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Optimization of process parameters for spray drying of Tongkat Ali extract

Article · January 2015

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Journal of Engineering Science and Technology
Special Issue on SOMCHE 2014 & RSCE 2014 Conference, January (2015) 31 - 41
© School of Engineering, Taylor’s University

OPTIMIZATION OF PROCESS PARAMETERS

FOR SPRAY DRYING OF TONGKAT ALI EXTRACT

NOOR H. HARUN1, A. ABDUL-AZIZ1,*, WAN M. WAN-ZAMRI1,

ROSHANIDA A. RAHMAN2, R. AZIZ1
1
Institute of Bioproduct Development, University of Technology Malaysia,
81310 Skudai, Johor, Malaysia
2
Bioprocess Department, Faculty of Chemical Engineering, University of Technology
Malaysia, 81310 Skudai, Johor, Malaysia
*Corresponding Author: azila@ibd.utm.my

Abstract
Tongkat Ali extract is well known for its aphrodisiac effect. Apart from that,
Tongkat Ali extract also exhibits other therapeutic effects such as cytotoxic,
antitumor, anti-pyretic and antimalarial activities. Most dried Tongkat Ali
extracts produced in Malaysia are obtained using spray drying as compared to
freeze drying because it is a cheaper process that produces dry particles of good
quality. However, a major drawback of the manufacturing of Tongkat Ali is the
low overall yield of dried Tongkat Ali, which is only about 3%. In this work,
the focus was on the spray drying process. The influences of four variables
(feed temperature, feed flow rate, air pressure, and air inlet temperature) on the
efficiency of spray drying were investigated using response surface
methodology (RSM). Based on the analysis of variance (ANOVA), the
optimum conditions obtained were air inlet temperature of 160°C, feed
temperature of 25°C, air pressure of 17.91 psi and feed flow rate of 4.86
ml/min. The efficiency of the spray drying process was 39.6%. The outcomes of
this study have provided useful information on the effects of process parameters
on the efficiency of the spray drying of Tongkat Ali extract.
Keywords: Tongkat Ali extract, Spray drying, ANOVA, Optimum conditions.

1. Introduction
Tongkat Ali or Eurycoma longifolia is a popular herb in tropical countries such as
Malaysia, Indonesia, Thailand, Burma and Vietnam due to its reputation since
time immemorial as a male sexual performance aid. Tongkat Ali is a small,

31
32 N. H. Harun et al.

Nomenclatures

H/D height of liquid in the vessel to diameter vessel

Ho null hypothesis
R2 determination of coefficient
R2adj adjusted determination of coefficient
w/w weight per weight
X1 air inlet temperature
X2 feed temperature
X3 air pressure
X4 feed flow rate
Y efficiency of spray drying
evergreen-type foliage that has the capability to grow up to 15 meters tall. It is a
slow growing herbal plant, which takes no less than five years to mature. It is part of
the Simaroubaceae family and is also known as Long Jack, Pasak Bumi, Cay ba
Binh, Penawar Pahit, Bedara Pahit, Tongkat Baginda, Petala Bumi and Setunjang
Bumi [1]. Besides enhancing the testosterone level in men and acting as an energy
booster, Tongkat Ali is also traditionally used as a health tonic by decoction of the
roots or bark to cure a variety of illnesses such as diarrhea, glandular swelling,
bleeding, dropsy, persistent cough, hypertension, and relief of pain in the bones.
To date, investigations and phytochemical screening done by researchers have
shown that Tongkat Ali extracts also possess cytotoxic, antiulcer, antitumor, anti-
pyretic, antischistosomal, and antimalarial activities [1-3]. Bioactive constituents of
Tongkat Ali extracts are from the group alkaloids, quassinoids, and saponins [4,5].
These active compounds have been demonstrated to be responsible for the
pharmacological activity and therapeutics effect [6-8] of Tongkat Ali extracts. They
include quassinoids glycoside [9,10], tirucallene-type triterpenes [11], squalene
derivatives [12,13], biphenyl-neo-lignans [14], anthraquinones [15], canthin-6-one-
alkaloids [16], α,b-carboline alkaloids [16,17], and dimeric dihydrobenzofuran [18].
Currently, Tongkat Ali extract is also used as an additive in coffee or as a
replacement for ginseng in certain health products, in a variety of forms such as
capsules, tablets, tea bags, etc. [5].
In order to meet the increasing demand for this herb, the processing of this
plant needs to be efficient. However, the overall yield of Tongkat Ali extracts in
industry is currently quite low, only about 3% [19]. Tongkat Ali is usually
extracted through high pressure water extraction, where Tongkat Ali roots are
boiled as decoctions. For the finishing step, most Tongkat Ali production
facilities in Malaysia apply spray drying system in their process train as compared
to freeze drying because it is a low cost process that produces dry particles of
good quality. Powder production using spray dryers resulted in powders with
consistent particle size distribution (homogenous powder) and the morphology of
powders can also be easily controlled [20].
Spray drying is a technique of producing a dry powder from pumpable liquid or
slurry using rapid drying with a heated gas media. The physicochemical properties
of powders produced by spray drying are very much dependent on significant
process variables such as air inlet temperature, feed temperature, air pressure and
feed flow rate. Other less important parameters are ignored in this study due to the
limitations of the equipment used (e.g., air outlet temperature, atomizer type and

Journal of Engineering Science and Technology Special Issue 6 1/2015

Optimization of Process Parameters for Spray Drying of Tongkat Ali Extract 33

size, air humidity, drying air flow rate). The liquid feed was assumed to be close to
water characteristics (e.g., viscosity, solid content, surface tension, solvent volatility).
In the production of dried Tongkat Ali extract, it is crucial to optimize the spray
drying process, in order to obtain products with better powder characteristics,
greater process yield and greater efficiency [21]. However, very limited studies
have been done on the optimization of spray drying of Tongkat Ali extract so far.
This study is aimed to elucidate the optimal processing conditions of spray drying
using response surface methodology (RSM). The design of experiments was
simulated using Design Expert (version 6.0.8) software. The effects of air inlet
temperature, feed temperature, feed flow rate and air pressure on the efficiency of
the spray drying process were investigated.

2. Materials and Methods

2.1. Materials
Tongkat Ali roots were purchased from Felda Agricultural Services Sdn. Bhd.,
Malaysia. They were planted and harvested in Jengka, Pahang, Malaysia. The
plant age was approximately five years and the average growth performance of
the cultivated plants was recorded as follows: 6 cm stem diameter at 15 cm above
ground and plant height of 470 cm, which met the requirements for production of
Tongkat Ali extract. After subjected to the pre-processing activities of cleaning,
drying, grinding and sieving, Tongkat Ali roots were then stored in a cool, dark
and dry environment in order to prevent fungal growth before proceeding with the
extraction process.

2.2. Water extraction of Tongkat Ali roots

The grinded Tongkat Ali roots of size of 0.5 to 1.0 mm were extracted using
water as solvent in a batch solid-liquid vessel of 1-Liter size. Extraction process
was carried out at the temperature of 100°C, solvent to solid ratio of 10:1 (w/w),
agitation speed of 400 rpm, and duration of one hour. These operating conditions
were based on our recent works (data not shown).

2.3. Spray drying of the Tongkat Ali extract

In this study, process optimization was performed in a lab-scale spray dryer
LabPlantTM SD-06 (UK) with a chamber size of 340×205 mm as shown in Fig. 1.
The spray chamber is of the short form type with H/D ratio of 1.66 and it has a
flat shape at the bottom.
The spray dryer was equipped with two types of atomizers, but only the two-
fluid nozzle was used in this study. The flow-pattern inside the spray chamber is
co-current as shown in Fig. 1. Feed solutions containing Tongkat Ali extract
(concentration 0.67%, w/w) were heated up from 25 to 100°C (feed temperature).
Then, they were constantly stirred and fed into the spray chamber using a
peristaltic pump. The feed flow rate was controlled from 2.27 to 6.67 ml/min, and
the air pressure was varied from 7.5 to 20 psi. The air inlet temperature was
controlled between 100°C to 220°C. These temperatures were selected according

Journal of Engineering Science and Technology Special Issue 6 1/2015

34 N. H. Harun et al.

to the minimum and maximum setting that the system can accurately operate for
the given feed content.

Fig. 1. Labplanttm SD-06 spray dryer and its flow pattern.

2.4. Analytical methods

2.4.1. Total solids content
Total solids content is a measure of the amount of material remaining after water
has evaporated. Five milliliter of Tongkat Ali extract solution was placed in a dish
and kept in an oven at 100°C until the weight became constant. According to
AOAC standard [22], determination of total solids is evaluated in terms of the
weight percentage of the amount of the water loss on drying using Eq. (1).
Total Solids (%) = 100 - Moisture (%) (1)

2.4.2. Moisture content test

Moisture content of a powder is the loss in weight (%), which is an important
characteristic to be measured for powdered extract as it may contribute to the
major stickiness problem during spray drying. One gram of sample was weighed
in a pan and then placed in the Moisture Analyzer MX-50 (A&D Weighing, US).
The temperature was set at 105°C and the value was obtained only after the
reading became constant. The analyzer was designed to measure the moisture
content of the sample by its weight, thus for accuracy, the termination value was
preset at 0.1% per minute.

2.5. Experimental design

According to the experimental design of a three level four factorial Box-Behnken,
a total of 29 experimental runs were generated. The range of values for each
variable and their coded level are shown in Table 1. The generated quadratic
response surfaces permit a second order polynomial model to be fitted. By means
of this experimental design, the influence of four significant factors, namely feed
temperature, feed flow rate, air pressure, and air inlet temperature were
investigated with the efficiency of the spray drying process as the response.
Efficiency of spray drying was calculated in terms of total solids recovery, which

Journal of Engineering Science and Technology Special Issue 6 1/2015

Optimization of Process Parameters for Spray Drying of Tongkat Ali Extract 35

was determined by the mass of the powder recovered in the system over the mass
of total solids in the feed solution. Analysis of the designed experiments was built
on the basis of the ANOVA with 95% reliability.
Table 1. Spray drying factors and their coded levels in Box-Behnken design.
Factor Unit Symbol Level
-1 0 +1
Air Inlet Temperature ⁰C X1 100 160 220
Feed Temperature ⁰C X2 25 62.5 100
Air Pressure psi X3 7.5 13.75 20
Feed Flow Rate ml/min X4 2.27 4.71 7.14

3. Results and Discussion

Table 2 shows the design matrix of the Box-Behnken analysis for the spray
drying of the Tongkat Ali extract. From the experiments, the greatest efficiency of
the Tongkat Ali spray drying process (i.e., 39.6%) was found at run 15 where the
processing parameters were set at air inlet temperature of 160°C, feed temperature
of 25°C, air pressure of 20 psi and feed flow rate of 4.65 ml/min. Meanwhile, the
lowest spray drying efficiency (9.95%) was observed with run 17 where the air
inlet temperature was 100°C, feed temperature was 62.5°C, air pressure was 7.5
psi and feed flow rate was 4.65 ml/min.
Table 3 shows the F-test from ANOVA that was used to evaluate the second
order model of the efficiency of the spray drying process. The F calculated for the
efficiency of the spray drying process was 10.85 while the F tabulated was found
to be 2.52 at the degree of freedom for regression and residual of 14. Thus, the
null hypothesis (Ho) was rejected at the confidence limit of 5%. Hence, there is
ground for believing that the optimization of Tongkat Ali spray drying process
can be done based on the parameters investigated to attain the highest efficiency
of the spray drying process. The efficiency of the spray drying model was also
significant on account of the P-value being less than 0.0001.
The determination of coefficient (R2) value was equal to 0.9156 indicating that
the model was fitted and was significant to the predicted values. Furthermore, the
value of R2adj was obtained at 0.8312 reaffirming that the model was significant.
The experimental and predicted values for the efficiency of Tongkat Ali spray
drying are tabulated in Fig. 2.
A full quadratic model was developed as in Eq. (2). It explained that the
efficiency of the spray drying (Y) can be increased with the increasing of the air
inlet temperature (X1), air pressure (X3), feed flow rate (X4), feed temperature power
two (X22), interaction between air inlet temperature and feed temperature (X1X2),
interaction between air inlet temperature and feed flow rate (X1X4), interaction
between feed temperature and feed flow rate (X2X4) and interaction between air
pressure and feed flow rate (X3X4), together with the decreasing of feed temperature
(X2), air inlet temperature power two (X12), air pressure power two (X32), feed flow
rate power two (X42), interaction between air inlet temperature and air pressure
(X1X3) and interaction between feed temperature and air pressure (X2X3).
Y = 33 .12 + 3.28 X 1 − 0.25 X 2 + 3.86 X 3 + 1.10 X 4 − 6.10 X 12 + 4.41 X 22 − 4.11 X 32 − (2)
8.26 X 42 + 2.13 X 1 X 2 − 3.07 X 1 X 3 + 6.64 X 1 X 4 − 1.53 X 2 X 3 + 1.24 X 2 X 4 + 1.93 X 3 X 4

Journal of Engineering Science and Technology Special Issue 6 1/2015

36 N. H. Harun et al.

Table 2. Box-Behnken arrangement for spray drying process.

Variables code Response
X1 X2 X3 X4 Y
No. of
Air inlet Feed Air Feed flow Efficiency of
experiments
temperature temperature pressure rate spray drying
(⁰C) (⁰C) (psi) (ml/min) (%)
1 100 25 13.63 4.71 31.46
2 220 25 13.63 4.71 35.40
3 100 100 13.63 4.71 25.44
4 220 100 13.63 4.71 37.89
5 160 62.5 7.25 2.27 16.38
6 160 62.5 20 2.27 21.91
7 160 62.5 7.25 7.14 17.98
8 160 62.5 20 7.14 31.22
9 100 62.5 13.63 2.27 22.72
10 220 62.5 13.63 2.27 13.16
11 100 62.5 13.63 7.14 13.81
12 220 62.5 13.63 7.14 30.82
13 160 25 7.25 4.71 29.78
14 160 100 7.25 4.71 33.07
15 160 25 20 4.71 39.57
16 160 100 20 4.71 36.76
17 100 62.5 7.25 4.71 9.95
18 220 62.5 7.25 4.71 23.84
19 100 62.5 20 4.71 23.12
20 220 62.5 20 4.71 24.72
21 160 25 13.63 2.27 29.62
22 160 100 13.63 2.27 27.13
23 160 25 13.63 7.14 23.92
24 160 100 13.63 7.14 26.41
25 160 62.5 13.63 4.71 33.07
26 160 62.5 13.63 4.71 32.75
27 160 62.5 13.63 4.71 34.03
28 160 62.5 13.63 4.71 32.03
29 160 62.5 13.63 4.71 33.71

Table 3. ANOVA for efficiency of tongkat ali spray drying process.

Sum of Degree of Mean F-
Source Prob>F F0.05 R2
squares freedom squares value
Regression 1529.56 14 109.25 10.85 < 0.0001 2.52 0.9156
Lack of fit 138.46 10 13.85 21.97 0.0046 - -
Pure error 2.52 4 0.63 - - - -
Residual 140.98 14 10.07 - - - -
error
Cor. total 1670.54 28 - - - - -

Fig. 2. Predicted value versus actual value plot

for the efficiency of spray drying process.

Journal of Engineering Science and Technology Special Issue 6 1/2015

Optimization of Process Parameters for Spray Drying of Tongkat Ali Extract 37

3.1. Interaction effects of the process variables on the efficiency of

the spray drying process
Interactions among the process parameters, i.e., air inlet temperature, feed
temperature, feed flow rate and air pressure are summarized in Fig. 3. Powder
characteristics such as moisture content were examined in this study to
evaluate the adequacy of the spray drying operating conditions. Interaction
between air inlet temperature and air pressure was crucial for adequate
formation of the dried Tongkat Ali extract, Fig. 3(b). The correct combination
of these variables produced better droplet sizes in the chamber, and resulted in
spray-dried powder with good properties. The highest efficiency of spray
drying (34.2%) was achieved when the air inlet temperature was 170.1°C and
air pressure was 16.16 psi. Greater air pressure would certainly increase the
contact areas between air and mixture solution, thus producing smaller
droplets. As a result, water uptake from the droplet would rapidly occur and
the moisture content of powder would be low.
There were also significant effects between air inlet temperature and feed flow
rate, Fig. 3(d), and between air pressure and feed flow rate, Fig. 3(f), on the
efficiency of spray drying. In order to keep the process stable and to minimize
disturbances, interactions between these variables need to be considered in spray
drying. The highest predicted efficiency of the spray drying (33.9%) was found at
air inlet temperature of 183.3°C together with feed flow rate at 5.21 ml/min.
Meanwhile, the concurrent setting of the air pressure at 16.9 psi and feed flow
rate at 5.03 ml/min resulted in the best spray drying performance (i.e., efficiency
at 34.2%). At these states, the high feed rates with enough heat could precisely
vaporize the mixtures in a short drying time, thus allowing better efficiency of
spray drying. Therefore, controlling those parameters must be taken into account
when operating the spray drying in order to avoid problems like stickiness and
deposition on the chamber wall [23]. The powder recovery was also subjected to
feed characteristics [24].
However, there were no obvious interactions between feed temperatures
towards air inlet temperature (Fig. 3a), air pressure (Fig. 3c) and feed flow rate
(Fig. 3e). Feed temperature was found to have little effect on the efficiency of
the spray drying and varied accordingly with the input of the amount of drying
air, which reflected the energy available for evaporation in the chamber. There
was not enough heat to dry the solution when using low air inlet temperature,
and hence some water still remained in the end product which caused the
powder to easily adhere to the drying chamber and cyclone wall. As a result,
most of the desired materials were lost due to the attachments and tend to
decrease the recovery process in the cyclone [25-27]. However, a very high
temperature would melt the powder and cohesion wall, thus, causing low
powder production and its efficiency [28].

3.2. Optimal conditions for spray drying

From the results, the air inlet temperature was found to be the most important
variable in examining the effect of spray drying heat on Tongkat Ali extract. Air
inlet temperature affects powder properties such as moisture content,
hygroscopicity and morphology as it has the ability to influence initial drying rate,
rate of heat transfer to particle and efficiency of heat and mass transfer process
[28]. The optimum condition obtained for Tongkat Ali spray drying was at air

Journal of Engineering Science and Technology Special Issue 6 1/2015

38 N. H. Harun et al.

inlet temperature of 160°C, feed temperature of 25°C, air pressure of 17.91 psi
and feed flow rate of 4.86 ml/min. The efficiency of the spray drying of Tongkat
Ali extract at optimum process conditions was determined to be 39.6%. The
powder obtained has good characteristics with 5.70% moisture content. The BBD
result was validated and good agreements were obtained between the observed
and the predicted values (mean of triplicate runs). The error for the validation
experiment was only 1.9%.

Fig. 3. Response surface plots for interactions between the variables (a) feed
temperature versus air inlet temperature; (b) air pressure versus air inlet
temperature; (c) air pressure versus feed temperature; (d) feed flow rate
versus air inlet temperature; (e) feed flow rate versus feed
temperature; (f) feed flow rate versus air pressure.

Journal of Engineering Science and Technology Special Issue 6 1/2015

Optimization of Process Parameters for Spray Drying of Tongkat Ali Extract 39

4. Conclusions
The optimization of the processing parameters (air inlet temperature, feed
temperature, feed flow rate and air pressure) for spray drying of Tongkat Ali extract
was performed at laboratory scale using RSM of Box-Benhken design and
simulated using Design Expert software. The optimum condition achieved for
Tongkat Ali spray drying was at air inlet temperature of 160°C, feed temperature of
25°C, air pressure of 17.91 psi and feed flow rate of 4.86 ml/min, where the
efficiency of the spray drying was 39.6%.

Acknowledgement
The authors would like to acknowledge the financial support from Ministry of
Agricultural and Agro-based Industry, Malaysia under NKEA Research Grant
Scheme (project vote no. 4H022) and University of Technology Malaysia (UTM),
Skudai, Johor.

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