Optimization of hot air drying of olive leaves using response surface methodology

Zafer Erbay
a,
*
, Filiz Icier
b
a
Institute of Natural and Applied Sciences, Food Engineering Branch, Ege University, 35100 Izmir, Turkey
b
Department of Food Engineering, Faculty of Engineering, Ege University, 35100 Izmir, Turkey
a r t i c l e i n f o
Article history:
Received 28 August 2008
Received in revised form 5 October 2008
Accepted 8 October 2008
Available online 17 October 2008
Keywords:
Olive leaves
Drying
Optimization
Response surface methodology
Exergy
Total phenolics
Antioxidants
a b s t r a c t
Recently, the interest in olive leaves has increased due to its high phenolic content. Olive leaves have a
high potential for industrial exploitation in the food industry and drying is the main process in olive leaf
treatment. In this study, response surface methodology was used to optimize operating conditions of the
drying of olive leaves in a tray drier and desirability function used as the methodology for the optimiza-
tion. Optimization factors were air temperature (4060 C), air velocity (0.51.5 m/s) and process time
(240480 min) while investigated responses were total phenolic content (PC) and antioxidant activity
loss (AC), nal moisture content (MC), and exergetic efciency (g). The optimum conditions for drying
of olive leaves in a tray drier were determined to obtain the criteria; minimum PC and AC, and maximum
g for MC value below 6% and the optimum condition was found to be the temperature of 51.16 C with
the air velocity of 1.01 m/s for the process time of 298.68 min. At this optimum point, PC, AC, MC and g
were found as 10.25%, 41.88%, 6.0% and 65.50%, respectively.
2008 Elsevier Ltd. All rights reserved.
1. Introduction
The low incidence of cardiovascular diseases and cancer in
Mediterranean countries has drawn the attention of investigators,
and the Mediterranean diet consisting of olive and olive products
has been thought to be the reason for this. Recent studies on olive
trees have shown the richness of phenolic compounds in the olive
leaves, especially. More common phenolic compounds present in
olive leaves are oleuropein and hydroxytyrosol that have high anti-
oxidant activities (Benavente-Garcia et al., 2000; Bouaziz and
Sayadi, 2005). Oleuropein prevents cardiac disease by protecting
membrane lipid oxidation, acting on coronary dilation and through
antiarrythmic action, improves lipid metabolism, helps in obesity-
related problems, protects enzymes, prevents hypertensive cell
death in cancer patients and exhibits antiviral properties. Hydroxy-
tyrosol, the principal product of oleuropein degradation, also has
similar effects as those of oleuropein. In addition, it protects
against atherosclerosis and prevents diabetic neuropathies. The
anti HIV effect of these compounds has been investigated (Markin
et al., 2003; Micol et al., 2005; Ranalli et al., 2006; Lee-Huang et al.,
2007a,b).
Olive leaves have to be dried for the purpose of using as an
ingredient in dry mixes, for extracting phenolics having antioxi-
dant properties and for use in olive leaf tea, so drying is a critical
process in olive leaf treatment. During drying, the products quality
characteristics change in considerable ratios because of the applied
heat treatment and sometimes these changes are not desirable.
Furthermore, drying is an energy-intensive process since its energy
consumption value is 1015% of the total energy consumption in
all industries in developed countries (Mujumdar, 1997; Erbay
and Icier, in press-a). The optimization of drying would be critical
for solutions of main problems in the whole world such as the
depletion of fossil fuels and environmental pollution.
During the past few decades, thermodynamic analyses, particu-
larly exergy analyses, have appeared to be an essential tool for sys-
tem design, analyses and optimization of thermal systems. Exergy
is a measure of the potential of a stream to cause change, as a con-
sequence of not being completely stable relative to the reference
environment (Dincer and Sahin, 2004). By using exergy analysis
method, magnitudes and locations of exergy destructions (irrever-
sibilities) in the whole system can be identied, while potential for
energy efciency improvements can be introduced (Kuzgunkaya
and Hepbasli, 2007). Recently, exergy analysis has been used rather
than energy analysis for evaluating the performance of food sys-
tems (Dincer and Sahin, 2004; Akpinar et al, 2005; Colak and
Hepbasli, 2007; Corzo et al., 2008b).
Response surface methodology (RSM) is a statistical procedure
frequently used for optimization studies. It uses quantitative data
from an appropriate experimental design to determine and simul-
taneously solve multivariate problems. Equations describe the ef-
fect of test variables on responses, determine interrelationships
among test variables and represent the combined effect of all test
0260-8774/$ - see front matter 2008 Elsevier Ltd. All rights reserved.
doi:10.1016/j.jfoodeng.2008.10.004
* Corresponding author. Tel.: +90 232 3880110x3049; fax: +90 232 3427592.
E-mail address: zafererbay@yahoo.com (Z. Erbay).
Journal of Food Engineering 91 (2009) 533541
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j our nal homepage: www. el sevi er . com/ l ocat e/ j f oodeng
variables in any response. This approach enables an experimenter
to make efcient exploration of a process or system (Madamba,
2002). Therefore, RSM has been frequently used in the optimiza-
tion of food processes (Liyana-Pathirana and Shahidi, 2005; Eren
and Kaymak-Ertekin, 2007; Corzo et al., 2008a; Wani et al., 2008;
Changrue et al., 2008; Mestdagh et al., 2008; Shi et al., 2008; Altan
et al., 2008).
Olive trees cover 8 million hectares, and almost 98% of them in
the whole world are in the Mediterranean countries. But olive
leaves have not yet been exploited industrially; they have been
only used as by-product. Although scientic studies have shown
the importance of olive leaves and their drying behavior has re-
vealed (Erbay and Icier, in press-b), there has been no study inves-
tigating main effects of drying process variables on the product
quality or optimizing the drying of olive leaves ever carried out
in open literature according to the authors knowledge. The main
objective of this study was; (1) to investigate main effects of pro-
cess variables on the product quality during hot air drying of olive
leaves, (2) to determine optimum process conditions for drying of
olive leaves in a tray drier.
2. Materials and methods
2.1. Olive leaves
Olive leaves (Olea europaea L. var Memecik) were harvested
from the trees grown in Ege University campus (Izmir, Turkey).
Collected leaves were washed with tap water and then the excess
water on surfaces of leaves was removed with lter paper. Col-
lected leaves were processed within 24 h. 100 g of fresh leaves
were used in experiments.
The moisture content of fresh olive leaves was determined with
vacuum oven method (Anonymous, 1990). The protein (N 6.25)
content (Anonymous, 1995a), the oil content (Anonymous, 1987),
the crude ber content (Anonymous, 2003) and the ash content
(Anonymous, 1995b) of leaves were determined with appropriate
methods.
2.2. Drying procedure and measurements
The olive leaves were dried in a laboratory-type tray drier (Arm-
eld UOP8, Hampshire, UK) shown schematically in Fig. 1. The dry-
ing air velocity was regulated by an axial ow fan and fan speed
control unit. The air was heated with an electric 3000-W heater
placed inside the duck, and air temperature was controlled by a
heater power control unit. Drying compartment dimensions were
0.3 0.3 0.4 m. The drier included four sample trays.
The leaves were spread onto the trays in a thin layer position.
Trays were relocated in every 30 min to support uniform drying.
Anova results of preliminary experiments have allowed choose of
factors affecting response variables, and determination of their
ranges. Drying experiments were carried out at a drying air tem-
perature range of 4060 C with a drying air velocity range of
0.51.5 m/s for a process time range of 240480 min. Humidities,
temperatures and velocities were measured with robust humidity
probes (Testo, 0636.2140, Freiburg, Germany), vane/temperature
probes (Testo, 0635.9540, Freiburg, Germany), professional tele-
scopic handle for plug-in vane probes (Testo, 0430.0941, Freiburg,
Germany), respectively. Measurements of drying air temperature,
velocity and relative humidity were recorded at inlet and outlet
holes at every 10 min. An infrared thermometer (Testo 552-T2,
Freiburg, Germany) and a surface thermometer (METEX ME-32,
Seoul, South Korea) were used to measure surface temperatures
of product and drying chamber walls, respectively. A digital bal-
ance (Scaltec SBA 61, Goettingen, Germany) was used to measure
the weight loss of sample during drying experiments. The ambient
temperature and the relative humidity were also measured and re-
corded with a multi-function instrument (Testo 350-XL/454, Con-
Nomenclature
C
P
specic heat (kJ/kg C)
Ex exergy rate (kW)
ex specic exergy (kJ/kg)
F function
h specic enthalpy (kJ/kg)
m mass (kg)
P pressure (kPa)
R ideal gas constant (kJ/kg K)
R
2
regression coefcient
s specic entropy (kJ/kg K)
T temperature (C) or (K)
t time (min)
X mass fraction (dimensionless); independent variable in
Eq. (12)
U, u uncertainty
Y dependent variable (response) in Eq. (12)
z independent variable
t air velocity (m/s)
b constant regression coefcient
g exergetic efciency (%)
x humidity ratio of air (kg water/kg dry air)
relative humidity (%)
Abbreviations
AC total antioxidant activity loss (%)
Adj-R
2
adjusted regression coefcient
Adeq.Precision adequate precision
ANOVA analysis of variance
CCRD central composite rotatable design
C.V. coefcient of variation
MC moisture content of dried product (% w.b.)
PC total phenolic content loss (%)
PRESS predicted residual error sum of squares
Pre-R
2
predicted regression coefcient
RSM response surface methodology
Subscripts
rate
a air
out outlet
g gas
in inlet
p product
v vapor
w water
0 dead state
534 Z. Erbay, F. Icier / Journal of Food Engineering 91 (2009) 533541
trol unit, Freiburg, Germany). The ow diagram of the drying pro-
cess is presented in Fig. 2.
2.3. Experimental uncertainty
Uncertainty analysis is needed to prove the accuracy of the
experiments. Errors and uncertainties in the experiments can arise
from the instrument selection, condition, calibration, environment,
observation and reading, and test planning (Akpinar et al., 2003). An
uncertainty analysis was performed using the method described
by Holman (2001)
U
F

@F
@z
1
u
1

2

@F
@z
2
u
2

2

@F
@z
n
u
n

2
" #
1=2
1
2.4. Total phenolic content
Dried products obtained from all trays were mixed. Then, the
samples were taken by sampling method and used in extraction
procedure. The conventional extraction procedure was used to
extract phenolics (Bouaziz and Sayadi, 2005; Japon-Lujan et al.,
2006a, 2006b). Samples and the extractant (4:1 vol/vol, ethanol
water mixture) were placed in a beaker and left to stand 24 h
under agitation at 40 C in a shaking water bath (DKZ, Shaking
Water Bath, Beijing, China) in the dark and ltrated with the syr-
inge lters combination (Millipore, Cat.:AP2501000 and Millipore,
Cat.:HATF01300).
Total phenolic content of the samples was determined using the
modied Folin-Ciocalteu procedure described by Singleton and
Rossi (1965). A diluted sample extract (1.0 mL) or a series of gallic
acid (Sigma, G7384-100G) standards (0, 40, 80, 120, 160, 200 and
240 ppm) were mixed with 1.0 mL of the Folin-Ciocalteu reagent
(Carla Erba Reagenti, UN 3264) and 25 mL deionized water. The
mixture was held at room temperature in the dark for 5 min before
adding 10 mL of 7.5% sodium carbonate (w/v). Then, mixture was
completed to 100 mL with deionized water and held at room tem-
perature in the dark for 1 h before measuring the absorbance at
755 nm with spectrophotometer (Cary 50, UVvisible spectropho-
tometer, Palo Alto, CA, USA). Three replicates were measured and
the average was recorded and total phenolic content loss (PC) val-
ues according to raw olive leaves were calculated.
2.5. Total antioxidant activity
Total antioxidant activity of the samples was determined by
using improved ABTS radical cation decolorization assay (Re
et al., 1999; Karakaya and Ylmaz, 2007). Stock solution of ABTS
+
Fig. 1. The schematic illustration of the tray drier used in the study.
Tray
Fig. 2. The ow diagram of the drying process and measurements.
Z. Erbay, F. Icier / Journal of Food Engineering 91 (2009) 533541 535
radical cation was prepared by mixing 7 mM ABTS [2,2
0
-azinobis-
(3-ethylbenzothiazoline-6-sulphonic acid) Diammonium salt]
(Fluka, Sigma-Aldrich, EC No. 25003966, Steinheim, Germany)
and 2.45 mM potassium persulfate (Merck, UN 1492). Absorbance
readings were taken at 734 nm and at 30 C exactly 1 min after ini-
tial mixing and up to 6 min. Following the absorbance readings,
percentage inhibition of oxidation was calculated for each sample.
Five replicates were measured and the average was recorded and
total antioxidant activity loss (AC) values according to raw olive
leaves were calculated.
2.6. Exergetic efciency
The exergetic efciency of the dryer (g) can be dened as the ra-
tio of the product exergy to exergy inow for the chamber. Thus,
the general form of exergy efciency is written as (Akpinar, 2004)
g
_
Ex
out
_
Ex
in
100 2
In order to write the mass, energy and exergy balance equations for
the dryer shown in Fig. 3, three components such as product, air and
water were considered (Dincer and Sahin, 2004). Exergy equations
used in the present study are as follows (Dincer and Sahin, 2004):
_
Ex
in
_ m
a
ex
1
_ m
p
ex
p

2
_ m
w

2
ex
w

2
3
_
Ex
out
m
a
ex
3
_ m
p
ex
p

4
_ m
w

4
ex
w

4
4
_
Ex _ m:ex 5
ex
1
Cp
a
x
1
Cp
v
T
1
T
0

T
0
Cp
a
x
1
Cp
v
ln
T
1
T
0

R
a
x
1
R
v
ln
P
1
P
0

T
0
R
a
x
1
R
v
ln
11; 6078x
0
11; 6078x
1

1; 6078x
1
R
a
ln
x
1
x
0

6
ex
3
Cp
a
x
3
Cp
v
T
3
T
0

T
0
Cp
a
x
3
Cp
v
ln
T
3
T
0

R
a
x
3
R
v
ln
P
3
P
0

T
0
R
a
x
3
R
v
ln
11; 6078x
0
11; 6078x
3

1; 6078x
3
R
a
ln
x
3
x
0

7
ex
p
h
p
T; P h
p
T
0
; P
0
T
0
s
p
T; P s
p
T
0
; P
0
8
ex
w
h
f
T h
g
T
0
t
f
P P
g
T T
0
s
f
T s
g
T
0

T
0
R
v
ln
P
g
T
0

x
0
v
P
0

9
h
1
h
a

1
x
1
h
v

1
h
a

1
x
1
h
g

1
10
h
3
h
a

3
x
3
h
g

3
11
x
0; 622/P
g
P /P
g

12
s
p
s
0

C
P;p
C
P;0
2

ln
T
p
T
0

13
The reference-dead state condition was determined as T
0
= 32 C,
P
0
= 101.325 kPa and
0
= 55%.
In this study, the specic heat for olive leaves was determined
using the relations proposed by Choi and Okos (1986) with the spe-
cic heat of pure components given as Singh (1992)
C
P

X
C
P;i
X
i
14
X
i

m
i
m
total
15
The composition of olive leaves was used in the calculations of spe-
cic heat of the olive leaves (Table 1).
2.7. Experimental design, statistical analysis and optimization
RSM was used to investigate the main effects of process vari-
ables on the moisture content (MC), total phenolic content loss
(PC), total antioxidant activity loss (AC) and the exergetic efciency
(g) during the drying of olive leaves. Drying temperature (x
1
), dry-
ing air velocity (x
2
) and process time (x
3
) were selected as indepen-
dent variables. Process variable ranges were determined by means
of preliminary experiments (Erbay, 2008).
A Central Composite Rotatable Design (CCRD) including 20
experiments formed by 6 central points and 6 (k = 1.68179) axial
points to 2
3
full factorial design was used (Table 2).
Experimental data were tted to a second order polynomial
model and regression coefcients obtained. The generalized sec-
ond order polynomial model used in the response surface analysis
was as follows:
Y b
0

X
3
i1
b
i
X
i

X
3
i1
b
ii
X
2
i

X X
3
i<j1
b
ii
X
i
X
j
16
Mathematical models were evaluated for each response by means
of multiple regression analysis. The modeling was started with a
quadratic model including linear, squared and interaction terms.
Signicant terms in the model for each response were found by
analysis of variance (ANOVA) and signicance was judged by the
F-statistic calculated from the data (Eren and Kaymak-Ertekin,
2007).
Model adequacies were checked by R
2
, adj-R
2
, pre-R
2
, Adeq.Pre-
cision, PRESS and C.V. (lack of t > 0.1; R
2
> 0.95; (Adj-R
2
Pre-
R
2
) < 0.2; max.PRESS; C.V. < 10; Pre-R
2
> 0.7; Adeq.Precision > 4)
(Myers and Montgomery, 2002). After model tting, residual anal-
yses including the examination of diagnostic plots and calculation
of case statistics were conducted to validate assumptions used in
Fig. 3. Input and output terms for exergy analysis of drying (Dincer and Sahin,
2004).
Table 1
The composition of olive leaves.
Component Amount (g/100 g)
Protein 5.45 0.22
Oil 6.54 0.27
Carbohydrate 27.58 0.24
Crude ber 7.00 0.18
Ash 3.61 0.25
Water 49.83 0.51
536 Z. Erbay, F. Icier / Journal of Food Engineering 91 (2009) 533541
ANOVA. Design Expert Ver. 7.0.0 (Stat-Ease, 2005) was used to t
response surfaces and optimize the drying process.
During optimization of industrial processes, several response
variables describing the quality characteristics and performs mea-
sures of the systems are usually to be optimized. Some of these
variables are to be maximized while some are to be minimized.
In many cases, these responses are competing, i.e., improving one
response may have an opposite effect on another one, which fur-
ther complicates the situation. Several approaches have been used
to handle this problem. One approach uses a constrained optimiza-
tion procedure, the second is to superimpose the contour diagrams
of the different response variables, and the third approach is to
solve the problem of multiple responses through the use of a desir-
ability function combining all responses into one measurement
(Eren and Kaymak-Ertekin, 2007).
Specic steps of desirability functions for optimization in-
cluded: (1) to make response variables dimensionless, (2) to decide
weighting coefcient, (3) to constitute desirability function and
solution (weighted linear method; multiplication and division
method; shortest distance ideal point method) and (4) to make
optimization by fuzzy similar precedable ratio method (Shi et al.,
2008).
In the present study, desirability function were developed for
the criteria that minimum PC and AC, and maximum g, and not
more than MC value of 6.0%.
3. Results and discussion
Results of different runs of drying experiments were shown in
Table 2. The detailed uncertainty analysis was performed for
experimental measurements of parameters and total uncertainties
of predicted values. Results of uncertainty analysis were listed in
Table 3. It was obtained that all uncertainties were in an acceptable
range.
Multiple linear regression analysis of the experimental data
yielded second order polynomial models for predicting PC, AC,
MC and g same as assumed at the beginning of the study. ANOVA
was conducted to determine signicant effects of process variables
Table 2
Experimental values of response variables for central composite rotatable design.
Run # T (C) t (m/s) t (min) PC (%) AC (%) MC (%) g (%)
1 44 (1) 0.7 (1) 289 (1) 33.11 41.88 24.53 67.04
2 56 (+1) 0.7 (1) 289 (1) 8.21 42.99 4.49 59.27
3 44 (1) 1.3 (+1) 289 (1) 28.84 42.36 15.16 73.05
4 56 (+1) 1.3 (+1) 289 (1) 9.08 43.50 6.45 62.93
5 44 (1) 0.7 (1) 431 (+1) 37.25 43.78 19.35 70.72
6 56 (+1) 0.7 (1) 431 (+1) 28.77 52.95 3.83 60.36
7 44 (1) 1.3 (+1) 431 (+1) 28.90 43.97 9.02 75.26
8 56 (+1) 1.3 (+1) 431 (+1) 22.22 53.97 3.66 64.60
9 40
(1.68)
1.0 (0) 360 (0) 34.26 45.03 25.59 73.20
10 60 (+1.68) 1.0 (0) 360 (0) 11.08 53.45 4.88 56.09
11 50 (0) 0.5
(1.68)
360 (0) 35.45 44.29 11.73 63.89
12 50 (0) 1.5 (+1.68) 360 (0) 27.96 45.65 3.52 74.92
13 50 (0) 1.0 (0) 240
(1.68)
8.13 39.03 11.93 64.28
14 50 (0) 1.0 (0) 480 (+1.68) 24.27 49.32 3.77 70.84
15 50 (0) 1.0 (0) 360 (0) 13.16 44.56 6.25 66.75
16 50 (0) 1.0 (0) 360 (0) 15.62 43.68 4.20 68.02
17 50 (0) 1.0 (0) 360 (0) 15.88 44.44 3.76 69.61
18 50 (0) 1.0 (0) 360 (0) 20.66 43.23 4.21 66.74
19 50 (0) 1.0 (0) 360 (0) 16.54 45.04 4.60 66.38
20 50 (0) 1.0 (0) 360 (0) 15.78 44.36 4.70 64.03
Table 3
Uncertainties of the experimental measurements and total uncertainties for predicted
values.
Parameter Unit Comment
Experimental measurements
Uncertainty in the temperature measurement C 0.224
Uncertainty in the weight measurement g 0.00051
Uncertainty in the air velocity measurement m/s 0.21
Uncertainty in the measurement of relative humidity
of air
% 0.41
Uncertainty in the measurement of moisture content g 0.0016
Uncertainty in the surface temperature measurement C 1.0
Predicted values
Total uncertainty for MC Dimensionless 0.09%
a
Total uncertainty for PC Dimensionless 2.09%
b
Total uncertainty for AC Dimensionless 2.42%
c
Total uncertainty for g Dimensionless 6.54%
d
a
Nominal value was taken as 6.0.
b
Nominal value was taken as 15.88.
c
Nominal value was taken as 44.44.
d
Nominal value was taken as 70.05.
Table 4
ANOVA evaluation of linear, quadratic and interaction terms for each response variable and coefcient of prediction models.
Source DF PC DF AC DF MC DF g
Coefcient Sum of
squares
p-value Coefcient Sum of
squares
p-value Coefcient Sum of
squares
p-value Coefcient Sum of
squares
p-value
Model 7 16.32 1722.93 <0.0001 5 44.24 294.72 <0.0001 8 4.61 945.41 <0.0001 4 67.11 480.01 <0.0001
x
1
1 7.23 714.78 <0.0001 1 2.60 92.72 <0.0001 1 6.18 522.49 <0.0001 1 4.95 335.48 <0.0001
x
2
1 2.25 69.92 0.0006 1 0.33 1.48 0.0424 1 2.31 73.53 <0.0001 1 2.69 100.04 <0.0001
x
3
1 4.76 309.65 <0.0001 1 3.02 124.55 <0.0001 1 2.09 59.45 <0.0001 1 1.44 28.32 0.0016
x
1
x
2
1 2.66 57.79 <0.0001
x
1
x
3
1 3.69 108.80 <0.0001 1 2.11 35.82 <0.0001 1 0.98 7.72 0.0042
x
2
x
3
1 1.43 16.56 0.0440
x
2
1
1 2.35 80.79 0.0003 1 1.65 40.15 <0.0001 1 3.80 208.04 <0.0001 1 16.17 0.0111
x
2
2
1 5.55 451.75 <0.0001 1 1.11 17.81 0.0002
x
2
3
1 1.19 20.31 0.0001
Residual 12 39.25 14 4.16 11 6.56 15 28.94
Lack of t 7 9.38 0.9619 9 2.02 0.8120 6 2.79 0.7146 10 16.76 0.7131
Pure error 5 29.87 5 2.14 5 3.77 5 12.18
Total 19 1762.18 19 298.88 19 951.96 19 508.95
R
2
0.9777 0.9861 0.9931 0.9431
Adj-R
2
0.9647 0.9811 0.9881 0.9280
Pre-R
2
0.9528 0.9734 0.9787 0.9097
Adq.precision 24.952 49.599 43.780 27.880
PRESS 83.25 7.94 20.30 45.95
C.V. 8.31 1.20 8.79 2.07
Z. Erbay, F. Icier / Journal of Food Engineering 91 (2009) 533541 537
on each response and to t second order polynomial models to
experimental data.
Regression equation coefcients of the proposed models and
statistical signicance of all main effects calculated for each re-
sponse were obtained and effects being not signicant (p > 0.05)
were stepped down from models without damaging the model
hierarchy (Table 4). ANOVA also showed that the lack of t was
not signicant for all response surface models at 95% condence le-
vel. On the other hand, R
2
, Adj-R
2
, Pre-R
2
, PRESS, Adeq.Precision and
coefcient of variation (C.V.) were calculated to check the model
adequacy as lack of t > 0.1; R
2
> 0.94; (Adj-R
2
Pre-R
2
) < 0.2; max.-
PRESS; C.V. < 10; Pre-R
2
> 0.7; Adeq.Precision > 4 (Table 4).
To visualize the combined effects of two factors on any re-
sponse, the response surface and contour plots were generated
for each of tted models as the function of two independent vari-
ables, while keeping the other variable at the central value. Three
different response surface plots (Figs. 46) were illustrated by
maintaining one of factors constant for each gure. These gures
were typical examples plotted for center points of constant factor.
Effects of variables on responses were discussed by evaluation of
these plots.
3.1. Total phenolic content loss (PC)
High temperature and moderate velocity grades (0.851.25 m/s)
in a short process time minimized PC. Phenolics are heat sensitive
compounds (Podsedek, 2007). On the other hand Oleuropein which
is the most abundant compound in olive leaves could hydrolyze to
hydroxytyrosol in moderate heat treatment (Benavente-Garcia
et al., 2000). However, a long term effect of temperature should
cause a complete damage of the phenolics. Not only is the degree
of heat intense, but also heat treatment time important. Similarly,
the interaction effect of temperature and time was obtained as sig-
nicant for PC (p < 0.01) (Table 4 and Fig. 5).
On the other hand, enzymatic reactions or free moisture content
can affect the phenolics (Nicoli et al., 1999). For the stability of
phenolic compounds, free moisture in olive leaves should be de-
creased to prescribed levels. In this study, total moisture content
was able to decrease below 6% while the process time was short
at high temperatures. Optimization was necessary to obtain en-
ough process time to decrease the moisture content at moderate
temperatures by the purpose of minimizing PC.
3.2. Total antioxidant activity loss (AC)
According to the heat intense and type of the product, some-
times the antioxidant capacity can decrease (esp. foods that have
high ascorbic acid content) or sometimes antioxidant properties
of naturally occurring antioxidants can be improved (Dewanto
et al., 2002). This seems to be related to the presence of polyphe-
nols and their antioxidant properties may change as a consequence
of their oxidation state (Nicoli et al., 1999). Similarly, it was ob-
tained that the intense of heat was important and the moderate
temperature was desirable to increase the retention of the antiox-
Fig. 4. Response surface and contour plots for total phenolic content loss (PC) (a), antioxidant activity loss (AC) (b), nal moisture content (MC) (c) and exergetic efciency (g)
(d), at constant drying time (360 min).
538 Z. Erbay, F. Icier / Journal of Food Engineering 91 (2009) 533541
idant capacity of olive leaves during drying (Fig. 4). The interaction
effect of temperature and time was also signicant for AC
(p < 0.01). The temperature of 4855 C with low drying air veloc-
ity in a short process time should be done to minimize AC.
3.3. Final moisture content (MC)
Generally, high temperature, high air velocity and long process
time is needed for low MC. However, extreme rates of heat transfer
may cause case hardening in the drying of biological products like
olive leaves (Erbay and Icier, in press-b). If food is dried with high
heat transfer rates at the beginning of the second falling rate period
of drying, the entrance of the partially empty capillaries may
shrink rapidly and may prevent the removal of the remaining at
deeper locations, and that is called case hardening (zilgen and
zdemir 2001). In this study, the increase in temperature signi-
cantly decreased MC while the lowest MC was able to obtain by
moderate air velocities (1.01.25 m/s) (Figs. 4 and 6). Furthermore,
interaction effects of temperaturevelocity and temperaturetime
were signicant for MC (p < 0.01) (Table 4).
3.4. Exergetic efciency (g)
Exergy efciency was calculated in the range of 56.0975.26%
for drying of olive leaves in the tray drier used. Low temperature,
high air velocity and long process time was needed to increase g.
In this study, higher temperature affected heat losses signicantly
due to the insufcient isolation and the airproof in the tray drier
used. The effect of air velocity on heat losses and irreversibilities
was lower than the effect of temperature. The increase in air veloc-
ity caused the increase in g. In the beginning of the process, the in-
crease in heat losses and irreversibilities was proportionally higher
(Akpinar et al., 2005). Low temperature drying was needed for high
g. Furthermore, the process time has to be increased to obtain suf-
ciently dried product at low temperatures. Similar results have
been reported by several researchers (Dincer and Sahin, 2004; Akp-
inar, 2004; Akpinar et al, 2005; Colak and Hepbasli, 2007; Corzo
et al., 2008b).
3.5. Optimization
Optimum conditions for drying of olive leaves in a tray drier
were determined to obtain the criteria; minimum PC and AC, and
maximumg for MC value below 6%. Second order polynomial mod-
els obtained in this study were utilized for each response in order
to determine the specied optimum drying condition. These
regression models were valid only in the selected experimental do-
main. Thus, the operating region was determined considering some
economical, industrial and product quality related constraints.
In this study, the optimization was applied for selected ranges
of temperature, velocity and process time as 4060 C, 0.51.5 m/s,
and 240480 min, respectively. By applying desirability function
method, six solutions were obtained for the optimum covering
criteria with desirability value of 0.626 (Table 5). All were close
to each other such as temperatures, velocities and process times
varied between 50.9751.16 C, 1.001.01 m/s and 298.68
302.44 min, respectively. At this circumstance, the solution which
had the lowest PC and AC values to get the highest product quality
and the lowest process time to decrease the process costs was
selected. The solutions were obtained for the optimum drying
Fig. 5. Response surface and contour plots for total phenolic content loss (PC) (a), antioxidant activity loss (AC) (b), nal moisture content (MC) (c) and exergetic efciency (g)
(d), at constant drying air velocity (1.0 m/s).
Z. Erbay, F. Icier / Journal of Food Engineering 91 (2009) 533541 539
condition covering the criteria as 51.16 C for temperature, 1.01 m/
s for air velocity, 298.68 min for process time. At this point, PC, AC,
MC, and g were calculated as 10.25%, 41.88%, 6.0% and 65.50%,
respectively.
4. Conclusions
In this study, drying, which is the main process in olive leaf
treatment, was optimized. Optimization responses were the mois-
ture content of dried leaves, which is the main indicator showing
the success of the drying process, and important quality properties
of olive leaves; the total phenolic content and antioxidant activity,
and the exergetic efciency being the most powerful tool for anal-
ysis, design and optimization of thermal systems.
By using second order polynomial models tted in this study,
the moisture, total phenolic content and antioxidant activity loss
and the exergetic efciency of the dryer during drying of olive
leaves in the tray drier can be predicted. RSM and the conventional
graphic and desirability functions methods have been effective in
determining the optimum zone within the experimental region.
Optimal conditions for minimum total phenolic content and
antioxidant activity loss and maximum exergetic efciency at a -
nal moisture content below 6% in drying of olive leaves in a tray
drier corresponded to temperature of 51.16 C, air velocity of
1.01 m/s, process time of 298.68 min in order to obtain PC of
10.25%, AC of 41.88%, MC of 6.0% and g of 65.50%.
Although scientic studies have shown the importance of olive
leaves, olive leaves have not yet been exploited industrially. This
study should assist the widespread use of olive leaves.
Acknowledgements
This study is a part of the MSc thesis named as The investiga-
tion of modeling, optimization, and exergetic analysis of drying of
olive leaves, and is supported by Ege University Scientic Research
Project No. of 2007/MH/30.
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