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Journal of Food Process Engineering ISSN 1745-4530

APPLICATION OF PULSED ELECTRIC FIELD FOR OIL


EXTRACTION FROM SUNFLOWER SEEDS: ELECTRICAL
PARAMETER EFFECTS ON OIL YIELD
IVAN SHORSTKII1,2,3, MEYSAM SHARIFZADEH MIRSHEKARLOO1 and EVGENY KOSHEVOI2
1
Institute of Materials Research and Engineering, A*STAR (Agency for Science, Technology and Research), Singapore
2
Department of Process Equipment and Life-Support Systems, Kuban State University of Technology, 128 Krasnaya Street, Krasnodar 350072,
Russian Federation

3
Corresponding author. ABSTRACT
TEL: +65-831-261-00,
+7-967-652-5881; The application of pulsed electric field (PEF) as one of the nonthermal intensifica-
FAX: +7-861-275-22-79; tion methods has been proposed to increase oil yield extraction from sunflower
EMAIL: thegector@mail.ru seeds. PEF treatments have been carried out under various electrical parameters
such as electric field, pulsed frequency, pulse width, time of treatment and sample
Received for Publication April 30, 2015
Accepted for Publication August 6, 2015
conductivity. 55 fractional factorial design has been used for the analysis of the
impact of PEF parameters on oil yield, and oil yield square model parameters have
doi:10.1111/jfpe.12281 been investigated. The oil yield was found to increase by 9.1% after treatment of
sunflower seeds by variation of PEF parameters: 30 s under an electric field of
7.0 kV/cm having frequency of 15 Hz, solvent content of 40 wt% and pulse width
of 30 μs.

PRACTICAL APPLICATIONS
Here, we study the application of assisted pulsed electric field for oil extraction
from sunflower seeds and we find the most effective variation of pulsed electric
field parameters for treatment. It is very important in the industrial world as it
deals with the time, quality of production and cost, which are usually carried out
without preliminary treatment.

Screw presses are usually used for industrial-scale pressing;


INTRODUCTION
however, the hydraulic presses can also be employed (Evon
Sunflower (Helianthus annuus) oil is the most popular oil et al. 2007). Gasoline, super critical CO2, hexane and
produced in Russian Federation, Ukraine, Argentina and ethanol are usually used as solvents for extraction
some European countries. For example, production of sun- (Regitano-d’Arce et al. 1994; Hegel et al. 2011). To obtain
flower oil amounted 530 million tons in 2010 and the maximal value of the oil yield, solvent extraction is most
export exceeded 340 million tons (Bonos et al. 2011). Sun- commonly used after pressing. However, extraction process
flower oil is widely used in food processing, cooking, pro- required long time duration (ko0cvoj) and preliminary
duction of soap, mayonnaise, etc. The percentage of oil in treatments become necessary. To improve solvent extraction
this seeds can range from 45 to 52%. Standard sunflower efficiency, pulsed electric fields (PEFs) emerge as a possibil-
seeds mainly contain α-tocopherol, which accounts for ity to provide highly effective and nonthermal pretreatment
more than 90% of the total tocopherols. β- and process to seeds.
γ-tocopherols can be present in sunflower seeds usually in Various studies have investigated the effect of PEF treat-
amounts below 2% of the total tocopherols (Demurin et al. ment on cell disintegration (Lebovka et al. 2004). Many
1996). Moreover, sunflower seeds present high content of reports have demonstrated the advantages of PEF applica-
protein. The fatty acid content of this oil is composed tion that includes good extraction efficiency as well as high
mainly of linoleics, linolenic stearics, palmitic myristics and juice yield at minimum power consumption at low frequen-
arachidic oleics. Pressing and solvent extraction are the cies (Fincan and Dejmek 2002; Dymek et al. 2014). The
most common processes used for oil extraction from seeds. application of PEF for oil extraction from oilseeds and its

Journal of Food Process Engineering •• (2015) ••–•• © 2015 Wiley Periodicals, Inc. 1
PEF-ASSISTED OIL EXTRACTION FROM SUNFLOWER SEEDS I. SHORSTKII, M.S. MIRSHEKARLOO and E. KOSHEVOI

functional ingredients (Sarkis et al. 2015) has received Sunflower seeds were ground into powder in an agate
increasing interest during the last 10 years. Some reports mortar until particle size was less than 0.5 mm. Conductiv-
have found that PEF pretreatment could increase oil yield of ity of the samples was regulated by adding a liquid solvent,
maize germs (Guderjan et al. 2005) and olives (Kardjilova namely, bio-ethanol (absolute ethanol, 99.8%, Sigma
and Hlavacova 2013) by about 32.4 and 6.5–7.4%, Aldrich), in content ranging from 10 to 50 wt%.
respectively.
PEF treatment can improve oil yield as well as oil quality PEF Treatment
extracting from solid oil contain seeds. Guderjan et al.
(2007) reported that samples preconditioning before treat- Ground sunflower seeds were treated by PEF in a dielectric
ment, like moisture control of seeds, to increase conductiv- chamber, having two titanium top and bottom electrodes
ity during PEF treatment is required. (diameter 40 mm). Electrode gap was set as 5 mm to reach a
Soaking in tap water was used to receive optimal conduc- treatment volume of about 16 cm3, which is enough to
tivity of rapeseeds (Guderjan et al. 2007). However, drying obtain the required amount of samples for extraction
process is required after soaking, resulting in increased process. Square electric pulses were generated by a function
experimental time. Adding the solvent directly into the sam- generator (Agilent 33220A, Agilent Technologies, Loveland,
ple to increase the conductivity parameter of the sample is a Colorado 80537, USA) and amplified by a high-voltage
more efficient method that was used in the current work. amplifier (Trek COR-A-TROL 610D, TREK Inc, Lockport,
In summary, many reports have demonstrated the appli- NY 14094, USA) in range up to 10 kV.
cation of PEF for oil extraction from oilseeds as an intensifi- The chamber was filled with ground samples to form a
cation method, increasing oil yield. Although the effect of sunflower cake, and electrodes were fully covered. Positive
PEF-assisted intensification on oil yield of various oilseeds trains of pulses were applied to samples. The characteristics
has been studied in the literature, however, PEF-assisted of the applied electric pulses such as electric field, frequency
extraction of sunflower seeds with regulating conductivity and pulse width were monitored using a digital oscilloscope
as one of the nonthermal and more effective intensification (Tektronix TDS 220) with PHV 621 oscilloscope probe
methods and its impact on oil yield from sunflower seeds is (400 MHz, ×100). The experimental setup is shown in
yet to be investigated. Fig. 1a.
The aim of this work was to find the effect of different
PEF treatment parameter variations on the oil yield of sun- FFD
flower seeds with preliminary-adjusted conductivity via sol- Different variations of parameters were used in this study
vent adding. In addition, this study aimed to find the effect (Fig. 1b). Electrical parameter ranges were selected from
of each PEF parameter, such as electric field, frequency, sol- works based on PEF treatment of oilseeds, such as olives
vent content, pulse width and time of treatment, on the oil (Kardjilova and Hlavacova 2013), rapeseeds (Guderjan et al.
yield using fractional factorial design (FFD). The results of 2007) and sesame (Sarkis et al. 2015). As summarized in
oil yield were compared with control and treated samples. Table 1, a 55 (five levels and five factors) FFD (Ahnazarova
and Kafarov 1985) was used. A full replication would take
MATERIALS AND METHODS 55 = 525 runs. Hence, this design is a 1/25th rep = 525/
25 = 25 to test several factors with minimum number of
Materials trials. The effect of electric field (1, 3, 5, 6, 7 kV/cm), pulsed
Hulled sunflower seeds grown in 2014 in the U.S.A. were frequency (0.5, 1.5, 5, 10, 15 Hz), solvent content (10, 20, 30,
purchased at a local market (cold storage, Singapore). All 40 and 50 wt%), time of treatment (10, 30, 60, 90, 120 s)
seeds were stored in the dark at 4S until further analysis. and pulse width (10, 20, 30, 40, 50 μs) on oil yield was
Bio-ethanol (absolute ethanol, 99.8%, Sigma Aldrich, investigated.
Saint Louis, MO 63103, USA) was used as a solvent to adjust As a planning matrix, standard Graeco–Latin square was
conductivity of samples during PEF treatment. Hexane used (Ahnazarova and Kafarov 1985) as presented in
(n-Hexane, 99%, tech grade) was used as solvent during oil Table 2. Conductivity of samples was 30, 22.5, 15, 7.5 and
extraction. 3.5 μs/m for solvent content of 10, 20, 30, 40 and 50 wt%,
respectively. The PEF treatment was carried out at room
Moisture Content and Sample Preparation temperature, approximately 20C.

The initial moisture content of sunflower seeds was calcu-


Oil Extraction
lated on a dry weight basis and was found to be about
7.95% (dwb). The moisture content was measured Sunflower oil was extracted from the PEF-treated samples
gravimetrically (Moravec et al. 2008). by solvent extraction using hexane. Oil yield was deter-

2 Journal of Food Process Engineering •• (2015) ••–•• © 2015 Wiley Periodicals, Inc.
I. SHORSTKII, M.S. MIRSHEKARLOO and E. KOSHEVOI PEF-ASSISTED OIL EXTRACTION FROM SUNFLOWER SEEDS

FIG. 1. EXPERIMENTAL SETUP FOR PULSED ELECTRIC FIELD (PEF) TREATMENT (A); VARIATION OF PEF TREATMENT PARAMETERS (B): ELECTRIC
FIELD (E), FREQUENCY (F), SOLVENT CONTENT (C), TREATMENT TIME (Τ), PULSE WIDTH (W)

mined according to the method reported in Guderjan et al. Sunflower cake conductivity was measured and plotted
(2007). The PEF-treated sunflower seeds were heated to 40C over frequency. Because the phase angle was low, at least at
for 3 h in an oven to remove the ethanol. Subsequently, 2.3– frequencies above 100 Hz, conductivity can be calculated
2.5 g of samples was placed in a tube and mixed with 40 mL as:
of hexane. The mixtures were shaken in shaker at frequency
of 400 min−1 for 3 h at room temperature to extract the oil.
The extracted oils were filtered using filter paper. Finally, TABLE 2. FRACTIONAL FACTORIAL DESIGN, 55: THE EFFECT OF
DIFFERENT FACTORS ON OIL YIELD FACTORS: ELECTRIC FIELD, E;
hexane was removed by evaporation in a fume hood for
FREQUENCY, F; SOLVENT CONTENT, C; TIME OF TREATMENT, Τ; AND
24 h. PULSE WIDTH, W

Exp. E (kV/cm) f (Hz) C (wt%) τ (s) W (μs) Y (%)


Conductance Analysis 1 1 0.5 10 10 10 38.02
2 1 1.5 20 30 20 40.1
Conductance of samples was measured by a precision
3 1 5 30 60 30 38.37
impedance analyzer (Agilent Technologies, 4294A, Agilent
4 1 10 40 90 40 40.55
Technologies, Loveland, Colorado 80537, USA) using a 5 1 15 50 120 50 42.36
four-terminal pair connection (BNC, 16089A Large Kelvin 6 3 0.5 30 90 50 39.6
Clip Lead, TREK Inc, Lockport, NY 14094, USA) as shown 7 3 1.5 40 120 10 45.4
in Fig. 1a. Electrical impedance spectroscopy was conducted 8 3 5 50 10 20 44.17
at frequencies ranging from 100 to 1 MHz. 9 3 10 10 30 30 46.33
10 3 15 20 60 40 41.83
11 5 0.5 50 30 40 47.32
TABLE 1. GRAECO–LATIN SQUARE 55, AI – ELECTRIC FIELD, 1 KV/CM 12 5 1.5 10 60 50 40.46
(A1), 3 KV/CM (A2), 5 KV/CM (A3), 6 KV/CM (A4), 7 KV/CM (A5); BJ 13 5 5 20 90 10 43.21
FREQUENCY, 0.5 HZ (B1), 1.5 HZ (B2), 5 HZ (B3), 10 HZ (B4), 15 HZ 14 5 10 30 120 20 39.98
(B5); CQ – SOLVENT CONTENT, 10 WT% (C1), 20 WT% (C2), 30 WT% 15 5 15 40 10 30 47.38
(C3), 40 WT% (C4), 50 WT% (C5); DK – TIME OF TREATMENT, 10 S 16 6 0.5 20 120 30 44.19
(D1), 30 S (D2), 60 S (D3), 90 S (D4), 120 S (D5); EM – PULSE WIDTH, 17 6 1.5 30 10 40 44.34
10 ΜS (E1), 20 ΜS (E2), 30 ΜS (E3), 40 ΜS (E4), 50 ΜS (E5) 18 6 5 40 30 50 47.78
19 6 10 50 60 10 45.11
b1 b2 b3 b4 b5
20 6 15 10 90 20 45.6
a1 c1, d1, e1 c2, d2, e2 c3, d3, e3 c4, d4, e4 c5, d5, e5 21 7 0.5 40 60 20 47.32
a2 c3, d4, e5 c4, d5, e1 c5, d1, e2 c1, d2, e3 c2, d3, e4 22 7 1.5 50 90 30 48.24
a3 c5, d2, e4 c1, d3, e5 c2, d4, e1 c3, d5, e2 c4, d1, e3 23 7 5 10 120 40 47.03
a4 c2, d5, e3 c3, d1, e4 c4, d2, e5 c5, d3, e1 c1, d4, e2 24 7 10 20 10 50 44.77
a5 c4, d3, e2 c5, d4, e3 c1, d5, e4 c2, d1, e5 c3, d2, e1 25 7 15 30 30 10 47.15

Journal of Food Process Engineering •• (2015) ••–•• © 2015 Wiley Periodicals, Inc. 3
PEF-ASSISTED OIL EXTRACTION FROM SUNFLOWER SEEDS I. SHORSTKII, M.S. MIRSHEKARLOO and E. KOSHEVOI

σ = G ⋅l A (1)

where G, l and A are conductance, thickness and area of the


sample, respectively.

Disintegration Index
The cell damage induced by electrical treatment can be
indirectly quantified by measuring the electrical conductiv-
ity of the sunflower cake.
This factor allows the determination of the charged par-
ticle concentration (Lebovka et al. 2002; Lebovka et al.
2004). The cell disintegration index, Z, can be determined
by the following equation:
Z = (σ − σ i ) (σ d − σ i ) (2)
FIG. 2. OIL YIELD FOR 25 EXPERIMENTS AFTER PULSED ELECTRIC
In this equation, σ is the electrical conductivity after the FIELD TREATMENT

treatment, σi is the initial electrical conductivity of the


samples (which was very close to zero) and σd is the electri- General Effect of PEF on Oil Yield
cal conductivity of the maximally disintegrated samples.
Figure 2 represents the effect of PEF-processing factors on
For example, this index has been reported for different
oil yield of samples. In general, oil yield of sunflower seeds
PEF treatment times (1–7 ms) for sesame cake (Sarkis et al.
increased after PEF processing. Details of all of the param-
2015) and hulled and nonhulled rapeseed (Guderjan et al.
eters and their value are listed in Table 2.
2007). It has been shown that the cell damage increases as a
The oil yield ranged from 39.14 to 48.04% with its
function of PEF treatment time. However, disintegration
maximum at 22nd experiment, at electric field of 7.0 kV/
saturated at a certain critical treatment time. The
cm, frequency of 1.5 Hz, solvent content of 50 wt%, time of
disintegration of PEF-treated sesame and hulled and
treatment at 90 s and pulse width of 30 μs.
nonhulled rapeseeds reached a maximum of 67, 55 and
17%, respectively. Disintegration Index and Conductivity of
Sunflower Cake

Statistical Analysis PEF treatment increased sunflower cake tissue damage. At


electric fields higher than 1 kV/cm permanent pores were
The analysis of the results of the fractional factorial experi- generated and irreversible disintegration happened, which
ments was performed using the software MS Excel 2007 resulted in improved oil yield. From Eq. (2) for intact cells
(Redmond, Washington, USA). The effect of each of the Z = 0; for total cell disintegration Z = 100%. Figure 3a rep-
PEF-processing factors (electric field, frequency, pulse resents frequency dependence of conductivity of sunflower
width, treatment time and solvent content) on oil yield as cakes, with various solvent contents, before and after PEF
well as their square model parameters were calculated. treatment with electric field strength 5 kV/cm.
All experiments were carried out in triplicate. Average Figure 3b illustrates the cell disintegration of PEF-treated
values and standard deviations of data were calculated, and sunflower seed cakes at different electric fields as well as
statistical significance was declared at P < 0.05 tested by untreated samples. With increased electric field, the cell dis-
analysis of variance (ANOVA). integration index of sunflower seeds (Fig. 3b) increased to a
maximum of 41% at electric field of 7 kV/cm. The better
and easier disintegration of sunflower seedcake could be
RESULTS AND DISCUSSION due to the improved electrical conductivity of the PEF treat-
The sample specifications showed that the seeds used in this ment. Similar disintegration index values were also found
work had an oil content of 49.18 ± 0.01% (results expressed for PEF-treated rapeseeds (Guderjan et al. 2007).
in fresh matter basis). The initial moisture content of the
Main Effects of PEF Parameters on Oil Yield
material was measured to be about 7.95 ± 0.5%. The oil and
protein amounts were similar to those reported by Brevedan Graeco–Latin square 55 was analyzed by ANOVA software
et al. (2000). using dispersion analysis. Results were presented in Table 3.

4 Journal of Food Process Engineering •• (2015) ••–•• © 2015 Wiley Periodicals, Inc.
I. SHORSTKII, M.S. MIRSHEKARLOO and E. KOSHEVOI PEF-ASSISTED OIL EXTRACTION FROM SUNFLOWER SEEDS

FIG. 3. THE DEPENDENCE OF CONDUCTIVITY, Σ, ON FREQUENCY RECORDED AT DIFFERENT SOLVENT COMPOUNDS (A) AND THE
FREQUENCY-DEPENDENT CONDUCTIVITY, Σ, OF SUNFLOWER CAKE RECORDED FOR SAMPLES WITH DIFFERENT SOLVENT CONTENT (B)

The significance of the impact factors was checked by Fisher


Estimates for Graeko–Latin Square
criterion, expressed by the following equation:
To estimate the main parameters of square design model,
F = SASOV SAError > Ftable (3)
the following equations were used:
where SASOV is the square average of source variations
μ = average (Y )
(Table 3); SAError is the error square average (Table 3); Ftable is
the Fisher criterion table value for degrees of freedom
α i = Yi − average (Y )
F0,95(f1, f2) = 3.26, where f1 and f2 are degrees of freedom 4
and 12, respectively.
β j = Y j − average (Y )
The Graeco–Latin square design model for oil yield was
extracted from the obtained data using the following equa- γ q = Yq − average (Y ) (5)
tion (Ahnazarova and Kafarov 1985):
yijqkm = μ + α i + β j + γ q + δ k + ζ m + ε ijqkm (4) δ k = Yk − average (Y )

where μ denotes the general location parameter of all ζ m = Ym − average (Y )


experiments; αi, βj, γq, δk and ζm denote the effect for block i,
j, q, k and m, respectively; and εijqkm is the random experi- where (from Table 1) average (Y) is the average of all Y for
mental error. all experiments; Yi is the average of all Y for which a = i,
i = 1, . . . , 5; Yj is the average of all Y for which b = j, j = 1,
TABLE 3. DISPERSION ANALYSIS OF GRAECO–LATIN SQUARE BY . . . , 5; Yq is the average of all Y for which c = q, q = 1, . . . , 5;
ANOVA SOFTWARE Yk is the average of all Y for which d = k, k = 1, . . . , 5; Ym is
Source of Degrees of Square Square
the average of all Y for which e = m, m = 1, . . . , 5.
variations freedom sum average The impact of the PEF treatment factors on their square
model parameters is shown in Fig. 4. Zero point of y-axis is
a 4 5.533 1.383
b 4 0.336 0.084
the value μ = 43.85 from Eq. (5). The biggest effect was pro-
c 4 2.187 0.546 duced by electric field (Fig. 4a), solvent content (Fig. 4c)
d 4 1.051 0.262 and treatment duration (Fig. 4d).
e 4 0.429 0.107 From the obtained data shown in fig. 4, the optimized
Error 12 46,425.03 5,803.1 PEF parameters according to their effects on oil yield are:
Total 28 46,434.57 5,805.5 • Electric field has a monotonously growing effect. A
ANOVA, analysis of variance. similar dependence was reported in Kathiravan et al. (2014)

Journal of Food Process Engineering •• (2015) ••–•• © 2015 Wiley Periodicals, Inc. 5
PEF-ASSISTED OIL EXTRACTION FROM SUNFLOWER SEEDS I. SHORSTKII, M.S. MIRSHEKARLOO and E. KOSHEVOI

FIG. 4. (A–E) IMPACT OF PULSED ELECTRIC FIELD FACTORS ON THE SQUARE MODEL PARAMETERS (EXPERIMENTS RUN IN TRIPLICATE)

and Boussetta et al. (2015). From our experiments, the 40 wt% with treatment duration of 30 s and pulse width of
optimal value (maximum value at a5 in Fig. 4a) is 7 kV/cm. 30 μs.
• Frequency has also a monotonously growing effect. The results of this study show that treatment with pulsed
However, the impact of frequency is too small to be taken electrical field could be used as an intensification
into account. The maximum value of 15 Hz was obtained at nonthermal method to increase oil yield from sunflower
b5, Fig. 4b. seeds. The obtained results will be used in the future in food
• The effect of solvent content was found to have a processing technologies as a pretreatment method for larger
maximum value at c4, Fig. 4c, for 40 wt% of solvent. scale oil extraction from sunflower seeds.
• Optimal treatment duration is 30 s (at d2, Fig. 4d).
• Maximum effect value of pulse width (30 μs) was
obtained at e3, Fig. 4e.
ACKNOWLEDGMENTS
Additional experiments were carried out in an attempt to The authors would like to thank the President of Russian
determine the oil yield value for PEF parameters after opti- Federation Scholarship for financial support. Thanks to Dr.
mization: E = 7 kV/cm−1, f = 15 Hz, C = 40 wt%, τ = 30 s, Maria Antipina from the Institute of Materials Research and
W = 30 μs. Obtained value of oil yield was 48.24%, which is Engineering (IMRE, A*STAR, Singapore), for providing
0.2% greater than before optimization. research training opportunity in IMRE. This work was sup-
ported by the Federal Target Program “Research and devel-
opment on priority directions of scientific-technological
CONCLUSIONS
complex of Russia in 2014–2020 years” (Unique No.
In this work, the effect of PEF treatment on oil extraction RFMEF157714X0046).
yield from sunflower seeds was investigated. The optimal
variation of PEF parameters was determined, and oil yield
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6 Journal of Food Process Engineering •• (2015) ••–•• © 2015 Wiley Periodicals, Inc.
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Journal of Food Process Engineering •• (2015) ••–•• © 2015 Wiley Periodicals, Inc. 7

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