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Food Engineering Reviews

https://doi.org/10.1007/s12393-018-9175-0

REVIEW ARTICLE

Material Properties and Tableting of Fruit Powders


M. G. Aziz 1 & Y. A. Yusof 2 & C. Blanchard 3 & M. Saifullah 2 & A. Farahnaky 3 & G. Scheiling 4

Received: 6 June 2017 / Accepted: 5 March 2018


# Springer Science+Business Media, LLC, part of Springer Nature 2018

Abstract
The tableting of fruit powders is gaining popularity due to conveniences in its use, storage, transportation, and product formu-
lation. Food powders are generally cohesive in nature, and their compressibility is highly correlated with the material properties
of the powder. Here, the material properties of fruit powders and their respective compressibilities in relation to powder type,
drying technique and their operating parameters, portion of the fruit used to produce the fruit powder, and drying aids are
discussed. Among the material properties analyzed, moisture content, water activity, particle density, particle size and shape,
and powder surface properties are identified as vital properties that highly influence the tableting behavior of fruit powders. The
Kawakita and Lüdde model and Heckel equation are widely studied to describe the compressibility and compactibility of fruit
powders. A four-parameter model fits the sigmoidal compression data of food powders well.

Keywords Fruit powder . Flowability . Cohesiveness . Tableting . Compaction modeling . Dissolution

Introduction dietary supplements and functional foods/nutraceuticals [29].


Fruits are often taken fresh, but they are also processed into
A wide variety of fruits are produced in large quantities around various value-added products. The current market of food in-
the world, and their exportation value plays an important role gredients is increasing due to scientific-based formulations in
in the economy of many countries [80, 88]. Fruit is considered food manufacturing and the demand for creating diversity in
an important and indispensable source of dietary fiber, vita- food products [37]. Fruits and their extracts in powder form
mins, and minerals. Many fruits have distinct flavors and have potential applications as food ingredients in the prepara-
colors and are used to bring variety into the daily diet. tion of different processed food products. Recent studies have
Recent research has explored fruit extracts as one of their chest shown the use of fruit powders as carriers of probiotic cells
sources of natural health, promoting functional ingredients [51], in the preparation of chewy candies [22]; as food tablets
and including food products marketed in the form of both ([4, 69, 79]; Yusofet al. 2012); and as the main raw material in
fast dispersible fruit tablets [53, 63, 72, 88].
The processing of food powders into a tablet form is eco-
* M. G. Aziz nomical with respect to the conveniences of storage, transpor-
aziz_ftri@bau.edu.bd tation, and use by the customer. Like other types of food pow-
ders, fruit powders are bulky in nature and require more space
1
Department of Food Technology and Rural Industries, Faculty of for storage and transportation. Compressing the powder up to
Agricultural Engineering & Technology, Bangladesh Agricultural certain level and/or into a tablet form reduces the volume and
University, Mymensingh, Bangladesh
surface area of the fruit powder, thus reducing the chances of
2
Department of Process and Food Engineering, Faculty of rehydration and quality degradation. Even though tableting is
Engineering, Universiti Putra Malaysia, 43400 Serdang, Selangor,
already an established process in the pharmaceutical and met-
Malaysia
3
allurgical industries, food tableting is rather new, and new tab-
School of Biomedical Sciences, Graham Centre for Agricultural
let foods are being developed rapidly by the food industries.
Innovation and ARC Industrial Transformation Training Centre for
Functional Grains, Charles Sturt University, Wagga Tablets can be made from powder, granules, pellets, or multi-
Wagga, NSW 2678, Australia ple film-coated units. However, it is obvious that the powders
4
Laboratory of Food Physics, Institute of Food Science, Department must have good compressibility to form tablets, and tableting
of Food Science and Technology, University of Natural Resources is extremely well correlated with the powder properties.
and Life Sciences, Vienna, Austria
Food Eng Rev

Each fruit powder has identical properties and compress- [27]. To overcome this technological problem, high-
ibility behaviors, although the powders made from same fruit molecular-weight bulk additives, such as polysaccharides,
may show different compressibilities and material properties proteins, and/or lipids, are added during the drying of sticky
due to processing. The information about powder compress- products to change the mechanical state and Tg of the pro-
ibility and properties is thus very important in the selection of duced powders [75]. The high-molecular-weight biopoly-
the fruit powder tablet processing parameters and processing mers, as anti-plasticizing additives, are mixed with the fruit
equipment design. Compression has a strong relationship with juices prior to the drying process. The addition of high-
dissolution and processing cost. This review discusses the molecular-weight biopolymers will result in increasing the
current state of understanding and recent progress in (i) fruit average glass transition of the system in a way that the dried
powder properties, as influenced by the type and portion of the food powders would have a Tg greater than the storage tem-
fruit used to produce powder, the drying technique and oper- perature, such that the food powders behave as a glass under
ating parameters, and carriers used; and (ii) the tableting be- storage conditions, with no collapse or agglomeration during
havior of different fruit powders. storage [14]. The material properties of the food powders in-
fluence their flowability and compressibility, which is
discussed in the coming sections.
Fruit Powder
Fruit Extract Powder
The fleshy part of the seeds and/or closely associated part of
plants that can be consumed in its raw state is termed fruit. The Fruits and vegetables are good sources of pectin, polyphenols,
consumption of fruits in their raw state is desirable to obtain organic colors, dietary fibers, enzymes, flavonoids, vitamins,
the greatest health benefit. However, due to the short shelf life and oligosaccharides. These compounds are extracted to pro-
after harvest, it is not possible to have fresh fruit year round. duce enriched functional foods or medical supplements that
Processing fruits into fruit powders thus helps to prolong their are marketed as functional ingredients. The techniques and
shelf life by reducing their moisture content and water activity. processing conditions used to produce fruit extract powders
Drying is a necessary and therefore vital operation in produc- depend on the nature of the active compounds present in the
ing fruit powder. Based on the portion of the fruit to be dried, extract. Spray drying and freeze drying are the common
the resultant powders could be either fruit juice powder, fruit methods for producing polyphenol, organic color, and flavo-
extract powder, or whole fruit powder. noid extract powders, with spray drying being a widely prac-
ticed technique. Irrespective of the above two methods used
Fruit Juice Powder for drying, the use of the carrier or coating materials is oblig-
atory to avoid problems during drying, such as adhering to the
Fruit juice powder (FJP) is normally prepared by drying fruit drier wall, the development of a wet and plastic appearance,
juice into powder. Juice is extracted from the fruit pulp, the and agglomeration and clumping in the packing container
coarse particles are removed, the permitted additives are Verma and Singh [77]. About 94 to 96% polyphenol and an-
added, and the juice is dried using suitable drying techniques. thocyanin retention was reported by Fang and Bhandari [24]
Spray drying and freeze drying are the widely practiced during the spray drying of bayberry extract with maltodextrin.
methods of producing fruit juice powders. However, FJPs A comprehensive review on the production of functional pow-
are categorized as sticky products, with stickiness and the ders from fruits and vegetables was made by Jiang et al. [37],
caking of powders being potential problems during storage which explored the effects of drying type and operating con-
[14]. When fruit juices are dried by spray drying, they may ditions, such as the drying temperature and coating materials,
result in sticky lumps or heavy drier wall deposits [3], whereas in the production of polyphenol, flavonoid, dietary fiber, ly-
vacuum drying may cause the powder to become hygroscopic copene, and pectin powders. Solar or mechanical drying can
and get caked and agglomerated during storage and household be used without affecting the nutritional quality of dietary
use. The presence of high concentrations of amorphous mate- fiber, as reported by Chantaro et al. [18] for carrot peel fiber
rials, like low-molecular-weight sugars and organic acids, is and Ajila et al. [6] for mango peel fiber.
associated with the low glass transition temperature Tg of fruit
powders, which is the fundamental indicator of stickiness [13, Whole Fruit Powder
14]. Since amorphous fruit powders have relatively low Tg
values [13], they will be in a rubbery state (with a high mo- Whole fruit powder (WFP) is the dried powder from the whole
lecular mobility) under storage conditions. Moreover, the high fruit after removing the inedible part (Fig. 1). Juice production
molecular mobility rates allow the fruit powders to relax and from fruits at the laboratory-scale yields only 60% of the total
deform, with the powder particles having enough flexibility to weight of fruit, with the remaining 40% discarded as by-prod-
develop strong surface-to-surface and molecular interactions ucts, such as the peels, seeds, and part of the pulp, even though
Food Eng Rev

Fig. 1 Different types of fruit powder based on the portion of the fruit used, adopted from Gurak et al. [32]

they contain most of the nutrients and bioactive compounds of the key factors for maintaining the stability of the powders
the fruit. Current research is thus focused on either the utiliza- during storage, handling, and transport [23]. The commonly
tion of these co-products as valuable ingredients [8] or the used material properties of fruit powders are moisture con-
production of WFPs [32]. However, the selection of drying tent, water activity, mean particle size, particle shape and
techniques in producing WFP requires a degree of compro- distribution, density, cohesiveness, flowability, and micro-
mise and introduces a few issues. There are some difficulties structure. These properties vary with powder type, drying
in converting whole fruit into powder with spray drying due to technique and operating parameters, the portion of the fruit
the non-functioning of the atomizer for the larger particles in used to produce the powder, and the carriers used in the
fruit pulp. In this case, solar drying, cabinet drying, and freeze drying process. The common drying techniques used for
drying are the preferred methods for producing WFP. the production of fruit powders are spray drying, drum
However, even though mechanical or solar drying is a cheaper drying, foam-mat drying, refractance window drying,
drying method, it results in poor-quality powders with respect freeze drying, and vacuum freeze drying. Spray drying,
to their nutritional and powder properties. Even though freeze drum drying, and freeze drying are the most widely used
drying is costly, WFP production with this technique is the methods in commercial processes. Reflectance window
best option as far as sensory, nutritional, solubility, and wetta- drying is currently being reported as a promising drying
bility properties are concerned. Drum drying is commonly technique at relatively low processing temperatures and
used to produce low-moisture baby foods and fruit powders, cost, although it requires longer drying times [49]. The
and it could be the most viable technique for producing WFPs major material properties of fruit powders, as influenced
in terms of cost-effectiveness and the quality of the fruit pow- by the different drying techniques and operating parame-
der produced. ters, are discussed in the following sections.

Fruit Powder Properties Moisture Content

A description of the primary properties in a particulate system Moisture content determines powder flowability, sticki-
underlies all the work in particle technology, which highlights ness, and storage stability due to its effect on T g and
Food Eng Rev

crystallization behavior. It is even more critical in the case Density


of tableting, since it is positively correlated with bulk den-
sity and compressibility up to a certain limit (e.g., 14% for The density ρ of a particle is defined as its total mass divided
starch derivatives) but negatively correlated with by its total volume, which is expressed as
flowability [84]. Moisture content is also a measure of m
drying efficiency, and it should be < 5% to ensure the pow- ρ¼ ; ð1Þ
v
der is microbiologically safe. The employed drying tech-
niques and their operating parameters have the greatest where m is the mass and v is the volume of the powder.
influence on the moisture content of fruit powders. The Depending on the techniques used to measure volume, the
drying time and quality of the final products are the major measured particle densities are either bulk, tapped, or true
issues that are greatly influenced by the drying techniques. densities. The density of fruit powder plays an important role
In producing mango powder to a fixed moisture level in determining the mixing and packing properties of the pow-
(0.05 kg water/kg solid), spray drying achieved this mois- der in a predetermined container, as well as formulating the
ture level within a significantly shorter time (< 5 s) com- powder into tablet form.
pared to drum drying, freeze drying, and refractance win-
dow drying. However, freeze drying and refractance win- Bulk Density Bulk density is related to the bulk voidage or
dow drying obtained a powder color that resembled natural porosity of the powder and is one of the properties used to
pulp [15]. A recent report on vacuum spray drying of or- specify certain products, like coffee powder. The bulk density
ange juice found it to be faster than spray drying due to the of a known mass of powder is measured by pouring the pow-
higher heat gradient between the steam and atomized par- der into a graduated cylinder and recording the volume
ticles, which produced a powder with a lower moisture occupied.
content than that of spray drying [36]. In the case of indi- The bulk density ρb is
vidual drying techniques, the moisture content of the final
products is influenced by the operating parameters. As m
discussed in a mini review by Phisut [57], the residual ρb ¼ ; ð2Þ
vb
moisture content of FJP produced by spray drying was
decreased with the increase in operating parameters, such where vb is the volume of the powder without tapping. Drying
as inlet temperature, atomizer speed, and the low dextrose methods have a profound effect on the bulk density of fruit
equivalent of the carrier agents, and the moisture content powders. As reported by Caparino et al. [15], the bulk densi-
was increased by increasing the feed-flow rate and concen- ties of freeze- and spray-dried mango powders are low com-
tration of the carrier agents. The increased inlet tempera- pared to those of refractance window- and drum-dried mango
ture creates a greater temperature gradient between the at- powders, meaning that the former powders have a higher po-
omized feed and drying air, whereas a higher atomizer rosity. In the case of freeze drying, the juice is dried under
speed creates smaller particles that facilitate a greater total vacuum from solid phase (ice) to vapor phase without passing
surface area for drying, thus creating powders with lower through the liquid phase, which prevents the collapse and
moisture contents. Juice powders produce powders with shrinkage of the product, resulting in porous dried materials
higher moisture contents than those of WFPs, which could [41]. The addition of maltodextrin mostly contributes to the
be due to the pulp and fiber content of WFP helping in the increase in bulk density of the mango powder produced by
drying process [15, 53]. According to Gurak et al. [32], the spray drying, which is due to the accumulation and trapping of
moisture content of Jaboticaba fruit pomace powder was air in the skin-forming maltodextrin, which finally results in
much lower than that of the WFP, possibly due to the re- less dense and more porous particles [30]. However, the in-
moval of soluble materials with the extracted juice. There crease in the concentration of maltodextrin decreased the bulk
were hardly any sugar-acid molecules except high mole- density, as reported by Tze et al. [75] and Goula and
cule fibers in the pomace, which ultimately helped in the Adamopoulos [31]. The reasons behind the phenomena ex-
faster drying to the low moisture content. As discussed in plained by Zhao et al. [89] and Phisut [57] are the minimiza-
the BFruit Juice Powder^ section, fruit juice is a sticky tion of thermoplastic particles from sticking and the increased
product due to the presence of amorphous materials, such particle sizes. The operating parameters of the individual dry-
as low molecular sugars and organic acids, and freeze- or ing techniques influence the bulk density of fruit powders to a
vacuum-dried fruit powders are highly hygroscopic, which great extent. In the case of spray drying, the inlet temperature,
contributes to increased moisture content. The hygroscop- atomizer speed, and additive concentration have inverse ef-
icity of the produced Jaboticaba juice powder decreased fects on the bulk density [76], whereas the feed-flow rate has a
remarkably with the addition of the high-molecular- direct correlation on the bulk density, with a higher feed rate
weight biopolymer like maltodextrin [32]. yielding a greater bulk density. The effect of the air-flow rate
Food Eng Rev

depends on the moisture content of the final product, which significant influence on the tapped density of spray-dried
means that if the moisture content of the powder is high, then jamun powder, with lower inlet temperatures yielding higher
the bulk density will also be high [57]. The reason for decreas- tapped densities. Jamun powder exhibited the highest tapped
ing the bulk density with increasing inlet temperature during density at an inlet temperature of 145 °C and the lowest tapped
spray drying is due to the rapid drying of the droplet surface, density at 160 °C during spray drying. Tze et al. [75] ob-
which in turn creates expanded and hollow particles by served the same phenomenon for spray-dried pitaya pow-
forming vapor-impermeable films on the droplets [28, 73, der, where the tapped density was reported to decrease with
74, 78]. In terms of atomizer speed and additive concentration, increasing inlet temperature and maltodextrin concentra-
the development of small droplets due to the increase in the tion. As explained in the bulk density section, the high
atomizer speed, the increased inhibition ability of drying ad- inlet temperature creates a large cavity in the powder par-
ditives in sticking to the thermoplastic particles, and the skin- ticles, resulting in larger sizes, which ultimately affects the
forming ability of the drying additives in entrapping air bub- tapped density due to the high porosity of the particles. The
bles are the major factors that influence the bulk density [31, type of fruit powder also has a significant effect on the
42]. WFP has shown the highest bulk density among the fruit tapped density, as WFP generally exhibits a higher tapped
powder types [36, 53, 67, 88]. This implies that the WFP density than juice powder. Ong et al. [53] reported that the
particles occupy larger spaces and have fewer voids than juice tapped density was mostly influenced by particle size and
and extract powders. A lower bulk density indicates more shape. Studies of mango, guava, and pitaya WFPs have
entrapped air within the void spaces, which increases the pos- shown that the particle size, and thus the tapped density,
sibility of oxidation and subsequently decreases the storage of the guava powder was the highest [53, 88].
life of the powder. Lower bulk densities also imply poor pack-
ing and the need for larger packaging volumes [45, 67], which
Flowability and Cohesiveness
can have practical implications for transport costs.
Flowability and cohesiveness are two important properties of
Tapped Density During handling and transportation, the pow-
dried particles; the former is expressed as the Carr index (CI)
ders settle, resulting in an increase in bulk density. Therefore,
[16] and the latter as the Hausner ratio (HR) [33]. The Carr
the tapped density is the more appropriate term to use in these
index is also used to represent the compressibility of the pow-
cases, which is also called increased bulk density after me-
der, where higher values of the Carr index represent poor
chanical trapping. The tapped density also reveals the packing
flowability and high compressibility. The Carr index is calcu-
behavior of the powders, even though it is influenced by many
lated as
other factors, including particle size and distribution, shape,
surface roughness or morphology, cohesiveness, and surface ðρt −ρb Þ
CI ¼  100: ð4Þ
charges [10]. The tapped density is measured by pouring a ρt
defined mass of powder into a graduated cylinder and tapping
the cylinder until a final constant volume is achieved. The The classification of powder flowability according to the
tapped density ρt is calculated as Carr index is shown in Table 1.
The Hausner ratio is defined as the ratio of the tapped
m
ρt ¼ ; ð3Þ density to the bulk density and is expressed as
vt
ρt v0
where vt is the constant volume of the powder after tapping. HR ¼ ¼ ; ð5Þ
ρb v n
The bulk and flow properties of the powders are generally
influenced by the interparticulate interactions among the par- where v0 and vn are the loose and tapped volumes, respective-
ticles. A relative measure of these interactions is practically ly. The Hausner ratio is used to classify powder cohesiveness,
assessed through a comparison of the bulk and tapped densi- which is a good measure of powder consistency and
ties. This comparison is often used as an index of powder flowability. The lower the cohesiveness (lowHR), the higher
flowability. The interparticulate interactions are less signifi- the flowability of a powder. The classification of powder co-
cant for a free-flowing powder, with both densities exhibiting hesiveness, along with flow properties according to HR, is
considerable closure, whereas powders with a poor flowability shown in Table 1.
possess a significant difference between their bulk and the Specific reports that explore how different drying tech-
tapped densities due to the greater interparticulate interactions niques and drying parameters influence the flowability and
among the particles. Scientific reports related to the effects of cohesiveness of fruit powders are limited. Yusof et al. [87]
drying type, drying conditions, and powder type on the tapped reported that oven-dried pitaya powder had a good flowability
density are limited and inconsistent. According to and low cohesion, as indicated by its HR value, whereas spray
Santhalakshmy et al. [67], the inlet temperature had a drying yielded a poor flowability and high cohesion [75], and
Food Eng Rev

Table 1 Carr index [16] for powder flowability for this difference. The same finding has been reported for
CI (%) Flowability Hausner ratio spray-dried dairy powders [40], where powder flowability
was strongly influenced by its surface composition, particu-
< 10 Excellent 1.00–1.11 larly for fat-containing powders. Beside particle shape, the
11–15 Good 1.12–1.18 esterification of pectin influences powder flowability [20],
16–20 Fair 1.19–1.25 with high methoxy pectin having a fair flowability and less
21–25 Passable 1.26–1.34 cohesion than low methoxy pectin. Bhandari [12] reported
26–31 Poor 1.35–1.45 that increased fat coverage on the surface can result in poor
32–37 Very poor 1.46–1.59 wettability, reduced flowability, and increased oxidation po-
> 38 Very, very poor > 1.60 tential. Increased protein coverage also results in a change in
the surface morphology of the powder particles. For example,
a more wrinkled surface was found due to the high protein
fair flowability and high cohesion were observed for freeze- surface coverage [81]. The coverage of particles by high-
dried pitaya powder [88]. The larger sizes and irregular shapes molecular-weight compounds can reduce the hygroscopicity
of the particles of the oven-dried pitaya powder, compared to and encapsulation efficiency of the volatiles and bioac-
those of the spray- and freeze-dried powders, were described tives [25], with the high protein concentration and dense
as the major reasons for this variable behavior. The same trend surface structure (crust) normally occurring during the drying
was reported for spray-dried jamun fruit powder [67] and wa- process.
termelon and carambola powders [66]. However, spray-dried
pineapple powder was reported to have good flowability and Particle Size, Shape, and Distribution
medium cohesion, whereas mandarin yielded fair flowability
and intermediate cohesion [66]. Despite having a smaller par- Particle size, shape, and size distribution all play important
ticle size than pineapple juice powder, watermelon juice pow- roles in the processing, handling, and shelf life of food pow-
der would be expected to exhibit better powder flowability ders, with particle microstructure being an important factor
and lower cohesion due to the aggregation of the particles. that influences powder functionality, stability, and flowability.
However, the low particle size and lowest moisture content They are greatly influenced by the drying process employed,
of watermelon powder made it highly cohesive powder with a the conditions, and the powder type. Caparino et al. [15] re-
poor flowability. Decreased electrostatic forces and strength- ported on the influence of freeze drying, drum drying, reflec-
ened van der Wall forces attained due to low moisture content tance drying, and spray drying on particle morphology, where
in the watermelon powder contributed to the poor flowability mango juice powders with a 180–250 μm particle size range
and high cohesiveness. The high spray-drying inlet tempera- were compared. The particle shape of the spray-dried and
ture and addition of maltodextrin at a ratio of 1:4 produced an drum-dried mango powders was regular and irregular with
adequately free-flowing and less cohesive jamun juice powder sharp edges, respectively, whereas smooth, flaky, and uniform
[67]. The same trend was reported by Tze et al. [75] for pitaya thick particle sizes were observed in case of reflectance
powder produced at varying inlet temperatures and maltodex- window-dried mango powder. The freeze-dried mango pow-
trin concentrations. According to Cynthia et al. [21], good- der particles were reported to be most porous among the dry-
flowing tamarind powder was produced at an inlet temper- ing techniques studied. In a study of freeze-dried tropical
ature of 155 °C and a 70:30 pulp:maltodextrin ratio. When fruits, Athmaselvi et al. [9] reported that the average particle
drying whole fruits, powder flowability can vary based on size of guava, papaya, and sapota was all very small, with
the type and ripeness of the fruit. Whole green mango particle sizes in the 0.31–0.41 μm range. However, the sapota
powder was reported to possess a better flowability than juice powder exhibited free-flowing properties, whereas the
ripe mango powder or a mixture of green and ripe mango papaya powder was reported as sticky. Athmaselvi et al. [9]
powders [53]. However, powder from whole pitaya and attributed this stickiness due to the presence of pectic sub-
guava fruits produced by freeze drying exhibited poor stances, whereas the free-flowing properties of the sapota
flowability and high cohesion [88]. juice powder were due to a lamellar surface structure (with
Powder flowability is greatly influenced by the surface flake form) and a spherical arrangement. Lowering the freez-
composition of the powder, such as moisture, protein, fat, ing rate during the freeze-drying process of soursop fruit pulp
and fiber, with most of the reported results based on dairy resulted in particles with a higher porosity and a more ordered
powders. According to Saifullah et al. [65], high-fiber, low- structure [17]. Islam et al. [36] reported that vacuum spray
fat pitaya powder possesses a high flowability. Despite having drying produced orange concentrate powder with a smaller
same amount of fiber and protein, guava powder showed poor volume distribution and a smaller average particle diameter,
flowability compared to mango fruit powder. The high fat which was linked to atomization at low temperatures under
content of guava powder was described as the main reason vacuum conditions. However, the particle diameter increased
Food Eng Rev

with increasing maltodextrin in the feed, thus reducing the viscosity, watermelon and pineapple, had smaller particle
hygroscopic and stickiness properties of the powder during sizes than those of high viscosity fruit juices, carambola and
vacuum spray drying. mandarin. There were also large variations in their surface
Reports on spray-dried fruit powder are abundant, with morphology. Mandarin and pineapple powder particles were
most reports containing a discussion on how the spray- fused and clumped together, whereas small, large spherical,
drying parameters influence the particle size, distribution, and large globular, and ellipsoidal particles were observed in
and shape of the powder. Phisut [57] and Verma and Singh the carambola and watermelon powders.
[77] critically reviewed the influence of spray-drying param-
eters on spray-dried fruits and vegetable powders. As
discussed by Phisut [57], the inlet temperature has a great Glass Transition
influence on the particle morphology and size of spray-dried
fruit powders. Low inlet temperatures made the surface of the A phenomenon of changing glass into a supercooled melt
powder particles shriveled, and the surface became smooth (rubber) during heating, or to the reverse transformations dur-
with increasing inlet temperature. The higher inlet tempera- ing cooling, is termed glass transition, and the temperature
tures led to a higher drying rate, which facilitated the faster associated with it is called the glass transition temperature Tg.
evaporation of water, producing hard crusts and smooth sur- Both glass and rubber are in a non-crystalline state. Glass
faces. This discussion was based on the findings of Tonon transition is a property that specifically relates to an amor-
et al. [73] for acai juice powder and Alamilla-Beltran et al. phous material. A material in either a glassy or rubbery state
[7] and Nijdam and Langrish [48] for milk powder. is not at thermodynamic equilibrium and therefore is unstable
Another important parameter is the atomizer speed, which relative to the crystalline form [13]. Fruit powder is amor-
influences the particle size and morphology of the fruit pow- phous in nature, and this state is metastable, such that its
ders. According to Phisut [57], higher atomizer speeds result- components may undergo phase and state transitions through-
ed in smaller particle sizes and also prevented skinning on the out the drying process and during storage. The most common
droplets. The particle size and morphology are also influenced problem associated with the Tg of fruit powder is the sticki-
by the type, concentrations, and polymerization of the carrier ness and caking potential at a given condition [12]. About
agents [73, 74, 85]. The increased molecular size, as well as 90% of the dry substance of fruit juice contains different
the increased concentration of the carrier agents, resulted in types of sugars, and their effects on the glass transition-
the increased mean diameter of the powder particles. The feed related changes of fruit powder are well recognized [77].
viscosity and molecular size of the polymers are the main The stability of the glassy amorphous state of fruit powder
reasons behind this phenomenon. Similar observations were is very limited, and the storage temperature of the powder
reported by Cynthia et al. [21], where increased coating agents above the Tg of an amorphous solid changes its phase from
resulted in larger particle sizes, ranging from 147.9 to 480 μm the glassy to the rubbery state. In this state (rubbery), the
for spray-dried tamarind pulp. Compared to tamarind pulp molecular mobility of the matrix and the reactants are accel-
powder, the particle size of jamun powder was very small erated, which results in an increased rate of physicochemical
(145.30–463.23 nm), and the particle size increased with in- changes in the fruit powders, such as sticking, collapse, cak-
creasing inlet temperature, as reported by Santhalakshmy et al. ing, agglomeration, crystallization, loss of volatiles, brow-
[67]. However, the particles were spherical in shape, with ning, and oxidation [13]. These changes directly affect other
some degree of shrinkage when spray dried at a high inlet powder properties as well, including the flowability, com-
temperature, compared to the smooth surface when pro- pressibility, and compactibility. Fan and Roos [26] reviewed
duced at low temperatures. A similar trend was also report- the current understanding of the glass transition, structural
ed by Chegini and Ghobadian [19] for orange juice powder relaxations, and corresponding relaxation times, as well as
and Lee et al. [43] and Tze et al. [75] for dragon fruit. The their relevant applications on glassy food solids, and pro-
feed rate and inlet temperature were positively correlated posed the strength S concept in controlling solid properties,
and the atomizer speed was negatively correlated with the such as stickiness, caking, collapse, and crystallization. This
particle size of spray-dried orange juice powder according concept describes the solid flow characteristics and structural
to Chegini and Ghobadian [19]. The particles of spray- transformations within mixtures of glass-forming carbohy-
dried powders were generally spherical, with a smaller av- drates, proteins, and other food components by using WLF
erage diameter, whereas the particles of the lyophilized model-based analysis of τ above the calorimetric Tg [26, 46,
powders were characterized by sharp-edged, pale-colored 62]. According to Fan and Roos [26], the S concept was
particles with a larger average diameter [54]. developed to study non-crystalline food materials and their
Saikia et al. [66] observed broad variations in the particle solid flow properties in typical processing and storage condi-
size distribution of four different fruit powders produced by tions, where a component or miscible components within the
spray drying. According to their report, fruit juices with a low food structure may experience the glass transition.
Food Eng Rev

Compressibility of Fruit Powders plastic deformations, and/or the fragmentation of particles


[35]. Elastic deformation is reversible, whereas plastic, visco-
Tablets are one of the important forms of pressure agglom- elastic, and plastic/brittle deformations are time- and shear
erates in the pharmaceutical metallurgy, ceramic, and rate-dependent.
chemical industries. Moreover, they are also gaining popu-
larity as a form of compact food in the food industries. The list
Principles of Compaction
of foodstuffs prepared using compaction covers sweeteners,
confectioneries, dietary supplements, instant products (e.g.,
The types of tablet presses used for tableting studies are either
stock cubes), and functional foods [61]. Candies and several
single-station (eccentric), multi-station (rotary), or simulator
types of food supplements produced by compaction, shown in
presses. Uniaxial die compaction is a single-station cold press
Fig. 2, are available in retail markets.
widely used in tableting studies due to its simplicity in oper-
BTasty Hazmi^ is a salty-sour tablet that is believed to be
ation and data acquisition. The common features of uniaxial
helpful in digestion, and is very popular to the people of
presses consist of an upper punch, a lower punch, and a die as
Southeast Asia. Vitamin C tablets are common dietary supple-
the principle parts (Fig. 4). The basic principles of all tablet
ments. Sweet chewable tablets, produced in a range of differ-
presses are typically the same, where the process generally
ent colors and sizes, are available in the Asian market. Good
consists of filling the die with loose natural or prepared pow-
tablet formation largely depends on the compressibility and
der, pressing with a desire pressure, releasing the pressure, and
compactibility of the powders upon tableting.
ejecting the tablet from the die.
In uniaxial die compaction, the powder is fed into the
die cavity, and the load is applied to the upper puncher that
Compaction Stages
moves down to compress the powder while the bottom
punch is kept stationery. The punch movement is given
The compressibility of a powder is defined as its ability to
by an eccentric mechanism driven by an electric motor or
decrease in volume under pressure, and the compactibility is
by using a universal testing machine. The tablet ejection is
the ability of the powder materials to be compressed into a
carried out by a mechanism that operates the lower puncher
tablet at a specified tensile strength [44]. The common steps
via a lifting block.
involved in tableting food powders are (1) rearrangement by
particle sliding, (2) elastic (reversible) and/or plastic
(irreversible) deformation, and (3) brittle fracture (irreversible Compaction Modeling
deformation) [58], as shown in Fig. 3. According to Barbosa-
Cánovas and Juliano [10], the volume reduction occurred only The visualization of the particle movement at different stages
by particle rearrangement, followed by elastic and/or plastic of compaction, as shown in Fig. 3, is usually expressed in the
deformation in the case of fine powders, whereas particle form of compaction curves. A compaction curve typically
fragmentation, in addition to rearrangement and formation, contains several distinct regions where the density or volume
is highly evident in the case of coarse or agglomerate powders reduction is plotted against the logarithm of compaction pres-
or ductile materials. A closer packing of the powder particles sure used, which acts as the driving force to develop several
occurs in the first step, serving as the main mechanism for the models to fit the curves. These equations are normally used to
initial volume reduction. The closer packing was obtained by characterize the overall compaction process, as well as the
having the finer particles fill the voids between the larger compressibility and compactibility of the powder [58].
particles. In this stage, the energy due to friction and greater Powders are classified into different groups with respect to
surface area for interparticulate bonding evolved. As the pres- the stages of the particle rearrangement, particle fragmenta-
sure increases, further rearrangement is prevented, and any tion, and particle plastic deformation during compression
subsequent volume reduction is accomplished by elastic and using three primary compaction equations, Kawakita and

Fig. 2 Examples of food


supplements and chewable
candies that are produced by
compaction and available in retail
markets

Tasty Hazmi (chewable tablet) Ceevit (Vitamin C tablet) Sweet chewable candy
Food Eng Rev

where C is the degree of volume reduction, P is the compac-


tion pressure, V0 is the initial at P, a and b are constants, ρp is
the apparent density at P, ϵ0is the porosity at the bulk state, and
ϵp is the porosity at P.
The rearrangement of Eq. 6, proposed by Kawakita and
Lüdde [38], becomes

P 1 P
¼ þ ; ð7Þ
C ab a

where the constant a represents the initial bed porosity, max-


imum volume reduction, or initial packing, thus describing the
compressibility of the powder, and the constant b is related to
resistance force or volume reduction tendency of the powder,
Fig. 3 Stages of compaction, adopted from Abdel-Hamid [1] thus describing the cohesiveness of the powder. This equation
yields the best fit for soft fluffy pharmaceutical powders dur-
Lüdde [38], Heckel [34], and Shapiro [70], following a pro- ing the early phase of particle rearrangement and compaction
tocol proposed by Nordström et al. [50]. About 20 equations at low pressures.
have been listed for describing compressive behavior of dif- The application of the Kawakita and Lüdde equation to
ferent powders. However, the Kawakita and Lüdde, Heckel, assess the flowability and compressibility of fruit powders,
and Shapiro equations are widely used in the pharmaceutical including other food powders, is shown in Table 2. The con-
industry. Most research reports also used these equations to stants a and b for chebula fruit extract and its formulation were
describe the compressive behavior of food powders. The com- compared by Prakash et al. [60], who revealed that chebula
paction equations used to describe the compressive behavior fruit extract has poor flowability and compressibility.
of different fruit/food powders are described in the sections However, they showed that the cohesiveness was reduced
below and also summarized in Table 2. and compressibility was improved when a 75:25 formulation
of fruit extract powder to Avicel pH101 was compressed into
Kawakita and Lüdde Model The Kawakita equation relates the tablets [60]. Avicel is a commercial free-flowing microcrys-
degree of volume reduction for a powder column to the ap- talline cellulose binder that decreases the porosity by coating
plied pressure of the system [39], which is defined as small fruit particles and increases the bulk density by reducing
the interparticle friction. Yusof et al. [87] reported a lower
V 0 −V abP ρ ∈0− ∈p value of a and a higher value of b of pitaya fruit powder
C¼ ¼ ¼ 1− 0 ¼ ; ð6Þ compared to maltodextrin, which revealed pitaya powder as
V0 1 þ bP ρp 1−∈p
a highly cohesive powder with less flowability and compress-
ibility. However, when the maltodextrin level was increased in
the pitaya powder, the porosity was also increased due to the
presence of free-flowing maltodextrin within the small parti-
cles of the pitaya powder. This behavior of increasing porosity
with increasing binder concentration has also been reported by
other researchers studying on pitaya and guava powders, both
individually and in a binary mixture [88]; green mango and
ripe mango powders, both individually and in a binary mix-
ture [53]; and maize powder [86]. According to [88], guava
powder possessed the highest a value, followed by the binary
mixture, and then the pitaya powder, indicating the highest
initial porosity and compressibility of guava powder and the
lowest values for the pitaya powder, with binary mixture
possessing values that were in between. The porosity of
guava-pitaya mixture increased due to the larger particle size
of the guava powder. There is a direct relation between a and
1/b, which means that a degree of compression is achieved by
Fig. 4 Schematic diagram of uniaxial die compression, adopted from the applied pressure. A higher pressure is therefore necessary
Yusof et al. [87] to prepare guava tablets compared to the pitaya and mixed
Food Eng Rev

Table 2 Tableting of fruit/food powders

SL. No. Powder source Mixture type Model used Parameters studied Key compression behavior References

1. Pitaya Single Kawakita and Lüdde a and b Low a and high b indicate highly [87]
cohesive powder; low flowability.
2. Sweet potato Binary None Plastic and elastic Plastic deformation in stevia is [69]
and stevia work greater than in sweet potato
powder.
3. Sago starch Single Heckel and Kawakita A, K, Py, a, and b Pre-gelatinization improves [79]
compressibility.
4. Date and spirulina Binary None Hardness Force of 10 tons produced [4]
optimum tablet.
5. Rice starch Single Heckel and Kawakita A, K, Py, a, and b Deforms by plastic deformation. [5]
6. Yam, corn, Single Heckel and Kawakita A, K, Py, a, and [2]
and rice
7. Wheat meal Single Heckel, Kawakita, Lordi Fitted model to Moisture content of wheat meal [71]
et al., Ferraro et al., moisture content fits the compaction models
and Feborode-and- linearly.
O’Callaghan
8. Milk and coffee Single Peleg C1, K1, and K2 Four-parameter model is the best [83]
to the describe compression
characteristics of the selected
food powders.
9. Mango Single and binary Kawakita and Heckel A, K, Py, a, and b Green mango powder is poorly [53]
compressible compared to ripe
and mixed mango fruit powders.
10. Guava and pitaya Single and binary Kawakita and Heckel A, K, Py, a, and b Guava powder is poorly [88]
compressible, whereas pitaya
powder is highly cohesive.
11. Instant coffee Single Four-parameter model Good model descriptor for [52]
agglomerate food powder
compression.
12. Terminalia chebula Formulated powder Kawakita, Heckel, a and b; A, K, and Formulated powder with fruit [60]
fruit and Leuenberger Py; γ and σmax extract showed reduced
cohesiveness and improved
flowability.

fruit tablets. According to Ong et al. [53], green mango pow- The mean diameter and porosity of pre-gelatinized sago starch
der showed a higher a value and was thus more compressible were increased, but its densities decreased significantly.
compared to ripe mango powder and the mixed fruit powder.
However, improved compressibility of the mixed fruit powder Heckel Model Densification of the powder column with pres-
was obtained when effervescent agents were added to the sure was modeled by Heckel [34], following the first-order
tablets, which was explained as a decrease in initial porosity kinetics that relate the powder relative density, such that
due to the mixed fruit powder pores being occupied by the
1
smaller disintegrant agent particles [53], which is in agree- ln ¼ kP þ A; ð8Þ
ment with the findings reported by Podczeck and Sharma ð1−DÞ
[59]. According to Skonecki et al.[71], a values were found
to be stable across a wide range of wheat powder moisture where P is the compaction pressure, D is the relative density at
contents, and the b value was the highest at a moisture content a given P, and k and A are constants. A plot of ln1/(1 − D)
of 18% for wheat powder. However, due to the presence of versus P is usually referred to as the Heckel plot, with the
considerable variations between the experimental and predict- intercept of the straight line fits to the linear part of the plot
ed model data, the authors concluded that the Kawakita and yielding the parameter A, which indicates the initial volume
Lüdde model provided the best fit, with a limited use for reduction of the powder bed due to the process of die filling
biological materials. According to Adedokun and Itiola [2], and particle rearrangement (no deformation occurs in this
pre-gelatinized starches exhibited a lower a value and a higher stage). The gradient of the Heckel plot k gives the plasticity
b value compared to native starches, where four grain starches of the materials, such that the greater the value of k, the more
were compared. The same findings were reported by Widodo plastic the material. The value of k also relates to the yield
and Hassan [79] for different pre-gelatinized sago starches. strength, and the reciprocal of k has been defined as the mean
Food Eng Rev

yield pressure, which has been used for the comparison of surfactants modulated the compressibility and tablet-forming
properties between different materials. The Heckel equation ability of the amorphous lactose particles by changing the bulk
gives the best fit at intermediate to high pressures and low or particle surface properties.
porosity in comparison to Kawakita and Lüdde equation,
which fits well at low pressures and high porosity. This equa- Sone’s Compressibility Model The mechanism of powder de-
tion has been extensively studied for characterizing the com- formation without particle yield or breakage is the best candi-
paction of pharmaceutical and ceramic powders. A list of re- date for using Sone’s compressibility, with the model con-
ports on the characterization of food powder compaction stants related to the powder characteristics providing a clear
using the Heckel equation is presented in Table 2. Heckel sense of the mechanical behavior of a given powder, which is
analysis of ripe and green mango powders and their binary expressed as
mixture was reported to be linear at the early stages of com- ρb −ρb0
pression and highly plastic and compressible when the ripe Y ð σÞ ¼ ¼ C 1 þ C 2 logσ; ð9Þ
ρb0
mango powder was tableted compared to green mango pow-
der and their binary mixture, as revealed from their k values on where Y(σ) is the density or volume fraction, ρb is the bulk
the Heckel plots [53]. This result has been related to the var- density under compression σ, ρb0 is the bulk density before
iation in particle size and porosity among the powders, which compression, and C1 and C2 are characteristic constants of
is in agreement with other reports [2, 59]. The same behavior the powder, with C1 representing the value of Y(σ) at a unit
was reported by Zea et al. [88], who used guava, pitaya, and stress and C 2 (known as the compressibility index)
their binary mixture in their analysis. However, despite having representing the change in relative density with the applied
the larger particle size in the binary powder mixture, the k stress [56]. The natural logarithm gives a better reflection
value of the guava powder was quite close to that of the mixed of the compression characteristics of the food powder,
powder, which was interpreted to be due to the variation in where the density function Y(σ) is expressed as a function
moisture content and agglomeration during the mixing of the of the porosity ϵ, such that
fruit powders. Heckel analysis of the compression of Assam
Boro rice starch was reported to yield good fits, where it was 1−ϵ ¼ a þ blnσ; ð10Þ
found to be highly compressible compared to commercial
where a is a constant and b is the compressibility index.
starch that was studied and deformed by plastic deformation
Data from confined uniaxial confined tests, analyzed using
[5]. A strong linearity, indicating dominant plastic deforma-
the above models to evaluate the compressibility of food
tion during the evaluation of the pre-gelatinized sago starch
powders, including fine salt, fine sucrose, corn starch, baby
using Heckel analysis, was also reported by Widodo and
formula, coffee creamer, soup mix, baker’s yeast, milk
Hassan [79]. The pre-gelatinized starch possessed a low yield
powder, ground coffee, ground corn, corn meal, lactose,
strength Py, which was indicated by the high plasticity of the
and flour, were compiled by Barbosa-Cánovas and
starch in its pre-gelatinized form compared to the fresh starch.
Juliano [10]. The compressibility of many of the above
Similar findings were reported by Adedokun and Itiola [2] for
powders was shown to be correlated with the internal co-
yam, rice, and corn starch powders that were evaluated using
hesion C and with particle deformability to an extent, and
the Heckel model. Heckel model evaluation of chebula pow-
that high compressibility was related to low flowability
der at granular or direct formulation did not show any linearity
[55, 68].
in the early stage of compression, yielding a higher A value,
which suggested compression due to die filling and particle
Four-Parameter Model The stress-strain relationship be-
rearrangement. The A value of the granule was higher, which
tween cellular materials could be described clearly using
indicated defragmentation and rearrangement of the granules
three- or four-parameter models and have been proven suc-
at low pressure. At high pressures, Heckel plot evaluation of
cessful in describing sigmoidal deformation over the full
the chebula powder showed a strong linear relationship, sug-
compression region. Swyngedau’s model fits food powder
gesting a highly plastic and compressible powder in its gran-
compression data well for instant agglomerated coffee, in-
ular form, which was also confirmed by its low Py value [60].
stant agglomerated low-fat (2%) milk, and instant agglom-
The evaluation of wheat flour due to changes in moisture
erated nonfat milk after confined uniaxial compression [52,
content by Heckel plot analysis provided a good fit within
82], which is defined as
the moisture content range of 10 to 16%, with increasing
moisture content yielding an increase in k value, which relates F ¼ A1 δB1 þ A2 δB2 ; ð11Þ
to a decreased compressibility of the material [71]. The effec-
tive deformability of amorphous lactose particles was investi- where F is the compressive force, δ is the deformation length
gated by Berggren et al. [11] using the Heckel number, where unit, and A and B are constants. A is in units of force over
they reported that the addition of stabilizing polymers or deformation length, and B is dimensionless. B1 (≤ 1) is a
Food Eng Rev

measure of the downward concavity of the force-deformation when the effervescent tablets are dissolved in simulated
curve at lower deformation, whereas B2 (> 1) is a measure of saliva fluid [53, 63–65, 72]. Tablets that possess similar
the upward concavity of the curve at higher deformation [10]. particle sizes, ingredients, and dissolution media but dif-
The typical force-deformation curves obtained from the ex- ferent chemical compositions, such as moisture, protein,
perimental data represent three phases, which explain the three and fat, were reported to yield different dissolution kinetics
steps of the compression mechanism and fit the above four- [64]. According to Barbosa-Cánovas and Juliano [10], the
parameter model well. presence of free fat on the powder particle surface reduced
the wettability of the powder, thus yielding tablets with a
Compression Versus Dissolution low dissolubility. There are several processes involved in
the dissolution of solid or powder materials, such as wet-
Aqueous solubility/dissolution is an important property for ting, swelling, sinking, and dispersion. In the case of fruit
using tablets as ready-to-serve juices and refreshment tablets containing disintegrants, the common dissolution
drinks. From the consumer point of view, easy, rapid, and phenomena observed are the swelling and subsequent sur-
complete dissolution is expected, with its performance be- face erosion of the tablets.
ing a major quality indicator of the food tablet [47].
Powder compressibility and the compaction force used to
form the tablets have direct influences on their friability,
hardness, and disintegration time. According to Adiba Conclusion
et al. [4], tablets made with 10 t-strength (where 1 t-
strength = 9.81 kN) possessed an acceptable degree of fri- Fruits and their extracts in powder form have many poten-
ability. The tablets became very friable at lower forces, tial applications as foods and food ingredients. However,
whereas they were excessively harder above this force, food/fruit powders in the form of tablets, such as sweet-
with the required time for dissolution increasing as a func- eners, confectioneries, dietary supplements, instant prod-
tion of tablet hardness. However, Yusof et al. [87] reported ucts (e.g., stock cubes), and functional foods are also
that the maximum allowable load of 10 ± 1 kN was re- gaining popularity in the food industries due to their eco-
quired on the uniaxial die to form pitaya tablets using the nomic methods of production, as well as providing conve-
Instron Universal Testing 5566 machine (Instron Machine, nience to consumers. The compressibility of the powder is
Canton, MA). This force was about ten times (~ 1 t- an important attribute in forming food tablets, which most-
strength) lower than that reported by Adiba et al. [4]. ly depends on the physico-chemical properties of the pow-
Powders with larger particle sizes should theoretically der, such as moisture content, water activity, particle den-
form tablets with higher porosity, such that the rate of tab- sity, particle size and shape, and flowability. High-
let dissolution should increase with increasing porosity moisture powder is less flowable but highly compressible
Saifullah et al. [65]. However, fine powders normally and less disintegrable. Powders with larger particle size
formed more compact tablets that exhibited slower disso- have higher bulk densities, which inversely affect the com-
lution rates due to the insufficient contacts between the pressibility. There are many models used to assess the
dissolution medium and the tablet particles. According to compressibility and compactibility of food powders. The
Ong et al. [53], green mango powder particles take longer most used models in studying the compressibility charac-
to dissolve, even though they are larger in size and possess teristics of fruit powders reported in the literature are the
a higher porosity, which is likely due to the required ex- Kawakita and Lüdde, the Heckel, Sone’s, and the four-
cessive force to form the tablets, thus making them harder parameter models. Since food powders are highly cohe-
and reducing the ability of the dissolution media to pene- sive, the four-parameter model is found to be best-suited
trate into the tablet for swelling and disintegration. Guava for sigmoidal compression deformation data. However, the
tablets showed the same dissolution behavior due to the Kawakita and Lüdde model and Heckel equation are wide-
same reason reported by Zea et al. [88]. As the moisture ly used to assess the compressibility and compactibility of
content and water activity of fruit powders increased, the fruit powders. From a technological point of view, fruit
tablets became harder with the same applied force and also powder in its compact form is an excellent alternative for
took longer to dissolve [4]. Dissolution is also strongly overcoming the problems associated with post-processing
associated with the tablet ingredients, chemical composi- handling, packaging, and the storage of fruit powders.
tion of powders, and dissolution media. Beside fruit pow- Powders in tablet form will be less hygroscopic due to
der, disintegrants, sugars, fillers, and organic acids are the the reduction in surface area, which also results in reduced
common ingredients used in fruit tablets. Effervescent packaging and transportation costs and increased storage
agents, which act as disintegrants, have a strong influence shelf life, thus providing convenience and affordable
on tablet dissolution, with the quickest dissolution reported prices to consumers at all levels.
Food Eng Rev

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