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Keywords: at Pb 0.001. The flowability and cohesiveness as determined by Carr index and Hausner ratio of individual fruit powders and
Flow properties their formulation were also different but in the range of passable class. The relationship of total dissolution time with
Fruit powder moisture, protein, fat content and porosity of fruit powder tablets was polynomial as determined by multiple regression
Dissolution analysis. Dissolution rate of effervescent fruit powder tablets was much higher compared to normal fruit powder tablets in
Fast dissolve
both dissolution medium (water and simulated saliva fluid). Among the fruit powder tablets, pitaya powder tablet went for fast
Tablet
Flowability dissolution (6 min) in simulated saliva fluid whereas guava powder tablets took the longest time (90 min) for complete
dissolution in water. Based on this study, a better understanding of the physicochemical properties of fruit powder and their
relationship with the dissolution rate and the effect of effervescent agents on the dissolution rate has been obtained, which is
essential for processing and handling of fruit powder and tablet preparation as well as for the improvement of the dissolution
rate.
© 2016 Elsevier B.V. All rights reserved.
Department of Food Technology and Rural Industries, Faculty of Agricultural Engineering and Technology, Bangladesh Agricultural University, Mymensingh 2202, Bangladesh
Article history: This research was conducted aiming to assess the flow and physicochemical properties of fruit powder and their relationship
Received 6 November 2015 with the dissolution of tablets containing effervescent agents. Commercial pitaya, pineapple, mango and guava fruit powders
Received in revised form 13 June 2016 were used as samples in this research. Fruit powder tablets were prepared by using direct compaction method. Powder
Accepted 17 June 2016 properties of individual fruits as well as their tablet formulation (fruit powder +effervescent agent + artificial sweeteners)
Available online 19 June 2016 analysedusing standard methods were found significantly different
1. Introduction
⁎ Corresponding author.
Tropical and subtropical parts of the world are blessed with E-mail address: yus.aniza@upm.edu.my (Y.A. Yusof).
different types of fruit which are very popular all over the world in
terms of taste and nutritional value. Most of the fruits are seasonal.
http://dx.doi.org/10.1016/j.powtec.2016.06.035 0032-
Fruits are mainly consumed fresh in the peak season and also 5910/© 2016 Elsevier B.V. All rights reserved.
processed into different types of products for preservation and further different physical and chemical treatments of juices. However,
use, such as juice, squash, nectar, concentrate, puree, jam, jelly and sometimes these treatments affect the quality of the juice.
pickle [1–4]. Fruit selection for processing into a specific type of Food scientists adopt a simultaneous heat and mass transfer
product depends upon the content of the fruit. For example, fruits with approach to dry the fruit juice into powder form. Fruit juice powders
high sugar and juicy pulp content are mostly processed into juice and provide a number of benefits over their liquid counterparts such as,
squash. Fruit juices and fruit based drinks are equally popular with (1) reduced volume, weight and packaging; (2) easier preservation,
people of all ages. Juice processing requires number of unit operations handling, transportation and storage; (3) and increased shelf life [7].
that increase the chance of contamination and the cost of production. Fruit powders are mainly used as instant fruit drink powder and
Further, due to the presence of a high amount of water and sugar, fruit consumed directly as refreshing drink after dissolving in water. The
juices are prone to spoilage by yeasts, moulds and bacteria [5,6]. potential other uses of fruit powder are as ingredients in baby food,
Enzymatic reactions are also responsible for degradation of the quality sweets, fruit yogurt, soup, cake, ice cream and confections [8–10],
of fruit juices. Hence, fruit juices possess a very short shelf life. To to enhance the colour, flavour and nutritional value of the products.
increase the shelf life, food processors use
Several drying methods are available for fruit juices such as spray
drying, drum drying, freeze drying and vacuum drying. Each type of
397 M. Saifullah et al. / Powder Technology 301 (2016) 396–404
drying method has its own limitations and advantages [1]. The 2. Materials and methods
different methods operate under different drying conditions.
Therefore, the physicochemical properties of fruit powder are varied 2.1. Materials
according to the method. Among the various drying methods the
most common, convenient and widely practiced by the industry is Four types of fruit powders, namely pitaya, pineapple, guava,
the spray drying method [11,12]; which provides rapid production and mango were used in this research. Spray dried fruit powders
through continuous operation. containing 10% maltrodextrin were bought from Syarikat Sains
Fruit powder is a dry and granular material. It is also bulky and Maju, Petaling Jaya, Selangor, Malaysia. Citric acid (Chem Pure®,
highly hygroscopic in nature. Therefore, it requires careful handling R&M Marketing, Essex, UK), and sodium carbonate (Merck
and KGaA, 64,271 Darmstadt, Germany) were used as effervescent
Table 1 agents; these chemicals were brought from the local company LGC
Flowability classification (Lebrun et al., 2012). SCIENTIFIC, 43,200 Balakong, Selangor Darul Ehsan, Malaysia.
Flowability Carr Index (CI), % Hausner Ratio (HR) Stevia (Botanical Essence Marketing Sdn Bhd, Malaysia) was used
Excellent 0–10 1.00–1.11 as a natural sweetener in the formulation of the fast dissolving fruit
Good 11–15 1.12–1.18 powder tablets.
Fair 16–20 1.19–1.25
Passable 21–25 1.26–1.34 2.2. Formulation and mixing of fast dissolving tablets
Poor 26–31 1.35–1.45
Very poor 32–37 1.46–1.59
Each tablet contained 47.3% fruit powder, sodium carbonate
Very, very poor N38 N1.60
32.7%, citric acid 10% and stevia 10% [16]. All samples were
packaging during storage and transportation. Adiba et al. [13], Zea
measured and put into a plastic container, then mixed thoroughly in a
et al. [8] and Ong et al. [14] reported the compaction of fruit
mixing machine (Glas-Col, S/N 477625, USA) for 30 min at 15 rpm
powder for the preparation of fruit drink tablets, which offers a few
with 15 min clockwise and 15 min anticlockwise directions to create a
benefits over the powder form such as good physical and chemical uniform mixture. Then the sample mix was measured into 2.5 g
stability, prolonged shelf life, less space required for storage and portions and placed in plastic containers for further use, such as tablet
transportation, elegant appearance and greater acceptance in terms preparation and analysis of physical properties.
of presentation [15]. However, in tablet form the hygroscopicity of
the powder becomes low due to the reduction of the surface area of 2.3. Physical/powder properties
the powder. Therefore, it takes a longer time for dissolution.
However, people usually prefer rapid dissolving tablets. The 2.3.1. Particle size
application of super disintegrants to reduce the total dissolution The particle size and size range of the powder samples were
time has been reported by Zea et al. and Ong et al. [8,14]. The measured by using a particle size analyser (Malvern Mastersizer 2000
dissolution of a fruit powder tablet is a physicochemical process, Instrument Ltd., U.K.) using dry dispersion method. The Mastersizer
which is influenced by the physical and chemical properties of the 2000 utilises a laser light diffraction technique to analyse the size of
ingredients. Though a super disintegrant can improve the the particles. For this experiment, the powder samples were placed in
dissolution rate of fruit powder tablets, conversely it may affect the the particle size analyser and the data was recorded automatically.
physical properties of the fruit powder. However, to the knowledge
of the authors, no studies have been carried out to demonstrate the 2.3.2. Morphology of fruit powder and mixture of ingredients for
effects of a super disintegrant on the properties such as bulk tablet preparation
density, tap density, flowability and compressibility of the powder. The morphological structure of powder particles and the
This includes the porosity and dissolution of the fruit powder tablet distribution of different ingredients in the mixture were observed
when effervescent agents used as super disintegrants are mixed with through a scanning electron microscope (SEM) (Hitachi High
the fruit powder to produce fast dissolving fruit powder tablets. Technologies America Inc., IL). The samples were placed on double
Thus the objectives of this work were to investigate the physical adhesive tape stuck on gold aluminium pins. Then, the pins were
and chemical properties of four types of fruit powders; the physical positioned in the SEM machine, and the particle shape and particle
properties of the fruit powders after adding effervescent agents; and distribution visualised through a computer.
finally the effect of physicochemical properties of the fruit powders
on the dissolution of fast dissolving fruit powder tablets in different 2.3.3. Bulk density
dissolution mediums. The bulk density of the samples was determined manually by
pouring 2.5 g of fruit powder into a 10 mL graduated measuring glass
cylinder. The bulk density was calculated from the ratio of the mass of
powder to the volume occupied by the powder [17].
M. Saifullah et al. / Powder Technology 301 (2016) 396–404 398
Fig. 1. (a) Dissolution of fruit powder tablet in water; (b) dissolution of fruit powder tablet in simulated saliva.
Table 2
SEM image of fruit powder and fruit powder containing effervescent agents.
Sample Fruit powder Fruit powder mixture
399 M. Saifullah et al. / Powder Technology 301 (2016) 396–404
Pitaya powder
Pineapple powder
Mango powder
Guava powder
pineapple, guava, and mango fruit powders. Moisture content in the (Instron Universal Testing Machine-5566, Canton MA, UK) was
sample was measured by using an oven drying method. Ash content used to compress the powder samples into tablet form. The Bluehill
was determined using a standard method, in which 5 g of sample was software (Canton MA USA) was the operating software of that
kept in a muffle furnace and ashed at a maximum temperature of 525 particular machine, which helped to maintain a compaction speed of
°C for 6 h, then the ash was cooled in a desiccator and weighed [22] 0.1 mm/min at four different force settings of 9.8 kN, 8 kN, 6 kN
The Kjeldahl method (AOAC) [22] was used to determine the protein and 4 kN. After reaching the maximum force set for tablet
content of the sample. Fat content was determined by using the formation, the tablet was ejected from the die and the thickness of
Soxhlet method [22]. The determination of fibre content was based on the tablet was measured to calculate the final volume and density of
the method by Ranganna [23]. The total carbohydrate content of the the powder in tablet form.
sample was calculated by the difference of the total weight of the The Kawakita and Lüdde [28] model equation was used to
sample (100%) and the summation of all other constituents (crude determine the compressibility of four types of powder mixtures. The
protein, fat, moisture content, ash and crude fibre) [24]. All proximate mathematical formula of this equation is as follows:
analysis was performed in triplicate, and an average reading was
determined with standard deviation. P P 1C a ab
A0
At− 3.2. Physical/powder, chemical and flow properties of fruit powders
Percentage dissolution at any time ¼ 100
Af The chemical and physical properties of the fruit powders have a
major influence on the design, optimisation and performance of fruit
powder products. The physical properties/ powder properties
Here, A0 is the Absorbance of a control sample (fresh medium), A t include particle size, particle shape, surface morphology of the
is the Absorbance of the sample at any time, powder particles, bulk density, tapped density, true density and
Af is the Absorbance of the sample when complete dissolution porosity; the chemical properties include the proximate composition
occurs. such as protein, fat, carbohydrate, moisture content, and water
activity; and the flow properties include Carr Index, Hausner's ratio,
2.8. Statistical analysis and flowability.
Fig. 2. (a) Relationship between percent moisture content versus total dissolution time, (b) relationship between percent protein content versus total dissolution time, (c) relationship between percent
fat content versus total dissolution time, (d) relationship between percent porosity versus total dissolution time. *DTW = dissolution time in distilled water, *DTS =
403 M. Saifullah et al. / Powder Technology 301 (2016) 396–404
and 4.10 ± 0.03% respectively. During spray dying, usually Ash refers to the inorganic residue remaining after either ignition
denaturation of protein occurs. Anandharamakrishnan et al. [40] or complete oxidation of organic matter in a foodstuff. The ash content
reported the denaturation of whey proteins during spray drying. The of pitaya, pineapple, mango, and guava powder were 1.20 ± 0.08%,
rehydration capacity of denatured protein differs from the normal 2.60 ± 0.07%, 2.10 ± 0.08% and 3.10 ± 18%, respectively. Like other
protein. The denaturation of protein results in a decrease in components, the carbohydrate content in the fruit powder varies from
wettability/solubility of powdered foodstuff [41]. Fig. 2 (b) one type to another. Table 2 shows that the highest carbohydrate
indicates the relationship between protein content and dissolution content was in pineapple and mango powders with 88.10 ± 0.16% and
time. The fat content of any powdery product has a significant 87.00 ± 0.09% respectively, while the lowest carbohydrate content
influence on its solubility capacity or dissolution rate. Usually fat was in guava powder at 79.50 ± 0.2%. The water activity of any
exhibits hydrophobic behaviour and hinders the water absorption foodstuff represents the ratio of the vapour pressure of water in the
capacity of fruit powders. Millqvist-Fureby et al. [36] reported sample and the vapour pressure of pure water. It is a very important
similar findings for milk powder. Fig. 2 (c) shows that there is a parameter to indicate the availability of water in food systems for
polynomial relationship present between the dissolution time of biochemical reactions and microbial activity. When the water activity
fruit powders and the fat content for both dissolution mediums. value in any food product is b0.6, it is microbiologically stable and
Table 4 shows that the highest amount of fat was found in guava indicates no growth of spoilage organisms and pathogens [45]. The
powder 4.10 ± 0.19%. The fat content in pitaya, pineapple, and water activity value of all four types of fruit powders indicated that the
mango was 1.00 ± 0.09%, 0.5 ± 0.03% and 2.3 ± 43%, respectively. pitaya, pineapple, mango and guava powders were microbiologically
The multiple regression analysis results presented in Table 5 show stable.
that the polynomial model is the most suitable model to express the
relationship of dissolution time with moisture content, protein 3.2.3. Powder flow properties of fruit powders
content and fat content of the fruit powder, as well as the porosity Flowability is an important parameter for a powdered material
of fruit powder tablets. measured by the Carr index and Hausner ratio. The flowability usually
The fibre content in pitaya was found to be the highest amount at depends on the physical properties of the powder, such as particle size
8.0 ± 0.25% among all the four types of fruit powders. The fibre and shape, surface structure, particle density, and bulk density [46–
content for the other three types of fruit powders, which include 48]. The powder surface composition, such as fat, protein, moisture
pineapple, mango, and guava powder, were 0.93 ± 0.25%, 1.00 ± content also affects the flowability of a powder [49]. Table 3 depicts
0.05% and the flowability of the fruit powders and fruit powder mixtures. The
5.0 ± 0.3% fibre, respectively. The hydration rate of fibre is important variation in the flowability of the fruit powders was due to the powder
for fast dissolution rate of the products. However, the processing particle morphology (different particle sizes and shapes of the fruit
conditions such as grinding, drying, heating and the environmental powder particles) and the interaction of the powder particles. When the
conditions such as temperature, pH, ionic strength, dielectric constant powder contains particles of different sizes, then the smaller particles
of the surrounding solution and nature of the ions can also influence fill the void spaces created by the larger particles. This causes an
the hydration characteristics of fibre [42–44]. The hydration or increase in resistance to flow and reduces flowability which may be
solubility rate of fibre also depends upon the type of fibre. due to an increase in inter-particle friction. Irregular particle shapes
Table 5
Regression analysis result of dissolution of fruit powder tablet in relation to different parameters.
Dissolution in water Dissolution in saliva
2 2
Relationship Model Equation R Equation R
Relationship between percent moisture content versus total dissolution time Exponential y = 31.524e-0.396x 0.7615 y = 33.34e-0.452x 0.7647
Linear 0.7375 0.7375
y = −3.2777× + 19.431 y = −3.2777× + 18.431
Logarithmic y = −11.74ln(x) + 22.618 0.7668 y = −11.74ln(x) + 21.618 0.7668
Relationship between percent protein content versus total dissolution time Exponential y = 4.7111e0.1332x y = 0.7005 y = 3.825e0.1516x 0.7016
Linear 1.1121× + 3.671 0.6914 0.6914
y = 1.1121× + 2.671
Logarithmic y = 3.6639ln(x) + 3.1345 0.5911 y = 3.6639ln(x) + 2.1345 0.5911
Relationship between percent fat content versus total dissolution time Exponential y = 6.4337e0.1032x 0.9683 y = 5.4533e0.1174× 0.9697
Linear y = 0.862× + 6.2716 0.9569 y = 0.862× + 5.2716 0.9569
Relationship between percent porosity versus total dissolution time Exponential y = 61.867e-0.077x 0.7098 y = 71.971e-0.088x 0.7135
Linear y = −0.6378× + 24.944 0.6824 y = −0.6378× + 23.944 0.6824
Fig. 3. (a) Pressure versus density relationship for normal fruit powder tablet, (b) pressure versus density relationship for effervescent fruit powder tablet.
and particle surfaces reduce the contact surface area among the hence had the lowest compressibility among all four types of fruit
particles and reduces the cohesive force among the particles, which powders. The compressibility, porosity and resistivity to
results in an increase in flowability. Table 2 shows that pitaya powder compaction values for the raw fruit powders were changed when
contains particles with shrinkage of the outer surface and less particle mixed with other ingredients (effervescent
size variation. These aspects may cause pitaya powder to be more
flowable than other types of fruit powders. Table 6 also shows that Table 6
mixing of fruit powder with effervescent agents and artificial Kawakita and Ludde equation constants for fruit powder tablets.
sweeteners results in a decrease in flowability for all types of fruit Normal fruit powder Fruit powder mixture
powders. Saifullah et al. [16] reported same type of results for mix Sample a b R2 a b R2
fruit powders with effervescent agent and artificial sweeteners.
Pitaya powder 0.43 0.12 0.997 0.53 0.18 0.994 Pineapple powder 0.54 0.09
However, according to Carr [25] and Hausner [26], all types of fruit 0.994 0.46 0.79 0.982 Guava powder 0.36 0.19 0.998 0.41 0.49 0.998 Mango
powders and fruit powder mixtures have been shown to have a powder 0.53 0.07 0.970 0.40 0.15 0.996
passable flowing characteristic. Variation was found in the flowability
among the fruit powders and fruit powder mixtures such pitaya powder agent and sweetener) as part of the preparation of the effervescent fruit
showed the highest flowability; on the other hand guava powder powder tablets (Table 6). Ong et al. [14] and Saifullah [16] also
reported that changes in compressibility, porosity and resistivity to
mixture showed the lowest flowability among all types of fruit
compaction values of fruit powders when mixed with effervescent
powders and fruit powder mixtures. The compressibility of the powder
agents. Among the four types of mixtures, pitaya powder mixture was
was different due to the flow property. Knowlton et al. [50] reported
found to be the most porous and resistant to compaction was less than
that flowability has a great influence on transportation, formulation and
pineapple and guava powder mixtures. Therefore major changes
mixing, compression and packaging.
occurred in volume and density during compaction and tableting. Fig.
3 (b) shows the pressure versus density relationship for the fruit
3.3. Compressibility of fruit powders
powder mixtures. Mango powder exhibited the lowest porosity and
resistance to compaction. The guava powder mixture showed a
In the direct compaction tableting method, a compression load is
minimum change in density under applied pressure compared to the
applied to the powder sample in a die cavity through upper and
other mixtures. When a powdery material is more porous and the
lower punches. During compression, plastic deformation of the
resistance to compaction is low, then the powdery material is more
powder occurs. The compressibility property of a powder is very
compressible. Porosity and resistance to compressibility of a powder
important during tableting. The physical deformation of particles,
inter particle bonding, and tablet quality all depend upon it. In this depend upon its particle size, shape and flowability. When any
study, the Kawakita and Lüdde model Eqs. (4) and (5) has been powdery material contains particles of a regular shape with a high
used to describe the compressibility behaviour of all types of fruit variation in particle size, then it becomes less porous, because the
powder mixtures. The constants a and b were determined by small particles fill up the void spaces between the larger particles [52].
plotting the data in a P/C versus P graph and linear fitting of the Particle size and particle size distribution affects the compatibility
equation (Table 6). The constant a represents the initial and rearrangement of particles [53]. Optimal particle shape, size and
compressibility and porosity, while the constant b represents the particle distribution can provide better flow properties and compaction
resistance to compaction of the material. The value of b represents behaviour. The mechanical strength of a tablet depends upon the
the resistance force of the powder particle against compressive load compatibility of the powder particles, which has a strong influence on
[51]. the total dissolution time and the rate of dissolution [54].
Table 6 shows that among the four types of fruit powders,
pineapple powder and mango powder showed maximum porosity
and less resistance to compaction. Fig. 3 (a) shows a pressure versus
density relationship for a normal fruit powder tablet. The guava
powder showed less porosity and high resistance to compaction and
405 M. Saifullah et al. / Powder Technology 301 (2016) 396–404
3.4. Relationship between porosity and dissolution of fruit powder
tablets