Journal of Food Processing and Preservation ISSN 1745-4549

EXTRACTION OF CURCUMIN AND ESSENTIAL OIL FROM

CURCUMA LONGA L. BY SUBCRITICAL WATER VIA RESPONSE
SURFACE METHODOLOGY
POUYA MOTTAHEDIN, ALI HAGHIGHI ASL1 and MARYAM KHAJENOORI
Extraction Research Group, Faculty of Chemical, Gas and Petroleum Engineering, Semnan University, Semnan 35195-363, Iran

1
Corresponding author. ABSTRACT
TEL: 198 23 33654120;
FAX: 198 23 33654120; In this study, subcritical water extraction (SWE) was applied to extract the essen-
EMAIL: ahaghighi@semnan.ac.ir tial oil (especially curcumin) from Curcuma longa L. (turmeric) rhizome.
Response surface methodology was used to evaluate the extraction conditions.
Received for Publication August 1, 2015
Experiments were carried out using a three-factor Box–Behnken design under fol-
Accepted for Publication April 30, 2016
lowing conditions: temperature (90, 120 and 150C), water flow rate (1, 2.5 and
doi:10.1111/jfpp.13095 4 mL/min) and mean particle size (0.5, 1 and 1.5 mm). This is the first time that
effects of mentioned variables were considered on SWE of curcumin. The opti-
mum conditions were temperature of 150C, water flow rate of 1 mL/min and
mean particle size of 0.5 mm. The maximum curcumin extraction yield was
90.1947 6 0.26%, which was in a good agreement with the predicted value of
92.0097%. The extracts were analyzed by gas chromatography and gas
chromatography-mass spectrometry. Also, results of SWE were compared with
conventional methods.

PRACTICAL APPLICATIONS
Curcumin is an important pharmacological agent that can be extracted from tur-
meric rhizome. In recent years, subcritical water has been used as a solvent for
extraction of flavors, fragrances and antioxidant components from plant materi-
als. Subcritical water is a good solvent for curcumin as well as other organic com-
pounds but is safer than the organic solvents. Subcritical water extraction of
curcumin from turmeric rhizome is an alternative method for increasing the qual-
ity of the extract.

INTRODUCTION Extensive investigations over the last two decades have

In recent years, the extraction and purification of natural
pharmaceuticals from medical plants is noteworthy due to
less side effects on human body. One of the most important
medical plants is turmeric rhizome (scientific name of Cur-
cuma longa L.). It was used in traditional medicine, but in
recent years the interest for this rhizome increased due to its
potential use as a food colorant. The yellow characteristic of
turmeric is due to the presence 3–5% of curcuminoids
(Ching et al. 2014). The curcuminoids include curcumin,
demethoxycurcumin and bisdemethoxycurcumin. Among
them, curcumin is the major pharmacological agent and has
the best inhibitory effects for various cancers by arresting
the activation and propagation of carcinogen (Basnet and
Skalko-Basnet 2011).
indicated that curcumin produces different effects such as
reduction of blood cholesterol, prevention of low-density
lipoprotein oxidation, inhibition of platelet aggregation and
suppression of thrombosis and myocardial infarction (MI).
It suppresses symptoms associated with type II diabetes,
rheumatoid arthritis, multiple sclerosis (MS) and Alzhei-
mer’s disease. Moreover, it inhibits human immunodefi-
ciency virus (HIV) replication, enhances wound healing,
protects from liver injury, increases bile secretion, protects
from cataract formation and protects from pulmonary tox-
icity and fibrosis. It is an antileishmaniasis and an antiather-
osclerotic (Ravindran et al. 2007). Curcumin has
antioxidant and free radical scavenging activities (Borra
et al. 2013; Asouri et al. 2013). Curcumin can bind with
heavy metals such as cadmium and lead, thereby reducing

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SWE OF CURCUMIN AND ESSENTIAL OIL VIA RSM
the toxicity of these heavy metals. This property of curcu-
min explains its brain protection features (Akram et al.
2010). Also curcumin has anti-inflammatory and anti-
cancer properties (Alexandrow et al. 2012; Darvesh et al.
2012; Killian et al. 2012; Huang et al. 2013; Jiang et al. 2013;
Zlotogorski et al. 2013). Curcumin’s anti-inflammatory
effects have been revealed to be similar to the powerful drugs
hydrocortisone and phenylbutazone. Despite of the men-
tioned drugs, curcumin has no toxic effects such as declined
white blood cell count, ulcer creation and intestinal bleeding
(Aggarwal et al. 2007). In addition, curcumin is used to
color butter, cheese and other foods (Goel et al. 2008).
The conventional methods such as Soxhlet and liquid–
liquid extraction have been applied for the extraction of cur-
cumin (Braga et al. 2003). The organic solvents such as ace-
tone, methanol, ethanol, and isopropanol were
recommended as suitable solvents which selectively extract
the coloring agent. The use of organic solvents needs long
time and causes toxicity, problems of residual content in the
final product. These methods have a few adjustable parame-
ters for controlling the selectivity of the process. In the last
literatures turmeric extraction using ultrasound-assisted
method and supercritical carbon dioxide (SC-CO2) with
different co-solvents were performed too (Braga et al. 2003;
Chang et al. 2006; Rouhani et al. 2009; Sawant and God-
ghate 2013).
Nowadays subcritical water technology at temperatures
between 100 and 374C and pressure high enough to main-
tain the liquid state has been suggested as a green and
powerful alternative method to extract new pharmaceuticals
from plants. Water as a solvent has good advantages such as
being nonflammable, nontoxic, inexpensive, environmen-
tally friendly and available in high purity. Also the subcriti-
cal water extraction (SWE) is prospering due to the unique
properties of subcritical water. With increasing temperature,
the dielectric constant, surface tension and viscosity of sub-
critical water are dramatically decreased. It leads to high
selective extraction of different classes of compounds, with
more polar organic compounds at lower temperatures to
less polar organic compounds at higher temperatures
(Smith 2006). Many researchers have utilized this method
for isolation of biologically active compounds from natural
sources (Khajenoori et al. 2009; Eikani et al. 2013; Wang and
Lu 2014).
The objective of this research is SWE of essence (especially
curcumin) from turmeric rhizome without any organic co-
solvent. Curcumin is poor soluble in water at room temper-
ature. The use of subcritical water enhanced its solubility. In
previous works the influence of only temperature (Osorio-
Tobon and Meireles 2013) and temperature, pH and buffer
concentration on the pressurized liquid extraction of curcu-
min were investigated (Euterpio et al. 2011). This is the first
report considering simultaneous effect of various parame-
2 of 9 Journal of Food Processing and Preservation 2017; 41: e13095; V
P. MOTTAHEDIN, A. HAGHIGHI ASL and M. KHAJENOORI
ters (temperature, mean particle size and flow rate) on SWE
of the essence from turmeric rhizome. The present study
tries to show the optimization of the above mentioned vari-
ables through experimental design, using response surface
methodology (RSM). RSM has been shown to be a powerful
tool for determining the effects of the probable extraction
factors. The results obtained from SWE of turmeric rhizome
were compared by two conventional techniques including
hydrodistillation and Soxhlet extraction. Identification and
analyze of the extracts were carried out using GC/GC-MS.
MATERIALS AND METHODS
Materials
The fresh turmeric rhizomes of Indian origin were pur-
chased from a local market (Shahmizad, Semnan, Iran) in
March 2014. Curcumin analytical grade (Aldrich Chemical
Co., Milwaukee, WI) was used as a standard component.
NaCl, Na2SO4 and n-pentene (Merck, Darmstadt, Ger-
many) were used as demulsifier, drying agent and extract-
ant, respectively, in liquid–liquid extraction of aqueous
extracts. HPLC grade, de-gassed water purified through a
Milli-Q de-ionizing unit (Millipore, Bedford, MA) was used
as extractant. N-hexane (Merck, Germany) was applied as
maintaining solvent for essence before analyses.
Sample Preparation
Turmeric rhizomes were dried in shadow at room tempera-
ture for 2 days. They stored in polyethylene bags at 220C
until used. Immediately, they were cut into small pieces and
ground to fine powder before experiments. The powder was
prepared using suitable standard sieves. The moisture con-
tent of seeds was 5% (dry basis).
Subcritical Water Extraction: Apparatus and
Procedure
SWEs were carried out in a dynamic flow type laboratory-
built apparatus (Semnan University, Semnan, Iran) shown
in Fig. 1. One HPLC pump (SY-8100 series, BFRL Co., Ger-
many) was used to transfer water through the system with
various flow rates. A burette is equipped in the inlet of pipe-
lines for checking the flow rate of the pump. A coil made
from 3-m stainless steel tubing was used for preheating the
water. The extractor consisted of a stainless steel cylindrical
chamber (120 3 12 mm id, 13.6 mL effective internal vol-
ume). Preheating coil and the extraction cell were placed in
an oven. The oven controlled the temperature (up to 250 6
1C) with PID controller. The outlet stream of extractor was
cooled by a double pipe heat exchanger (tube side:
C 2016 Wiley Periodicals, Inc.
P. MOTTAHEDIN, A. HAGHIGHI ASL and M. KHAJENOORI
FIG. 1. SCHEMATIC DIAGRAM OF SWE SYSTEM, B-1: BURETTE, C-1:
NITROGEN CYLINDER, EC: EXTRACTION CELL, PC: PREHEATING COIL,
OV-1: OVEN, P-1: HPLC PUMP, P-2: WASHING PUMP, T1: WATER
TANK, T2: SOLVENT TANK, T3: RINSING SOLVENT TANK, HX-1: HEAT
EXCHANGER, WI: WATER INLET, WO: WATER OUTLET, BP: BACK
PRESSURE REGULATOR
30.48 mm i.d. 3 45.72 mm o.d., cooling surface area:
75 cm2) to about 15C. A back pressure regulator (Go Com-
pany, Pmax 5 35 bar) was used to control the pressure of the
system.
HPLC grade water, as the only solvent, was put into ultra-
sonic cleaner apparatus for 20 min at 60C. Then, water was
filled into a 5-L Pyrex feed tank and was purged for 1 h with
N2 to remove dissolved O2 . In all experiments, the extractor
was filled with 1.0 g of ground turmeric rhizomes. Two
pulpy and cloth-filters sandwiched between two stainless
steel filter were inserted in both sides of the chamber to pre-
vent from particles flow.
It is well known that the effect of pressure on the SWE
process is negligible (Ong et al. 2006; Teo et al. 2010). There-
fore, for all SWEs, the pressure was selected to be 2 MPa to
maintain the water as a liquid at the extraction tempera-
tures. While terminal valve and back-pressure regulator
were closed, the HPLC pump was started to reach to the
required pressure. Then, the pump was turned off, the by-
pass valve was closed and the oven was brought up to the
required temperature. After reaching the corresponding
subcritical water conditions, the HPLC pump was turned on
with a desirable flow rate. At that time, water was delivered
to preheating coil, the extraction cell, heat exchanger, back
pressure regulator, respectively. Samples were collected after
back pressure regulator. Regarding the selected flow rate and
void volume between the extractor and collection vessel
(40 mL), about the first 20 mL of collected sample was dis-
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SWE OF CURCUMIN AND ESSENTIAL OIL VIA RSM
carded. By GC analysis, it was observed that this amount of
the extracts was clean and no peak was detected. At the end
of each run, the obtained extract was used for liquid–liquid
extraction and pre-concentration before GC/GC-MS analy-
sis. The extraction time for determining the best operation
conditions was selected to be 100 min. The experiments
were performed twice. The reported results are the average
of the two experiments.
Sample Preparation for GC/GC-MS
At the end of extraction time, a liquid–liquid extraction step
using n-pentene was carried out. The volumetric ratio of n-
pentene to the extract was 1:2 in all experiments. Extractions
were completed by two equal volumes of solvent in two
steps. NaCl was added to obtain 25% saturated solution and
facilitate the breaking of the emulsion. After liquid–liquid
extraction, all samples were centrifuged in two steps: first 15
min at 700 g, and then 5 min at 1,792 g. Samples were
installed at room temperature to evaporate n-pentene and
only essential oil remained in the little beakers. The essential
oil was dissolved in 1 mL hexane before GC/GC-MS
analysis.
Hydrodistillation
Extraction was carried out by Clevenger-type apparatus
(Ashk-e shisheh Co., Iran) in accordance with the descrip-
tion of the British Pharmacopoeia for 3 h (British Pharma-
copoeia 1999). Hundred gram of powdered rhizome were
mixed with 1,000 mL of distilled water into the 2,000 mL
balloon. About 1.8 mL oil, present at the upper layer in the
tube, was separated from the water. The essential oil was
stored in a dark glass bottle at 4C before the examination of
the presence of curcumin.
Soxhlet Extraction
Soxhlet extraction was carried out using standard apparatus
(Ashk-e shisheh Co., Iran). Fifteen gram of powdered rhi-
zomes with 250 mL n-hexane as solvent were used (Furnis
et al. 1989). The extraction time was 10 h. The organic
extract was concentrated using a rotary evaporator (Rotova-
por R-210, Water bath B-491, Buchi, Switzerland) and
stored at 4C before analysis.
Curcumin Quantification Analysis
The GC-flame ionization detection analysis was performed
using a gas chromatograph (ACME 6100, 6000 series)
equipped with a TRB-WAX capillary column (60 m 3
0.25 mm i.d.) with 0.5 lm film of poly ethylene glycol. The
carrier gas was helium (99.999%, Roham Gas Co., Tehran,
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SWE OF CURCUMIN AND ESSENTIAL OIL VIA RSM P. MOTTAHEDIN, A. HAGHIGHI ASL and M. KHAJENOORI

TABLE 1. FACTORS, RANGES AND LEVELS OF INDEPENDENT

VARIABLES IN RSM DESIGN
Levels

Description 21 0 1
Temperature (C) 90 120 150
Subcritical water flow rate (mL/min) 1 2.5 4
Mean particle size (mm) 0.5 1 1.5

where X1, X2, . . ., Xk are the independent variables. b0 , bi

FIG. 2. CALIBRATION CURVE FOR CURCUMIN
Iran) at a flow rate of 1 mL/min (constant flow). The col-
umn was heated at 50C for 5 min, programmed at 5 mL/
min to 220C and held at 220C for 5 min. Both temperatures
of the injector and detector were 240C. 2 lL of each sample
was injected using splitless mode. Software supplied by
Chrompack was used to handle the data.
GC-MS analysis was carried out using a Hewlett-Packard
5973 with a HP-5MS column (30 m 3 0.25 mm, film thick-
ness 0.25). Temperature was programmed from 60C (3 min)
to 240C at 6C/min and kept constant at 240C for 5 min. The
flow rate of Helium, as carrier gas, was 1 mL/min. MS were
at 70 eV. The mass spectra and fragmentation patterns were
compared with the published mass spectra or Wiley and
NIST libraries (Adams 1995). GC was calibrated by solu-
tions of 500, 250, 125 and 50 ppm from a curcumin stock
solution in n-hexane. The calibration curve was fitted using
a linear regression line with 0.99 (Fig. 2).
and bii (i 5 1, 2, . . ., k; j 5 1, 2, . . ., k) are the regression
coefficients for intercept, linear, quadratic and interaction
terms, respectively; k is the number of variables.
A response surface design based on the Box–Behnken (B-
B) method (Zivorad 1995) was used to evaluate the effects
of extraction temperature (T), subcritical water flow rate
(Q) and mean particle size (dp) on the yield of extraction.
This design provides three levels for each factor. Box–
Behnken design is popular in industrial research because it
is an economical design that requires only three levels for
each factor (Khuri and Mukhopadhyay 2010). The inde-
pendent variables used in the RSM design and their respec-
tive levels were listed in Table 1.
The essential oil and curcumin extraction yield (Y1, Y2)
were considered as the response functions using the follow-
ing equations:
Weight of oil extracted by SWE
Y1 5 3100; (2)
Weight of dried rhizome sample
Weight of curcumin extracted by SWE
Y2 5 3100: (3)
Weight of curcumin extracted by Soxhlet

Response Surface Design

In previous works, experiments were performed by one
parameter methodology (Khajenoori et al. 2009; Khajenoori
et al. 2013). In other words, only one factor was variable and
the others were constant. This method was expensive and
time consuming. Also, interactions between the parameters
were neglected. Design of experiments by RSM can over-
come these problems. RSM is a collection of mathematical
and statistical techniques. These techniques are used to opti-
RESULTS AND DISCUSSION
GC/MS Analysis
The chemical constituents of the oil are reported in Table 2.
GC/MS analysis of the oil showed the presence of 10 major
TABLE 2. CHEMICAL COMPOSITION OF TURMERIC RHIZOME

mize a response (output) which is influenced by several No. Oil component Component (%) Retention time (min)
independent variables (input). The aim of RSM to design 1 a-Phellandrene 6.50 12.34
optimization is reducing the cost and time of expensive 2 b-Caryophyllene 1.32 21.80
analysis methods (Hinkelmann and Kempthorne 2008). 3 Trans-b-Farnesene 0.54 21.98
Experimental data were fitted to the following second-order 4 Curcumin 10.49 22.70
polynomial model. The coefficients of the response surface 5 b-Bisabolene 3.12 23.14
6 b-Sesquiphellandrene 9.62 23.49
equations were estimated by MINITAB 16.
7 Cis-a-Bisabolene 1.11 23.56
8 b-Bisabolene 2.59 24.68
X
k X
k X
k21 X
k
9 Ar-Turmerone 62.88 26.11
Y 5b0 1 bi Xi 1 bii Xi2 1 bij Xi Xj ; (1)
10 c-Curcumin 1.83 26.47
i51 i51 i51i<j j52

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P. MOTTAHEDIN, A. HAGHIGHI ASL and M. KHAJENOORI SWE OF CURCUMIN AND ESSENTIAL OIL VIA RSM

TABLE 3. RESULTS FOR THREE FACTORS–THREE LEVELS USING B-B where T is extraction temperature (C), Q (mL/min) is sub-
METHOD critical water flow rate and dp (mm) is mean particle size.
Exp. T (C) Q (mL/min) dp (mm) Y1 (w/w)% Y2 (w/w)% The variables with the most significant effect on the essential
1 90 1.0 1.0 0.3010 56.4297 oil extraction yield were the linear terms of temperature,
2 150 1.0 1.0 0.8653 78.8321 flow rate, particle size and quadratic terms of temperature
3 90 4.0 1.0 0.4421 34.2333 and particle size (P < 0.05). According to Table 4, the quad-
4 150 4.0 1.0 1.2421 56.9854 ratic term of temperature has the highest effect on essential
5 90 2.5 0.5 1.2541 56.3400
oil extraction yield. The response equation fitted the experi-
6 150 2.5 0.5 1.5732 78.7224
7 90 2.5 1.5 0.7368 45.1276
mental data with R2 5 0.98. It means that the predicted val-
8 150 2.5 1.5 1.1087 67.4449 ues represent the experimental data adequately.
9 120 1.0 0.5 2.8875 86.8986 The linear term of temperature, flow rate and particle
10 120 4.0 0.5 3.6971 69.0224 size, also significantly influenced the curcumin extraction
11 120 1.0 1.5 2.4321 59.8109 yield (P < 0.05). The following equation was obtained from
12 120 4.0 1.5 3.1261 46.2121
curcumin extraction data:
13 120 2.5 1.0 3.2751 63.0263
14 120 2.5 1.0 3.5201 60.0798 Y2 50:187210:0665T 20:2936Q22:6285dp
15 120 2.5 1.0 3.4412 61.1911
22:080331024 T 2 20:0122Q 2 10:8339dp 2 (5)
25 25
18:6778310 TQ24:9833310 Tdp 10:0636Qdp ;
components. The main medicinal properties of oil are due
to presence of curcumin ( 10.5%). where T is extraction temperature (C), Q (mL/min) is sub-
critical water flow rate and dp (mm) is mean particle size.
The response equation fitted the experimental data with
Response Surface Analysis R2 5 0.96.
The obtained experimental results from essential oil and
curcumin extraction are summarized in Table 3. The experi- Effect of Independent Variables on the
mental data were applied to evaluate the coefficients of the Extraction Yield
second-order polynomial equation (Eq. 1). Table 4 repre-
The influence of operating conditions (temperature, sub-
sents the significance of each parameter by t-ratio and P
critical water flow rate and mean particle size) on the essen-
value. The smaller amount of P value and the larger absolute
tial oil and curcumin extraction yield was studied. Relative
amount of t-ratio are significantly the corresponding coeffi-
standard deviation percent (%RSD) was calculated on the
cients. Fitting the constants and coefficients into Eq. 1 for
basis of the obtained peak areas. The %RSD values were
the essential oil extraction yields, the following equation was
ranged from 1 to 14%. Response surface plots were drawn
obtained:
using the response (essential oil and curcumin extraction
Y1 5229:315010:5447T 10:4020Q22:8879dp yield) against two independent variables while the other
independent variable was constant at its zero level.
22:251131023 T 2 20:0704Q2 11:1883dp 2 (4)
As can be seen in Fig. 3, at constant water flow rate,
23 24
11:3099310 TQ18:7933310 Tdp 20:0385Qdp; increasing temperature causes the essential oil extraction

TABLE 4. REGRESSION COEFFICIENT OF THE FITTED QUADRATIC EQUATION AND STANDARD ERRORS FOR THE ESSENTIAL OIL AND CURCUMIN
EXTRACTION YIELD
Y1 Y2

Term Regression coefficients Std error t-ratio P value Regression coefficients Std error t-ratio P value
T 0.2568 0.0668 3.85 0.0120* 0.5013 0.0767 6.54 0.0013*
Q 0.2526 0.0668 3.78 0.0128* 20.4213 0.0767 25.49 0.0027*
dp 20.2510 0.0668 23.76 0.0132* 20.4038 0.0767 25.27 0.0033*
dp*dp 0.2971 0.0983 3.02 0.0293* 0.2085 0.1129 1.85 0.1241
T*T 22.0260 0.0983 220.61 <0.0001* 20.1872 0.1129 21.66 0.1581
Q*dp 20.0289 0.0944 20.31 0.7719 0.0477 0.1084 0.44 0.6783
Q*Q 20.1585 0.0983 21.61 0.1678 20.0276 0.1129 20.24 0.8168
T*Q 0.0589 0.0944 0.62 0.5599 0.0039 0.1084 0.04 0.9727
T*dp 0.0132 0.0944 0.14 0.8944 20.0007 0.1084 20.01 0.9948

*P < 0.05 indicates that the model terms are significant.

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SWE OF CURCUMIN AND ESSENTIAL OIL VIA RSM
FIG. 3. SURFACE PLOT OF THE ESSENTIAL OIL EXTRACTION YIELD AS
A FUNCTION OF TEMPERATURE AND FLOW RATE AT 20 bar AND 100
min EXTRACTION TIME
yield to increase up to 120C. After that, the yield decreases.
Temperature has a dual effect on essential oil yield. Increas-
ing the temperature, improve the solubility of essential oil.
This fact causes a higher extraction yield. On the other
hand, increasing the temperature, due to degradation of
thermally unstable compounds, results in a lower yield. A
burning smell produced in laboratory may be the result of
degradation of some of the constituents at higher tempera-
tures. Eikani et al. (2013) reported a similar result for SWE
of essential oils from Cinnamon Bark. Due to the discussion
mentioned in section 3.2, P value for temperature is lower
than the others. Temperature is the main parameter which
affects the physicochemical properties of water and the
compounds to be extracted.
According to Fig. 4, at a constant particle size, increasing
the flow rate leads to increase the essential oil extraction
yield. It is because of increase in superficial velocity and
quicker mass transfer. It is in accordance with previous
works (Eikani et al. 2007; Khajenoori et al. 2009; Eikani
et al. 2013). It is clear that using higher water flow rates leads
to increase the extract volume and to decrease the concen-
tration of final extracts. So, to prevent from low extract con-
centration and long time, the flow rate upper 4 mL/min and
lower 1 mL/min were not selected.
FIG. 4. SURFACE PLOT OF THE ESSENTIAL OIL EXTRACTION YIELD AS
A FUNCTION OF FLOW RATE AND MEAN PARTICLE SIZE AT 20 bar AND
100 min EXTRACTION TIME
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P. MOTTAHEDIN, A. HAGHIGHI ASL and M. KHAJENOORI
FIG. 5. SURFACE PLOT OF THE ESSENTIAL OIL EXTRACTION YIELD AS
A FUNCTION OF TEMPERATURE AND MEAN PARTICLE SIZE AT 20 bar
AND 100 min EXTRACTION TIME
Figure 5 indicates the effect of mean particle size and tem-
perature on the essential oil extraction yield. It shows that at
constant temperature, the yield decreases with increasing
mean particle size. It is the result of lower mass transfer
resistance and higher contacting surface between solvent
and solute in smaller size particles. Therefore due to better
mass transfer rate at smaller particle size, the extraction yield
increases. Mortazavi et al. (2010) achieved this result for
extraction of essential oils from Bunium persicum Boiss.
Figures 6–8 show the effects of temperature, water flow
rate and mean particle size on curcumin extraction yield.
Figure 6 demonstrates that, at constant water flow rate,
increase in temperature results in increase in curcumin
extraction yield, but this increasing slope is sharp in the
temperature range of 90–120C and 120–150C, the yield
increase with a mild slope. Because of apparatus operating
limitation, temperatures higher than 150C were not applied.
Although the essential oil yield decreases at 150C, curcumin
extraction yield increases. It may be the result of improved
curcumin solubility at elevated temperatures. The result is
in agreement with previous studies when subcritical water
FIG. 6. SURFACE PLOT OF CURCUMIN EXTRACTION YIELD AS A
FUNCTION OF TEMPERATURE AND FLOW RATE AT 20 bar AND 100
min EXTRACTION TIME
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P. MOTTAHEDIN, A. HAGHIGHI ASL and M. KHAJENOORI SWE OF CURCUMIN AND ESSENTIAL OIL VIA RSM

was used for extraction (Anurukvorakun 2013; Khajenoori

et al. 2015). Cheigh et al. (2012) reported the maximum

yields of Aavanones including hesperidin and narirutin
from Citrus unshicu by SWE at the temperature of 160C.
However, degradation of compounds could be occurred
with increased temperature.
According to Fig. 7, at a constant mean particle size,
increasing the flow rate leads to decrease in curcumin extrac-
tion yield. At higher water flow rates, the resident time of
water in the cell is decreased and the solvent remains in con-
tact with the sample for a shorter time, therefore the extraction
yield of curcumin decreases (Reverchon and Marco 2006).
Also turmeric rhizome is physically hard and contacting its FIG. 8. SURFACE PLOT OF CURCUMIN EXTRACTION YIELD AS A
essential oil which bears cells to the solvent is difficult. There- FUNCTION OF TEMPERATURE AND MEAN PARTICLE SIZE AT 20 bar
AND 100 min EXTRACTION TIME
fore, at higher water flow rates, turmeric rhizomes do not
have sufficient time for mass transfer. Because of long extrac-
son between SWE and two other methods indicated that
tion time, the flow rates lower than 1 mL/min were not tested.
Soxhlet has the highest and hydrodistillation has the least
The effect of mean particle size on curcumin extraction yield
yield. But, due to the chromatograms obtained from the
is presented in Fig. 8. It displays that at constant temperature,
three methods, SWE had the most oxygenated compounds.
curcumin extraction yield decreases with increasing mean par-
Also in SWE, the extraction time is very short and this leads
ticle size. It is similar to the manner of the essential oil yield.
to reduction of energy and time.
The optimum curcumin extraction conditions were tem-
perature of 150C, subcritical water flow rate of 1 mL/min
and mean particle size of 0.5 mm. For verifying the predic- CONCLUSION
tive capacity of the model, the optimum condition was used
Experimental subcritical water extraction of curcumin from
for two extraction tests. In this condition, the average of cur-
turmeric rhizome was carried out at temperature range of
cumin extraction yields was 90.1947%. Predicted value by
90–150, water flow rate of 1–4 mL/min, and mean particle
MINITAB is 92.0097%. In other words, experimental result
size of 0.5–1.5 mm. Response surface methodology was used
confirms the predicted result obtained from the model for
to optimize the operating conditions. In this study, for the
the extraction of curcumin from turmeric rhizome.
first time, the effect of three parameters (temperature, mean
particle size and flow rate) was considered on SWE of essen-
Comparison With Hydrodistillation and
tial oil and curcumin from turmeric rhizome. The optimal
Soxhlet Method
conditions for curcumin extraction were: temperature
Curcumin extraction yields obtained from hydrodistillation 150C, mean particle size 0.5 mm and flow rate 1 mL/min.
and Soxhlet were 2.9837 and 4.4629, respectively. Compari- The value of the coefficient of determination, R2, as a mea-
sure of the degree of fit, for essential oil and curcumin
extraction yields were 0.98 and 0.96, respectively. Therefore,
the model adequately represents the experimental data.
Comparison between SWE, hydrodistillation and Soxhlet
methods showed that the extraction yield of Soxhlet was
higher than the other two methods, but SWE was more
selective for desirable compound. Also, subcritical water
extraction time is shorter than Soxhlet and hydrodistillation
methods. Therefore consuming time and energy in SWE is
lower than the conventional methods and SWE is a green
and effective method for extraction of essential oil and cur-
cumin from turmeric rhizome.

NOMENCALTURE
FIG. 7. SURFACE PLOT OF CURCUMIN EXTRACTION YIELD AS A
FUNCTION OF FLOW RATE AND MEAN PARTICLE SIZE AT 20 bar AND
dp mean particle size (mm)
100 min EXTRACTION TIME k number of variables

Journal of Food Processing and Preservation 2017; 41: e13095; V

C 2016 Wiley Periodicals, Inc. 7 of 9
SWE OF CURCUMIN AND ESSENTIAL OIL VIA RSM
Q subcritical water flow rate (mL/min)
%RSD relative standard deviation percent
R2 coefficient of determination
T extraction temperature (C)
X1, X2, . . ., Xk independent variables
Y extraction yield, b0 : regression coefficients
for intercept term, bi : regression coeffi-
cients for linear term, bii : regression coeffi-
cients for quadratic term, bij : regression
coefficients for interaction term
ACKNOWLEDGMENT
The authors tend to appreciate for the partial financial sup-
port from the Science & Technology Park of Semnan
University.
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