Drying 2004 Proceedings of the 14th International Drying Symposium (IDS 2004)

So Paulo, Brazil, 22-25 August 2004, vol. A, pp. 597-604

OPTIMIZATION OF SPRAY DRYING OF ROSELLE EXTRACT (HIBISCUS

SABDARIFFA L.)

Isaac Andrade and Hctor Flores

Instituto Tecnolgico Agropecuario de Jalisco, Km. 10 Carr. San Miguel Cuyutlan,
Tlajomulco de Z., Jalico, Mxico CP 45640, E-Mail: isaacag2001@yahoo.com.mx
Keywords: response surface method, spray drying, roselle extract, roselle
ABSTRACT
The objectives of this research were to select the range of operational parameters for
spray drying of a roselle extract in such a way to minimize the changes in color, pH and
powder yield and develop a mathematical model that determines optimum operating
parameters. The experimental data were obtained in Minispray Dryer with a capacity of
0.11.0 kg/h. An experimental design 33 was developed where the factors were; feed
rate, inlet drying air temperature and pressure compressed air of nozzle with the levels;
(5%, 10%, 15%), (180C, 190C, 200C) and (5 bar, 6 bar, 7 bar) respectively. The
color of the powder product was measured by spectrophotometer. To find out optimum
operating parameters, we used the Response Surface Method of a second order model
with criteria based on acceptable moisture reduction and quality. Comparison between
the experimental and simulated results showed that the mathematical model could
predict fairly well. The optimal parameters claimed for the model of optimization to dry
the extract roselle with the best characteristic in color, pH and powder yield were: 5%
feed rate, 190C inlet air temperature and 7 bar pressure of the atomizing air.
INTRODUCTION
The roselle is a non traditional cultivation that has taken importance for the variety of nutritious and
due to the medicinal properties that are attributed. The calyces contain large amount of pectin,
anthocyanin, ascorbic acid and malate (Chen et al., 1998), and can be used for making jellies, jams,
preserves, sauces, and beverages (Esselen and Sammy, 1975). Roselle extract, having a brilliant red color
is a good source of natural food colorants, because the color in roselle is unstable (Chen et al., 1998). An
alternative of use of the roselle and stable color is to obtain the natural color from the calyce (Main et al.,
1978). The spray drying is one of the most frequently used operation for the removal of water from a fluid
feed. Spray drying is, by definition, the transformation of feed from a fluid state into a dry particulate by
spraying the feed in a hot drying medium (Nogueira et al., 2000). The resulting dried product may be

597

presented in different forms such as powders, granules or agglomerates, depending upon the physical and
chemical properties of the feed and dryer design and operation. Each foodstuff has powder requirements
to be met during manufacture (Masters, 1991). The advantages of spray drying as a continuous and
economic process allowing the production of good quality powders is established (Prez and Faras,
1995). However, few works of drying of the roselle extract exist, mainly to obtain the coloring. One of
this works is the Al-Kahtani and Hassan (1990) studied the existence of the changes of quality among the
roselle extract and the powder obtained by spray drying, settling down that the appropriate temperature of
drying for the roselle extract was of 198.5C, without carrying out a method of optimization.
The increased consumer awareness of food quality has emphasized the need to optimize the drying
process (Banga and Sing, 1994). The response surface methodology (RSM) is a useful technique for the
investigation of complex processes. It has been successfully applied to optimize food process operations.
It consists of a group of mathematical and statistical procedures that can be used to study relationship
between one or more responses (dependent variables) and a number of factors (independent variables).
This methodology generates a mathematical model that describes the overall process (Montgomery,
2001). The factorial design associated with the RSM gives secure information of the process reducing the
empirical solution that involves try and error techniques (Box et al., 1978). Using this technique to make
the tests, it is possible to estimate the principal effects of the variables in the desirable response or other
dependent variable. The variance table gives information on how good is the fit, then it is possible to
propound a probabilistic model that can correlate the response to the studied variables, constructing the
surface response to determine the optimal range of operation (Nogueira et al., 2000).
The objective of this study was to establish the good conditions of drying, through RSM, by means of the
combined effects of the spray drying parameters such as temperature, feed flow and atomizer pressure,
expressed in such a way to minimize the change in color, pH, product moisture content and powder yield,
obtained from roselle extract.
MATERIAL AND METHODS
Materials
The roselle calyces were harvest in Tepic, Nayarit a denominated variety Diamond. The calyces were
washed and sterilized by means of a constant flow of hot water at 80C during 30 min.. The roselle
extract was obtained by means of watery maceration until the content of soluble solids didn't increase.
The maceration consisted on placing a relationship of roselle-water 8:1 during a time of rest of 128 min to
ambient temperature. After that time the solid phase was separated from the liquid phase, by filtration,
which was concentrated in a pilot vacuum evaporator BUCHI until 12Brix. The concentrated extracts
were filled into a clean glass bottle and stored in a freezer at 5C to prevent deterioration.
Spray drier
The drying tests were performed in a Minispray Dryer BUCHI, model B-191with a capacity of 0.11.0
kg/h level laboratory, that is a parallel flow drier with a 1 mm hole nozzle atomizer feed by a peristaltic
pump. Drying conditions follow the experimental design.
Experimental design
The experimental design is a factorial 33, where the factors were the inlet air temperature, the feed flow
and the pressure of compressed air of the nozzle atomizer, at the levels (180C, 190C, 200C), (5%,

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10%, 15%) and (5 bar, 6 bar and 7 bar) for each factor respectively, as showed in Table 1. This
experimental design had 2 repetitions.
Table 1. Experimental design matrix for complete factorial for 3 variables.

Test
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27

X1
-1
0
+1
-1
0
+1
-1
0
+1
-1
0
+1
-1
0
+1
-1
0
+1
-1
0
+1
-1
0
+1
-1
0
+1

Number of tests = 3n = 3x3x3 = 27

X2
-1
-1
-1
0
0
0
+1
+1
+1
-1
-1
-1
0
0
0
+1
+1
+1
-1
-1
-1
0
0
0
+1
+1
+1

X2
-1
-1
-1
-1
-1
-1
0
0
0
0
0
0
0
0
0
0
0
0
+1
+1
+1
+1
+1
+1
+1
+1
+1

Ta (C)
180
190
200
180
190
200
180
190
200
180
190
200
180
190
200
180
190
200
180
190
200
180
190
200
180
190
200

Feed flow (%) Pressure (bar)

5
5
5
5
5
5
10
5
10
5
10
5
15
5
15
5
15
5
5
6
5
6
5
6
10
6
10
6
10
6
15
6
15
6
15
6
5
7
5
7
5
7
10
7
10
7
10
7
15
7
15
7
15
7

Table 2 presents the levels of the variables (codifies and real) used in the tests considering the
experimental design.
Table 2. Codes and real variables of the experimental design.

Variable
Ta
% FF
P (bar)

code
X1
X2
X3

-1
180
5
5

0
190
10
6

+1
200
15
7

This methodology allows the modeling of second order term and the interaction terms as
the equation 1:

599

y = o +

k
i =1

i xi +

ij x i2 +

i
V

1
1

ij x i x j +

(1)

The ratio y is the measured response variable, and the optimization it was analyzed by multiple
regression employment the response surface methodology (RSM). The RSM analysis was made through
pure error method to fit the equation 1 in the statistical program STATISTICA EDITION '98. The
parameters of the mathematical model were estimated and used to predict the curve generated by the
model and the variance analyses table (ANOVA).
Analysis
We use a phmeter Orion, for determination the pH of the rehydrated powder. The color settled down by
means of the absorbance relationship measured to 520 nm with the intensity of the red color, using a
spectrophotometer Espectronic 21. For the determination of the moisture content of the powder used the
method of the AOAC of constant weight in exposition to temperatures of 105C in a drying scale.
RESULTS AND DISCUSSION
Table 3 shows the experimental results of pH, A520, moisture content in the product and powder yield (y),
obtained in the spray drying tests.
Table 3. Real values of inlet temperature, feed flow, air pressure in the final time, moisture content in the product, color
absorbance, yield and pH in the powder.

600

Test

Ta (C)

FF (%)

P (bar)

tf (min)

Y
(mg/ml)

0
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27

180
190
200
180
190
200
180
190
200
180
190
200
180
190
200
180
190
200
180
190
200
180
190
200
180
190
200

5
5
5
10
10
10
15
15
15
5
5
5
10
10
10
15
15
15
5
5
5
10
10
10
15
15
15

5
5
5
5
5
5
5
5
5
6
6
6
6
6
6
6
6
6
7
7
7
7
7
7
7
7
7

176
160
153
79
77
78
55
54
56
164
154
155
76
79
77
55
58
56
95
138
143
71
61
53
53
52
52

11.89
11.64
12.98
14.57
13.89
12.15
12.8
11.77
13.68
11.99
12.23
11.22
13.24
13.54
12.2
13.95
11.94
11.87
12.04
12.45
14.38
12.64
11.44
11.59
12.92
12.81
12.28

H
(g Color
water/g dry (A520)
matter)
0.825
4.92
1.26
4.39
1.29
8.5
1.26
7
1.46
7
1.54
6
1.52
7.96
1.56
8.95
1.7
5.88
1.6
4.9
1.56
4.47
1.38
5.94
1.95
6
1.72
6
1.56
5.39
1.4
5.91
1.56
4.95
1.58
6.4
1.26
5.41
1.6
3.98
1.74
5.44
1.35
6.4
1.42
4.85
1.54
5.41
1.58
5.5
1.62
6
1.6
5.94
1.48

pH
2.86
2.87
2.89
2.86
2.91
2.91
2.92
2.93
2.93
2.92
2.91
2.95
2.91
2.97
2.94
2.51
2.92
2.92
2.92
2.49
2.43
2.42
2.46
2.47
2.46
2.47
2.48
2.48

The Statistica software (1998), version 5.1, was used to analyze the experimental data. In the first run, the
analysis was made considering all terms of the mathematical model (equation 1). The quadratic term,
linear term and the cross product terms between temperature, feed flow and pressure of atomizer were
considered statistically not significant within 95% of confidence. This analysis conducted using the pure
error option to estimate the experimental error. After, trying to obtain a better model, the analysis was
made considering only the significant terms of model. The ANOVA is shown in Table 4.
Table 4.- ANOVA for the complete codified model.

Factor
(1)Ta_C (L)
Ta_C (Q)
(2)FF__%(L)
FF__%(Q)
(3)P (L)
P (Q)
1L by 2L
1L by 2Q
1Q by 2L
1Q by 2Q
1L by 3L
1L by 3Q
1Q by 3L
1Q by 3Q
2L by 3L
2L by 3Q
2Q by 3L
2Q by 3Q
Error
Total SS

r2=0.759, p < 0.05

SS
5.14089
.52184
.21122
2.01070
2.11600
.61252
1.68750
2.68960
.18778
.75334
.10083
1.76890
.02890
.56623
.56333
.39271
4.00000
.68481
5.51019
21.99083

DF
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
8
26

MS
5.140890
.521840
.211218
2.010704
2.116000
.612517
1.687500
2.689600
.187778
.753337
.100833
1.768900
.028900
.566226
.563333
.392711
4.000000
.684815
.688773

F
7.463836
.757638
.306658
2.919254
3.072129
.889287
2.450008
3.904914
.272626
1.093738
.146396
2.568190
.041959
.822079
.817879
.570160
5.807427
.994253

p
.025766*
.409426
.594873
.125906
.117739
.373273
.156156
.083553
.615721
.326212
.711969
.147700
.842814
.391064
.392220
.471838
.042517*
.347905

The results of Table 4 shows that the calculated of the probability value (p) is greater than 0.05, the factor
have secondary effect statistically significant on the response of the yield.. Consequently the model is
statistically significant only the factor of temperature and the quadratic product between the flow and
feeding pressure to the spray drying in lab scale.
In the Figures 1 and 2 can be observed the behavior of second order equation for the optimization of the
yield according to the relationship among each one of the independent variables. This behavior is called
point seat where you could present a minimum point and a maximum point. Therefore, the critical points
to reach a bigger yield of powder roselle settle down in 9.94% of feeding flow, 193.1C of inlet
temperature and 6.3 bar of pressure of the atomizer. The optimization of the moisture content presents a
behavior of a minimum point with the following values of optimization 10% of feeding flow, 190C of
inlet temperature and 6 bar of pressure of the atomizer (Figure 3). These conditions are ideal to obtain a
powder roselle with the smallest content of the moisture content, giving the opportunity to a long period
of storage. The intel temperature obtained in the two cases were near to the one reported of 198.5C by
Al-Kahtani and Hassan (1990).

601

Variable: Powder Yield

R2 = 0.75

11.096
11.434
11.773
12.111
12.449
12.788
13.126
13.465
13.803
14.141
above

Variable: Intense color A520

R2 = 0.75

1.188
1.243
1.298
1.353
1.408
1.463
1.518
1.573
1.628
1.683
above

Figure 1.- Response surface showing the temperature and percentage feed flow with constant pressure 6 bar in powder roselle
yield and 5 bar in intense color.

602

Variable: Powder Yield

Variable: Intense color A520

R2 = 0.75

R2 = 0.75

16

16

14

14

12

10

4
178

182

186

190

194

198

202

1.188
1.243
1.298
1.353
1.408
1.463
1.518
1.573
1.628
1.683
above

%F__Flow

11.096
11.434
11.773
12.111
12.449
12.788
13.126
13.465
13.803
14.141
above

%F__Feed

12

10

4
178

182

186

Ta_C

190

194

198

202

Ta_C

Figure 2. Contour plot showing the temperature and percentage feed flow in powder yield.

Observing the contour plot, the optimal range of process is:

178 Ta 190
9.5 % FF 15
5 < P (bar) < 6
CONCLUSIONS
To obtain a roselle powder with the best yield characteristics, color and moisture content for their
conservation, the spray drying should be managed according to the following operation range:
temperature 178-190C, flow of feeding 9.5-15% and pressure of the atomizer 5-6 bar. This characteristic
solves the problem of stickiness in the drying chamber. The good operation characteristics were obtained
by means of the method of response surface (RSM). You can also conclude that variation doesn't exist in
the pH in the reconstituted powder, but however, there are not flavor in the reconstituted powder. Further
work is needed to continue studying the spray drying in roselle and to determine that original constituents
are getting lost during the process.
ACKNOWLEDGMENT
We are very grateful to the CoSNET, DGETA, ITAJ, and to those who collaborated in this invetigation.
NOTATION
FF
H
SS
DF
MS
F
p
P
Ta
X1
X2
X3

feed flow of roselle extract

product moisture contens
sum of squares
degree of freedom
mean of squares
statistical distribution
statistical probability
pressure of atomizer
air temperature
variable code of temperature
variable code of % feed flow
variable code of pressure of atomizer

%
g water/g dry matter
variance component
variance component
variance component
variance component
variance component
bar
C

603

r2
Y
y

regression coefficient
Powder yield
Response variable

Greek Symbols
0 , i, i,j

regression coefficient of the model

mg/ml

LITERATURE
Al-Kahtani, A. A. and Hassan, B. H. (1990), Spray drying of roselle (hibiscus sabdariffa) extract, J. of
Food Science, Vol. 55, pp. 1073-1076.
Banga, J. R. and Singh, R. P. (1994), Optimization of air drying of foods, J. Food Engineering, Vol. 3, pp.
189-211.
Box, G.E.P., Hunter, W.G., Hunter, J.S. (1978), Statistics for experimenters - an introduction to design,
data analysis and model building, John Wiley & Sons, N.Y.
Esselen, W. B.; Sammy, G. M. (1975), Applications for roselle as a red color food colorant, Food Prod.
Dev., 9(8), pp. 37-40.
Main, J. H., Clydesdale, F. M., and Francis, F. J. (1978), Spray drying anthocyanin concentrates for use as
food colorants, J. Food Sci., Vol. 43, pp. 1693-1701.
Master, S. P. (1991), Spray Dryer, Hand Book, 3a edition, Loongman scientific and Technology. pp.8182
Montgomery, D. C. (2001), Design and analysis of experiments, John Wiley & Sons, Inc., 5th Edition, pp.
427-500.
Prez-Correa, J. R. and Faras, F. (1995), Modelling and control of a spray dryer: a simulation study,
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intybus L.) obtained by spray drying, Proceedings of the 12th International Drying Symposium
IDS2000, Paper No.143.
Chen S.H., Huang T., Ho C., and Tsai P., (1998), Extraction, analysis and study on the volatiles in roselle
tea, J. Agric. Food Chem., 46, pp. 1101-1105.

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