2014)
vacuum drying (FMVD) Reduced soluble sugars content and polyols due to the
Maillard reaction.
Barley grass Ultrasonic pretreatments with freeze drying Improved quality, flavor, and energy consumption Cao et al. (2018)
Reduced drying time and energy consumption in
contrast with no treatment
Inactivated total microbial colony and bacterial colony
Yielded high contents of flavonoid and chlorophyll
Mandarin snack Biopolymers and freeze drying Gum Arabic and a whey protein isolate increased the Martínez-Navarrete et al.
color purity, crunchiness, and firmness of the snack (2019)
Decreased hygroscopicity
Stem lettuce cubes Blanching on microwave freeze drying (MFD) Higher electrical conductivity of samples blanched by Wang et al. (2012)
microwave compared to boiling water blanching
MFD duration of microwave-blanched samples
reduced by 30% compared to boiling water-blanched
ones
Potato tissue Pulsed electric field on freeze drying Reduced drying time by 31.47% Wu and Zhang (2014)
Increased drying rate by 14.31%
Kimchi powder Hot air drying and freeze drying FD samples scored a higher rating in sensory than hot Park et al. (2016)
air dryer samples
FD is more suitable for producing high-quality kimchi
powder than hot air drying
Okra snacks Microwave vacuum drying-assisted FD Reduced drying time and energy consumption by Jiang et al. (2017)
approximately 75.36% and 71.92%, respectively
Apple Microwave-assisted vacuum freeze drying MFD greatly reduced the drying time and can provide Duan et al. (2012)
high product quality
Button mushroom Microwave-assisted vacuum freeze drying MFD can lead to similar product quality compared with Duan et al. (2016)
FD, color deterioration of MFD mushroom is higher
than FD ones
Banana Microwave-assisted vacuum freeze drying The drying time was shortened with an increase of Jiang et al. (2010a)
both microwave power and the degree of maturity of
the banana. MFD can obtain better product quality
Results for MFD and FD samples are similar, major Jiang et al. (2010b)
changes found in the primary drying stage in starch
content, reducing sugar content, structure, and
color, the major change in expansion ratio occurs in
the secondary drying stage
The method that increases the heating power in the Jiang et al. (2013a)
secondary drying stage of MFD can potentially
reduce the energy consumption without sacrificing
the color of dried product
Compared with FD, MFD can accelerate the drying rate. Jiang et al. (2013b)
The temperature distribution is uniform during the
sublimation stage, but not at the start of the
desorption stage. The major dissimilarity between
the FD and MFD samples is observed in their pore
size and distribution

Table 1 Some current application researches of freeze drying for the preservation of fruits and vegetables.dcont'd
Banana slices Microwave freeze drying and pulse-spouted The color of FD was better than that of MFD and pulse- Jiang et al. (2014)
microwave vacuum drying spouted microwave vacuum drying
Foamed raspberry Microwave-assisted freeze drying Drying techniques resulted in 66%–81% retention of Ozcelik et al. (2019)
puree ascorbic acids and 53%–84% retention of total
anthocyanins
Shiitake Freeze drying assisted with mid-infrared The combination of MIRD with FD had a significant Wang et al. (2014)
mushroom radiation effect on aroma retention and caused an increase of
sulfur compounds such as dimethyl, trisulfide, and
1,2,4-trithiolane
Strawberry chips Ultrasound and ultrahigh pressure-assisted Resulted in a decrease in the drying duration and total Zhang et al. (2020)
vacuum freeze drying energy consumption of samples
Purple potato Vacuum freeze drying FD methods result in less specific energy Qiu et al. (2019)
slices consumption, effective functional properties, and
digestibility
Strawberries Ultrasound-assisted osmotic dehydration USOD and freeze drying results in improved quality Prosapio and Norton
(USOD) and freeze drying properties of dried foods: Rehydration capacity was (2018)
enhanced as compared to freeze-dried samples;
color was better retained, the texture was largely
improved, and the fruit shape was maintained as the
microstructure was well preserved
Egg plant Ultrasound-assisted atmospheric freeze The application of power ultrasound proved to be Colucci et al. (2018)
drying effective at shortening the drying time and, at the
ultrasonic power level tested, did not significantly
affect the eggplant antioxidant content
Garcinia fruit Freeze drying Freeze drying technique was used for Ezhilarasi et al. (2013)
microencapsulation of Garcinia fruit extract. The
encapsulated were incorporated into bread dough
and the implications on quality were evaluated
Table 2 Some current researches into freeze drying in the area of meat and poultry products.
Mealworms Comparison of microwave drying to freeze The application of a vacuum during microwave Lenaerts et al. (2018)
drying drying did not appear to show any advantages
Microwave drying can be an alternative to freeze
drying
Broiler chicken meat Ozone and freeze drying Retarded the growth of microorganisms Cantalejo et al. (2016)
Extended the shelf life by up to 8 months
Turkey meat Salted, pressed, and freeze-dried Reduced freeze drying time to 7 h from 27 h of Yalçin and Şeker
complete drying in the freeze dryer (2016)
Chicken meat Modified atmosphere packaging and 20%CO2/80%N2 gas combination was found to be Zouaghi and Cantalejo
ozonated freeze-dried the most effective treatment for maintaining the (2016)
textural and sensory properties of ozonated
dried chicken samples
Egg yolk Freeze drying The retention of total xanthophyll content over Wenzel et al. (2011)
6 months of shelf life depended on the
distribution of natural and synthetic pigments in
the egg yolk
Egg yolk-based extenders Freeze drying Antioxidant supplemented freeze-dried egg yolk- Alcay et al. (2016)
based extenders have a positive effect on goat
sperm parameters
Egg white protein (EWP) Freeze-drying and spray-drying processes Freeze drying was the most effective treatment for Liu et al. (2015)
the production of modified EWP powders
Duck egg white protein Freeze drying and microwave Significant reduction in drying time by FD þ MVD Zhou et al. (2014)
powders Vacuum drying (FD þ MVD) compared to those obtained by the FD
Better retention of color, lower apparent density,
and lower foaming stability but higher
emulsifying index

Table 3 Some current researches into freeze drying in the area of seafood.
Sea cucumber Microwave freeze drying (MFD) Improved the drying rate Duan et al. (2010)
Reduced drying time by about half of the
conventional FD process with similar
product quality
Microwave freeze drying can replace
conventional freeze drying
Sea fennel extracts Ultrasonication and freeze drying Sea fennel extracts suitable for producing Alemán et al. (2019)
liposomes with antioxidant properties
Gelatin from Labeo rohita swim Comparison between spray drying, freeze Highest gelatin yield obtained in freeze drying Kanwate et al. (2019)
bladder drying, and vacuum drying
Fish muscle Microwave-assisted freeze drying Decreased the concentration of Zhang et al. (2014)
organochlorine pesticides extracted from
fish muscle tissue
Hake muscle Freeze-dried soy phosphatidylcholine Phosphatidylcholine liposomes stabilized by Marín-Peñalver et al.
liposomes freeze drying (2018)
Chinese-style ham Vacuum freeze drying Less nutrient loss, lightweight, easy to carry Ma et al. (2018)
transportation, easy long-term
preservation, and on quality is far superior
to other dried food
recent research on the freeze drying of seafood. Apart from fish and fish products, freeze drying has been evaluated for other seafood
products. Indrawati et al. (2015) freeze-dried brown seaweed pigment. They reported that the dominant pigments were pheophytin
a and trans-fucoxanthin, which have potency as bioactive compounds. The pigment powder could be stored at 28 C under an inert
atmosphere for at least 63 days before significant pigment degradation.
3.05.6.4 Coffee
Coffee is one of the most popular beverages that is cherished by consumers around the world. Spray freeze drying is a unique drying
technique that can produce a free-flowing coffee powder with a porous microstructure. Spray freeze drying retains more aroma and
flavor compounds than conventional freeze drying (Anandharamakrishnan, 2019). Ishwarya et al. (2015) found that spray freeze
drying retains 93% volatiles in soluble coffee, whereas FD and SD hold 77% and 57% volatiles, respectively. Another study on
encapsulation of phenolic compounds extracted from spent coffee grounds indicated that freeze drying using maltodextrin as
a coating material retains 62% and 73% of phenolic compounds and flavonoids, respectively (Ballesteros et al., 2017).
3.05.6.5 Other Applications

Smaniotto et al. (2020) reported that the active release behavior from alginate fluid gels (AFG) was not affected by freeze drying
when AFG was formed of nanoparticles. However, the active release behavior was affected by freeze drying when AFG was formed
from microparticles, explaining the size-dependent impact on release behavior. Moayyedi et al. (2018) revealed that the freeze-
drying method showed the lowest loss in cell survival during storage Also, the results showed the superiority of freeze-dried micro-
capsules to prolong L. rhamnosus ATCC 7469 survival when exposed to digestive system conditions.
Vincenzetti et al. (2018) studied the effects of freeze-drying and spray-drying process on the b-lactoglobulin and lysozyme
content in donkey milk. In particular, the spray-drying process decreased significantly the lysozyme enzymatic activity (58% of
residual activity) and b-lactoglobulin content (6.43 mg/mL in fresh milk vs. 5.51 mg/mL in spray-dried milk) due to the high
temperature to which the donkey milk was subjected. Wang et al. (2017) studied the production of bovine lactoferrin (LFb)
powders using spray drying and freeze drying. The results showed that both spray-dried LFb (SDLFb) and freeze-dried LFb (FDLFb)
powders had negligible denaturation and conformation changes compared to the liquid LFb. Both SDLFb and FDLFb showed type
II sorption behavior with almost identical monolayer moisture content. Similarly, the study reported the effects of freeze-dried Japa-
nese quince fruit (FJQF; 0%–9%) added to cookies to improve their antioxidant attributes during storage, sensory, and volatile char-
acteristics and acceptability by consumers (Antoniewska et al., 2019).
3.05.7 Conclusion and Future Perspectives
Unlike several other drying approaches, freeze drying is valued for the superiority it offers in terms of product quality. This approach
best suits foods with heat-sensitive components, and when maintaining “close-to-fresh” appearance is the priority. Nevertheless,

though freeze drying is widely used in research and industry for a range of applications involving food, pharma, and other ingre-
dients, the concern on process costs and associated product costs remains. In recent years, several techniques have been established
by researchers for pretreatment of materials to be freeze-dried. Another emerging area is the development of hybrid freeze-drying
systems that provide benefits in terms of reduced drying time, reduced process costs, and improved product quality. The task is to
scale-up such techniques established at the lab level to the industry. The immediate requirement is to strike a balance between cost
and product quality. As novel drying techniques, hybrid versions of the conventional approach must focus on sustainability.
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Recent Developments in Freeze Drying of Foods

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Roji Waghmare Anand Babu Perumal

J.A. Moses Anandharamakrishnan Chinnaswamy

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3.05 Recent Developments in Freeze Drying of Foods

3.05.2 Fundamental Principles of Freeze Drying

82 Innovative Food Processing Technologies, Volume 3 https://doi.org/10.1016/B978-0-12-815781-7.00017-2

Innovative Food Processing Technologies, 2021, 82–99

3.05.3 Changes in the Product During Lyophilization

Innovative Food Processing Technologies, 2021, 82–99

3.05.4 Types of Freeze Drying Process

3.05.4.1 Vacuum Freeze Drying

Innovative Food Processing Technologies, 2021, 82–99

3.05.4.2 Atmospheric Freeze Drying

3.05.4.3 Spray Freeze Drying

Innovative Food Processing Technologies, 2021, 82–99

3.05.5 Combined Freeze Drying With Other Methods/Modification in Freeze Drying

3.05.5.1 Infrared-Assisted Freeze Drying

Innovative Food Processing Technologies, 2021, 82–99

Innovative Food Processing Technologies, 2021, 82–99

Innovative Food Processing Technologies, 2021, 82–99

3.05.5.2 Microwave-Assisted Freeze Drying

3.05.5.3 Ultrasonic-Assisted Freeze Drying

Innovative Food Processing Technologies, 2021, 82–99

3.05.5.4 Pulsed Electric Field-Assisted Freeze Drying

Innovative Food Processing Technologies, 2021, 82–99

3.05.5.5 Osmotic Dehydration is a Low-Cost Pretreatment for Freeze Drying

3.05.6 Applications of Freeze drying

3.05.6.1 Fruit and Vegetable Products/Fresh Produce

Innovative Food Processing Technologies, 2021, 82–99

Innovative Food Processing Technologies, 2021, 82–99

3.05.6.2 Meat and Poultry

Innovative Food Processing Technologies, 2021, 82–99

Product Process Key highlights References

Innovative Food Processing Technologies, 2021, 82–99

Product Process Key highlights References

Product Process Key highlights References

Innovative Food Processing Technologies, 2021, 82–99

Product Process Key highlights References

3.05.6.5 Other Applications

3.05.7 Conclusion and Future Perspectives

Innovative Food Processing Technologies, 2021, 82–99

Innovative Food Processing Technologies, 2021, 82–99

Innovative Food Processing Technologies, 2021, 82–99

Innovative Food Processing Technologies, 2021, 82–99

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