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Article history: Peppermint is one of the most important aromatic plants because it has wide range of industrial uses and
Received 3 December 2009 is widely accepted by the public for its flavoring and pharmaceutical properties. Hot air or natural drying
Received in revised form 29 May 2010 of medicinal and aromatic plants, including peppermint, is a common postharvest operation. Drying the
Accepted 4 June 2010
product reduces biochemical and microbiological degradation. However, many studies in the literature
report the results of drying only a small amount of plant material (less than 1 kg) and do not consider the
performances of industrial scale dryers in terms of their effect on product quality, energy consumption
Keywords:
and throughput. A rotary drum dryer was used to dry 15 kg of fresh chopped peppermint plant. The rotary
Peppermint
Rotary drum dryer drum dryer was programmed to operate under two different drying schemes: constant air temperature
Drying kinetics drying and rectangular wave-shaped drying air temperature profiles. The drying durations were 15–18 h
Essential oil and 12–15 h for constant temperature profile and rectangular wave-shaped temperature profiles, respec-
Color change tively. Hot air drying caused considerable darkening of the dried peppermint leaves. Essential oil contents
Aromatic plants of peppermint samples dried by the two different drying procedures were relatively unaffected by dry-
ing scheme (2.08–2.7 mL 100 g dry matter−1 ). The menthol content of the leaves increased from 32.52%
(fresh) up to 44.52% (dried), their menthone content decreased from 24.85% (fresh) down to 9.07% (dried).
However, the variations within replications were relatively high in terms of the menthol (25.39–44.52%)
and menthone (9.07–18.49%) contents of the dried leaves. These variations might have been caused by
the uncontrolled morphological and physiological changes of the fresh peppermint materials associated
with their maturity. These variations are the main obstacle to obtaining reproducible results and there-
fore dried peppermint products with consistent quality. The specific energy consumption values ranged
from 7.88 to 15.08 MJ (kg water removed)−1 . Daily fluctuations in ambient air conditions directly affected
the specific energy consumption of rotary drum dryer.
© 2010 Elsevier B.V. All rights reserved.
0926-6690/$ – see front matter © 2010 Elsevier B.V. All rights reserved.
doi:10.1016/j.indcrop.2010.06.003
S. Tarhan et al. / Industrial Crops and Products 32 (2010) 420–427 421
A rotary drum dryer was designed and built specifically for this
research study (Fig. 1). The main components of the rotary drum
dryer are an electrical heating/fan unit, a rotary drum horizontally
placed on four rubber wheels, a control panel, and an air chan-
nel/distribution room unit. This rotary drum dryer has a cylindrical
drum, 95 cm in outer diameter and 130 cm in length. The drum was
constructed of a 1-mm thick perforated chrome–nickel sheet with
2-mm diameter holes (112 holes per 10 cm2 ). Four 30-cm wide
baffles (inner wings) were attached lengthwise inside this drum
evenly distributed around the drum to mix the drying materials
uniformly (Fig. 2). The drum was placed on four rubber wheels
and its bottom faced to the air distribution room. One of the rub- Fig. 2. Inner wings of drum and pipe for temperature/RH sensor.
422 S. Tarhan et al. / Industrial Crops and Products 32 (2010) 420–427
was taken with sufficient material to separate the sample into so layer drying assumes homogonous drying. Therefore, the pepper-
that two 30-g samples of leaves and two 30-g samples of stems mint drying in the rotary drum dryer was assumed to be equivalent
which were used to determine moisture contents. When the dried to thin layer drying because of mixing. Page’s equation is the most
sample moisture content reached approximately 9–11% wb, the convenient mathematical model of thin layer drying kinetics and
moisture content recommended for safe storage, the drying pro- has been widely used in thin layer drying studies (Muller, 2007):
cess was stopped. After the leaves became too fragile to handle,
two extra 30-g samples of leaves were taken and microwaved until MR = exp(−k · t n ) (5)
their weight did not decrease more than 0.3 g every minute. The where k and n are model parameters whose values are estimated
method of using a microwave to determine moisture content was from the experimental data. The calibration of model parameters
termed “rapid moisture determination” and was used to complete and the estimation of model variance were both performed using
the drying trials. Rapid moisture determination gave as approxi- SigmaPlot® software.
mate results but were not intended to replicate the exact results.
The exact results were obtained by oven drying and reweighing the
2.5. Color analysis
sample after being in the oven for 24 h at 105 ◦ C.
The total electrical energy consumption for the drying process
The colors of both fresh and dehydrated peppermint plants were
was measured using a Network analyzer (Entes MPR63, Turkey).
quantified by using a Minolta (CR-400) chromameter (Japan). Five
The dry bulb temperature and relative humidity of ambient air,
color measurements were taken for each treatment, resulting in
heated air, the air passing through the center of the drum and
numeric values for three chromatic scales (L*, a*, b*). L* is the bright-
the outgoing air were measured by sensors (HOBO S-THB-M008,
ness ranging from no reflection for black (L* = 0) to perfect diffuse
ONSET, USA) every 2.5 min and stored in the data logger (HOBO
reflection for white (L* = 100). The value “a*” is the redness ranging
H21-002, ONSET, USA).
from negative values for green to positive values for red. The value
“b*” is the yellowness ranging from negative values for blue and
2.4. Data processing and mathematical modeling positive values for yellow. The color at the grid origin (a* = 0 and
b* = 0) is achromatic (gray) (McGuire, 1992). A special white plate
Soysal and Oztekin (2001) reported both the specific heat was used to calibrate the chromameter.
energy consumption and the specific electrical energy consump-
tion, because they used an LPG burner to heat air for their dryer. In
2.6. Essential oil isolation
this study, both types of energy consumptions were combined and
renamed the specific energy consumption. Furthermore, the spe-
Essential oil was isolated using a Clevenger hydro-distillation
cific energy consumption was calculated by making two separate
apparatus. Ten grams of dried leaves were soaked in 100 mL
assumptions. The first approach assumed the air temperature did
distilled water (1:10). Distillation required approximately 4 h to
not rise in the drying air after heating. It was calculated as follows:
complete when heated to the boiling point of water using hot plates.
TEC The oil phase was separated and dried over anhydrous sodium sul-
SEC1 = 3.6 · (1)
MWR fate then stored in a dark glass bottle at 4 ◦ C for analysis (Telci et
where SEC1 is the specific energy consumption without considering al., 2006). Samples were prepared from both fresh and dried leaves
temperature rise (MJ kg water−1 ); TEC: total energy consumption for two replications of the two temperature profiles.
(kWh); MWR: mass of water removed from the drying material
(kg). 2.7. GC-FID analysis
The second approach considered the temperature rise in the
heated air, calculated as follows: GC analysis of the essential oil was performed by Perkin-Elmer®
Clarus 500 model Autosystem GC with built-in autosampler. Oil
TEC
SEC2 = 3.6 · (2) was diluted in acetone (1:10) and injected into the BPX5 col-
MWR · (Tha − Taa ) umn (30 m × 0.25 mm × 0.25 m film) for separation. The carrier
where SEC2 is the specific energy consumption to produce tem- gas was helium at 5 psi inlet pressure. Injector and detector (FID)
perature rise in drying air (MJ kg water−1 ◦ C−1 ); Tha , the average temperatures were 230 ◦ C and 250 ◦ C, respectively. The column
temperature of heated air (◦ C); Taa , the average temperature of temperate was programmed from 60 to 230 ◦ C at 3 ◦ C/min with
ambient air (◦ C). initial and final temperature held for 3 min and 15 min, respec-
The second approach eliminates the impact of the ambient air tively. Diluted samples of 1.0 L were injected in the split/splitless
temperature differences when the drying trials were conducted. (5:1 split) mode. Quantitative data were obtained electroni-
The drying kinetics relate the moisture ratio to the drying time: cally from FID area percent data without the use of correction
factors.
M − Me
MR = (3)
M0 − Me
2.8. GC–MS analysis
where M is the moisture content of drying material at any sampling
time (% db); Me the equilibrium moisture content of drying material GC/MS analyses were obtained on Perkin-Elmer® mass spec-
based on drying conditions (% db); M0 is the initial moisture content trometer with built-in autosampler using a BPX5 column
of drying material (% db). (30 m × 0.25 mm × 0.25 m film). For GC/MS detection, an electron
The values of the equilibrium moisture content, Me , are rela- ionization system (ionization energy of 70 eV) was used. Helium
tively small compared to M and M0 . Thus, the moisture ratio can be was the carrier gas at a flow rate of 1.3 mL/min. The oven temper-
calculated as follows (Akpinar Kavak, 2006): ature programming was the same with GC-FID analysis. Injector
and MS transfer line temperatures were set at 230 ◦ C and 250 ◦ C,
M
MR = (4) respectively. Diluted samples (1/10 in acetone, v/v) of 1.0 L were
M0
injected in the split/splitless (5:1 split) mode. Compounds were
Many empirical equations are given in the literature to describe named based on comparison of their retention times with those
thin layer drying kinetics of agricultural and food materials. Thin of a standard, and by comparison of their mass spectral library and
S. Tarhan et al. / Industrial Crops and Products 32 (2010) 420–427 423
Fig. 3. Air temperature values recorded during the first replication of drying at
Fig. 5. Air temperature values recorded during the second replication of drying at
constant air temperature profile.
constant drying temperature profile.
Fig. 4. Air relative humidity values recorded during the first replication of drying at Fig. 8. Air relative humidity values recorded during the first replication of drying at
constant air temperature profile. rectangular wave-shaped air temperature profile.
424 S. Tarhan et al. / Industrial Crops and Products 32 (2010) 420–427
Table 1
The moisture content (% wb) of fresh and dried peppermint leaves and stems# .
Constant
R1 76.41a 78.84b 14.391 58.163
R2 81.17c 84.66d 12.141 30.852
Rectangular wave-shaped
R1 79.84b,c 86.75e 10.511 48.323
R2 81.12c 84.85d 10.861 33.082
#
Mean moisture contents of fresh materials with different superscripts (a, b, c and
d) are statistically different at ˛ = 0.05. Mean moisture contents of dried materials
with different superscripts (1, 2 and 3) are statistically different at ˛ = 0.05.
Fig. 10. Air relative humidity values recorded during the second replication of dry- Fig. 11. The drying curves of peppermint leaves under different drying air temper-
ing at rectangular wave-shaped air temperature profile. ature profiles (error bar of each sampling point equals to ± its standard deviation).
S. Tarhan et al. / Industrial Crops and Products 32 (2010) 420–427 425
tive approach (using a fixed drying time), the samples might not
reach the desired moisture content (9–11% wb) which affects the
dried products’ quality. Doymaz (2006) dried mint leaves in 10 h at
35 ◦ C and less than 5 h at 45 ◦ C. These drying times are shorter than
the ones obtained in this current study. Drying leaves and stems
together may slow down the moisture loss from leaves since heat
is also used for stems. Therefore, industrial drying of plant materi-
als needs rapid and reliable moisture content tests to be developed
because variations in plant materials and drying systems require
different drying times.
Page’s equation was able to represent the experimental data
from peppermint leaves very well as shown in Table 2. The model
parameters for the drying stems were not included since they have
no economic value. The model parameter values changed with the
replications and temperature profiles. The average values of each
Fig. 12. The drying curves of peppermint stems under different drying air temper- parameter are also given in Table 2 for the general description of
ature profiles (error bar of each sampling point equals to ± its standard deviation). the drying kinetics of peppermint plants in the rotary drum dryer.
Model goodness of fit values (R2 , RMSE and MBE) confirmed that
thicker stems than the second-cut ones since the density of pep- there were no biases or inaccuracy in predictions since the values
permint plants per m2 increased between the first cutting and the of R2 were very close to 1 (perfect fit) while the values of RMSE and
second due to self-propagation on the ground, decreasing the size of MBE were very close to zero (no deviation). Therefore, Page’s equa-
each plant. The increase of plant density possibly reduced the sun- tion was determined to be an easy-to-use model for representing
light and nutrients per plant and limited the growth of leaves and the drying of peppermint leaves.
stems. These morphological changes altered the drying characteris- The specific energy consumption values without and with
tics. The mass of the leaves and stems was not measured however. considering a temperature rise in the heated air are given in
Only second-cut peppermint samples were used for the first and Table 3. The specific energy consumption values without con-
second replications of drying at rectangular wave-shaped air tem- sidering a temperature rise in the heated air varied within
perature profile. The two replications have much closer drying replications more than between temperature profiles. These
curves compared to the two replications for the constant temper- deviations (8.78–11.77 MJ kg water−1 ) for constant temperature
ature treatment. These results indicate that the growing practices and (7.88–15.08 MJ kg water−1 ) for rectangular wave-shaped tem-
must be reported in addition to the drying kinetics of any medicinal perature profile within replications were mostly caused by
and aromatic plant studies. In addition, the parameters of drying differences associated with different ambient air conditions dur-
kinetics are only valid for the leaf fraction of the plant and may ing the drying trials. Considering the temperature rise in the
not be adequate to design dryers for whole plants. The completion heated air reversed the order of the specific energy consump-
of drying using the constant temperature profile required 18 and tion (0.86–0.72 MJ kg water−1 ◦ C−1 ) within the replications for the
15 h for the first and second replications, respectively while the constant temperature drying treatment while it reduced the dif-
completion of a drying process at rectangular wave-shaped tem- ference (0.47–0.72 MJ kg water−1 ◦ C−1 ) within the replications of
perature required 12 and 15 h for the first and second replications, drying with the rectangular wave-shaped temperature profile. The
respectively. The cyclical drying temperature in the wave-shape reason for that difference (0.47–0.72 MJ kg water−1 ◦ C−1 ) is likely
temperature treatment accelerated drying. Another experimental due to the higher relative humidities (59.6–73.5%) of ambient air in
approach to assess the effect of any temperature profile would be the second replication than those (36.6–51.6%) in the first repli-
to use a fixed drying time such as 15 h and to analyze the final cation. The variation in relative humidity values of ambient air
moisture contents of the material at the final time. In this alterna- must also be considered to truly compare the performances of
Table 2
Parameter values and model goodness of Page’s equation for peppermint leaves.
k n R2 RMSE MBE
Constant
Rep I 0.066 1.265 0.991 0.0284 0.005
Rep II 0.236 1.080 0.998 0.0140 −0.006
Average 0.151 1.173
Rectangular wave-shaped
Rep I 1.156 1.521 0.997 0.0209 −0.014
Rep II 0.095 1.405 0.995 0.0274 0.003
Average 0.626 1.463
Table 3
Specific energy consumption valuesa .
Drying air temperature profile SEC1 (MJ kg−1 water) SEC2 (MJ kg−1 water ◦ C−1 )
Table 4
Measured color values of fresh and dry peppermint leaves# .
L* a* b*
R1 R2 R1 R2 R1 R2
the dryers which use hot air to remove moisture. The average Microwave drying of these plants preserved their original colors
rise of adiabatic drying potential after heating can be used as an (Alibas, 2007; Arslan and Ozcan, 2008; Therdthai and Zhou, 2009).
alternative approach instead of the temperature rise in the heated These results also show the importance of the drying time since
air. The increase of drying air temperature in a cyclical fashion microwave drying normally take minutes instead of hours. On the
seems to slightly decrease the specific energy consumptions even other hand, microwave drying caused considerable essential oil
though more energy is needed to raise the temperature higher. losses (Jaganmohan et al., 1998) possibly because rapid changes
However, shortening the drying time by using higher temperatures to high temperatures modified the structure of leaves (Therdthai
reduced specific energy consumption. In a similar study, Martinov and Zhou, 2009). The color change of peppermint leaves by hot air
et al. found that specific energy consumption per kg of dry sage drying seems to be the main challenge which future drying research
increased from 13 MJ kg dry sage−1 at a drying temperature of 30 ◦ C projects should confront. The duration of high temperature drying
to 42 MJ kg dry sage−1 at 40 ◦ C (Martinov et al., 2007). However, and/or the value of high temperature can be increased to shorten
SEC decreased to ∼22 MJ kg dry sage−1 at a drying temperature the drying time. Drying whole plants and intermittent mixing may
of 50 ◦ C since drying time was reduced. The specific energy con- reduce color change by minimizing mechanical damage.
sumption of a batch dryer for peppermint drying ranged from 9.1 The essential oil content and the percentage of two major essen-
to 14 MJ kg water−1 even though the drying air was reused when tial oil components (menthol and menthone) of dried leaves are
its relative humidity was lower than a set value (Martinov et al., shown in Table 5. The essential oil content of fresh peppermint
2006). The specific energy consumption decreased from 14.0 to ranged from 2.71 to 3.03 mL 100 g dry matter−1 depending on the
9.7 MJ kg water−1 when the pile height of fresh material in the dryer age of the peppermint plants. The menthol percentage of fresh
increased from 40 cm to 60 cm. However, increasing pile height peppermint ranged from 31.02 to 34.02% (average value: 32.52%)
caused heterogeneous drying process and increased essential oil while the menthone percentage of fresh peppermint ranged from
losses at the lower levels of the pile since they were overdried 23.23 to 26.47% (average value: 24.85%). It has been previously
(below 9%). Inverting the pile was recommended when the mois- reported that related structures such as menthol, neomenthol and
ture content of the material at the bottom of pile fell down to methyl acetate showed increased levels from early to late bloom,
25–30%. whereas the ketone levels (menthone and isomenthone) decreased
The color values (a*, b* and L*) of fresh and dried peppermint from early to full bloom (Rohloff et al., 2005). Drying caused a
plants are given in Table 4. The brightness values (L*) of fresh slight reduction in the essential oil content of peppermint but no
leaves ranged from 34.86 to 39.67 while the greenness/redness val- major trend change in essential oil was found with respect to the
ues (a*) ranged −6.48 to −11.27. The yellowness/blueness values drying air temperature profiles. The variations in essential oil con-
of fresh peppermint leaves were more stable between replica- tent were possibly caused by the variations associated with the
tions. The drying process caused considerable changes in color. The age of fresh peppermint plants at harvest. The increase of drying
brightness values fell to 23.67 while the greenness/redness (a*) temperature above 50 ◦ C in the rectangular wave-shaped temper-
values rose to 0.82. The yellowness/blueness values fell to 11.10. ature profile did not cause a significant reduction in essential oil
These results show that drying with hot air caused darkening in content. However Rohloff et al. (2005) reported that the essential
the color. However, both drying air temperature profiles caused oil content of peppermint decreased from 2.54–2.64 mL 100 g dry
almost the same darkening in extent. Therefore, relatively long dry- matter−1 to 1.34–1.70 mL 100 g dry matter−1 when the tempera-
ing times are believed to be the main factor in color changes to ture of drying air increased from 30 to 50 ◦ C. The previous and
the leaves, together with mechanical damages caused by chopping current results show that using cyclic temperature profiles such
and mixing. Previous studies also reported that hot air drying of as the rectangular wave-shaped profile seems effective to preserve
aromatic and medicinal plants did not conserve original color val- essential oil content. Variations of menthol and menthone concen-
ues and caused considerable darkening (Alibas, 2007; Arslan and trations in the replications were higher than the variations seen
Ozcan, 2008; Martinov et al., 2007; Therdthai and Zhou, 2009). in the temperature profiles. Again, the variations associated with
Table 5
Amount and major components of dried peppermint essential oil‡ .
Sample status Essential oil content (mL 100 g dry matter−1 ) Menthol (%) Mentone (%)
R1 R2 R1 R2 R1 R2