Professional Documents
Culture Documents
The purpose of present study was to investigate the (g/m3), respectively; k mass transfer coefficient, ms−1; A
gum extraction process from wild sage seed. This study surface area for mass transfer process, m2.
also focuses on determination of the gum yield, effects of Since the extraction was conducted in a batch
pH and temperature, reaction time and water/seed ratio. process and the volume was constant throughout the
These optimum parameters were applied to a kinetic model experiment, eq. (2) can be written as [9]
based on mass transfer coefficient. Thermodynamic para-
dWA A
meters that include entropy, enthalpy and Gibb Free ¼ k ðwAi wA Þ ð3Þ
dt v
Energy of extraction of gum were also determined.
dWA
¼ K ðwAi wA Þ ð4Þ
dt
2 Materials and methods where K is volumetric mass transfer coefficient. To solve
eq. (4) by integration, following condition was used where
2.1 Extraction of gum the mass of wild sage seed gum is zero in liquid (WA) at
the beginning of the extraction process. Considering this
Wild sage seeds were purchased from a local market in condition, integration of eq. (4) resulted as
Gorgan, Iran. The cleaned wild sage seeds were soaked in h i
WA ¼ WAi 1 expðKtÞ ð5Þ
distilled water (for 0.5–60 min). In the extraction pro-
cesses, there are multiple independent variables affecting Rearranging eq. (5) in terms of yield per mass of wild
the gum yield. The effect of water/seed ratio (30:1 sage seed gum, the kinetic model used in this study was
and 40:1 at two levels), pH (5.5–8.5 at three levels) and h i
temperature (25–55°C at three levels) on the wild sage YA ¼ YAi 1 expðKtÞ ð6Þ
seed gum extraction was studied. Separation of the
hydrocolloid from the swollen seeds was achieved by where YA and YAi is yield of wild sage seed gum in liquid
passing the seeds through an extractor equipped with a at time, t (h) and equilibrium; and K volumetric mass
rotating plate that scraped the gum layer on the seed transfer coefficient. To determine the value of K (h−1) and
surface. The extracted solution was then filtered and YAi a nonlinear and multiple regression method was used
dried in an air forced oven at 50°C (convection oven, to calculate numerically. Curve Expert program version
Memmert Universal, Schwabach, Germany). The gum 1.34 was used to fit the data in order to obtain the mass
yield (gum content) of the wild sage seed was calculated transfer value and the yield of gum.
as below:
utilized by a large number of previous works to determine free energy of extraction. The plot of lnF against 1/T is
diffusivity values from experimental drying data [11], used to find the value of ΔH and ΔG from the slope and
leaching experiments [12] or extraction process [7, 9]. ΔS from intercept [9].
To determine the effect of mass transfer within the
seed on the extraction of the gum, Thiele modulus ’ was
calculated based on Giri and Sharma’s [13] equation:
3 Results and discussion
dp Kρp 0:5
’¼ ð8Þ
6 Deff In general, the extraction yield was influenced by the
interaction effect of aqueous extraction variables. The
The value dp represents the seed diameter, K is the
maximum value of gum obtained from extraction of
extraction rate, s−1, ρp is the density of the seed. The
wild sage seed was 12.5% at 55°C, pH ¼ 7 and water to
system is assumed to have no internal mass transfer
seed 40 to 1. This value was greater than the extraction
limitation if the Thiele modulus is <2, and the system
yield reported for Flaxseed gum 7.9% [14] and Yanang
suffers from the internal mass transfer limitation if it is
gum 4.54% [15].
above 10 [13].
Although the gum extraction yield was related to the
single main effects of all aqueous extraction variables,
but it was positively proportional to the interaction
2.4 Thermodynamic parameters effects of pH with water/seed ratio and temperature [8].
14
12
10
8
Yield%
pH = 5.5 pH = 7
2
pH = 8.5 Kinetic model
0
0 10 20 30 40 50 60 70
Time (min)
Figure 1 Effect of pH on gum extraction process at 40°C and water/seed ratio 30:1, experimental and the predicted values
14
12
10
8
Yield%
pH = 5.5 pH = 7
2
pH = 8.5 Kinetic model
0
0 10 20 30 40 50 60 70
Time (min)
Figure 2 Effect of pH on gum extraction process at 40°C and water/seed ratio 40:1, experimental and the predicted values
the gum to diffuse quickly from the seed to the water. Table 2 Parameters fitted for gum extraction process of wild sage
When the maximum amount of extractable gum was seed at water/seed ratio 40:1
reached, the gum yield remains the same even after
extending the extraction time. pH Temperature (°C) K (h−1) YAi (wt%) R
The graph illustrates that more carbohydrates were 5.5 25 5.03 11.11 0.99
extracted in neutral water. The highest value of gum was 5.5 40 14.78 9.58 0.96
obtained in the pH ¼ 7. The gum yield decreased on 5.5 55 14.29 10.57 0.94
average from 11.77% to 10.82%, with decrease in pH 7 25 4.70 12.56 0.99
7 40 9.99 11.78 0.98
from 7 to 5.5 (water/seed ratio 40:1).
7 55 14.60 10.39 0.96
Wu et al. [16] also reported that the optimum condi- 8.5 25 6.45 9.90 0.99
tions for the extraction procedure of crude polysacchar- 8.5 40 12.67 10.08 0.96
ides from boat-fruited sterculia seeds were pH equal 7. 8.5 55 15.64 10.51 0.95
Tables 1 and 2 show the calculated values of the mass
transfer coefficients (K) and the equilibrium yield of gum
(YAi) at various temperatures, pH and water/seed ratio using values were 5.42–16.87 (h−1) at water/seed ratio 30:1. The
eq. (6). Parameters of kinetic model, YAi and K, were esti- mass transfer coefficient value (K) increased from 11.45 (h−1)
mated by nonlinear square fit from equation to experimental to 11.84 (h−1), with increase in pH from 5 to 7 but it decreased
data using Curve Expert 1.34. The mass transfer coefficient from 11.84 (h−1) to 11.70 (h−1), with increase in pH from 7 to 9
(water/seed ratio 30:1).
Table 1 Parameters fitted for gum extraction process of wild sage
seed at water/seed ratio 30:1
3.2 Effect of temperature
−1
pH Temperature (°C) K (h ) YAi (wt%) R
Figures 3 and 4 illustrate the gum extraction yield of wild
5.5 25 5.42 12.41 0.99 sage seed at water/seed ratio 30:1 and 40:1, respectively,
5.5 40 12.05 10.13 0.95
at different temperature and pH ¼ 8.5. The increase in
5.5 55 16.87 9.88 0.94
7 25 11.11 9.13 0.99
temperature increases the gum yield during extraction
7 40 10.35 11.21 0.96 process. Increasing the temperature causes the reaction
7 55 14.06 10.51 0.94 time to be reduced as extraction occurs faster. The gum
8.5 25 6.18 8.86 0.99 yield increased from 9.96% to 10.90%, with increase in
8.5 40 13.99 8.95 0.95 temperature from 25°C to 55°C (water/seed ratio 30:1).
8.5 55 14.93 10.22 0.97
Temperature as an independent variable increases the
12
10
8
Yield%
2 25°C 40°C
Figure 3 Effect of temperature on gum extraction process at pH ¼ 8.5 and water/seed ratio 30:1
14
12
10
Yield%
4
25°C 40°C
2
55°C Kinetic model
0
0 10 20 30 40 50 60 70
Time (min)
Figure 4 Effect of temperature on gum extraction process at pH ¼ 8.5 and water/seed ratio 40:1
ability of the solvent to solubilize the compounds and easier mass transfer of water-soluble polysaccharide from
decreasing the viscosity of the liquid solvent which is the cell wall into the extract [8].
allowing better penetration of the solvent into the solid Although the extraction yield of polysaccharides was
matrix [17]. Mazza and Biliaderis [18] reported that tem- also high at 100°C, increasing temperature will bring
perature was the major factor affecting the extraction about the increase in cost for the extraction process
yields of flaxseed gum irrespective of the changes in pH from the industrialization point of view [21].
or water to seed ratio. In addition, Wu et al. [16] found At higher temperatures, the viscosity of mucilage
that the extraction temperature and time were the most decreases and makes the slurry less sticky and the muci-
important factors affecting the response variables (extrac- lage can be easily released. As a result, the mass transfer
tion yield, purity and relative viscosity of crude polysac- coefficient of the extraction process increases with tem-
charides). This result is in agreement with reports of other perature thus effecting the diffusion and viscosity. It is
authors in extracting polysaccharides [19, 20]. The extrac- found that the mass transfer coefficients increase with the
tion at the elevated temperature resulted in faster and increase in the temperature of extraction (Tables 1 and 2).
The K (h−1) value increased from 5.39 to 14.84, with Bostan et al. [6] reported the minor effect of pH on
increase in temperature from 25°C to 55°C (water/seed extraction yield of wild sage seed crude hydrocolloid and
ratio 40:1). The increase of the polysaccharides diffusion increasing the temperature and water to seed ratio
coefficient and the enhanced solubility of the polysac- increased the yield of extracted hydrocolloid due to
charides in the extracting solvent at higher temperatures enhanced mass transfer rate. The lowest yield of gum
caused the increase of the polysaccharides mass going (7.04%) was obtained at lowest water to seed ratio (25:1)
out from the mushroom particles into the solution [21]. at temperature of 52.5°C and pH of 6.0, while the highest
The extraction coefficient increased with increasing the value (12.2%) was obtained at the highest temperature
extraction temperature due to the increase of the poly- (80°C), water to seed ratio of 55:1 and pH of 6.0 [6].
saccharides solubility [22]. Tables 1 and 2 show the mass transfer coefficient (K)
values of wild sage seed extraction at water/seed ratios of
30:1 and 40:1, respectively, at different temperature and
3.3 Effect of water/seed ratio pH. The availability of high liquid content led to an
increase in the driving force of mucilage out of the
Figure 5 shows the effect of water/seed ratio and extrac- seeds into the extract. Response surface methodology
tion time on extraction of wild sage seed gum at 40°C and (RSM) was applied to optimize the extraction of crude
pH ¼ 8.5. Water to seed ratio will significantly affect polysaccharides from boat-fruited sterculia seeds by Wu
extract yield. If ratio of water to seed is too small, gums et al. [16]. They reported that extraction temperature, pH,
in wild sage seed cannot be completely extracted up. If extraction time and water to seed ratio were found to
ratio of water to seed is too big, this will cause high have a significant influence on the yield and purity of
process cost. The gum yield increased on average from the extracted crude polysaccharides.
10.52% to 11.06%, with increase in water/seed ratio from
30:1 to 40:1 under same conditions.
Sepulveda et al. [22] reported that when the volume ratio 3.4 Mass transfer within the seed
of water to seeds was increased, a greater mucilage yield
was obtained from Opuntia spp. seeds. Bendahou et al. [23] Effect of mass transfer within the seed was studied to
reported that the extraction yield of polysaccharides signifi- determine if the diffusion to the surface controls and
cantly increases as the ratio of water to seed was increased, water diffuses well into the seeds. The following data
which could be due to an increased driving force for the were used in eqs (7 and 8) in order to calculate the Thiele
mass transfer of the polysaccharides. Singthong et al. [15] modulus, density of wild sage seed: 970 kg/m3, effective
also reported a higher extraction yield for Yanang leaves diffusivity data (Table 3) and average value of seed dia-
gum at a low ratio of solid to water. meter, dp ¼ 1.32 mm.
12
10
8
Yield%
4
01:30
2 01:40
Kinetic model
0
0 10 20 30 40 50 60 70
Time (min)
Figure 5 Effect of water/seed ratio on gum extraction process at 40°C and pH ¼ 8.5
Table 3 Effective diffusivity and Thiele modulus on the internal process of wild sage seed. The values of the enthalpy
mass transfer were in the range of 0.52–14.99 kJ/mol. The value
obtained was in the range 4–13.5 kJ/mol obtained by
pH Temperature 30:1 40:1
other researches for extraction of melon, rubber seed
(°C)
Deff (m2 s−1) ϕ Deff (m2 s−1) ϕ and olive cake oil [25, 26]. Positive enthalpy change
−10 −10 indicates the endothermic nature of the extraction pro-
5.5 25 2.72 10 16.12 2.48 10 16.26
5.5 40 3.03 10−10 22.77 3.07 10−10 25.06 cess and requires energy during the process.
5.5 55 3.18 10−10 26.30 3.16 10−10 24.28 Entropy of the solution increases due to the gum
7 25 2.85 10−10 22.55 2.58 10−10 15.41 molecules extraction. The positive value of entropy change
7 40 3.07 10−10 20.97 3.12 10−10 20.43 describes the process is irreversible [27]. The values of the
7 55 3.14 10−10 24.16 3.15 10−10 24.59
entropy were in the range of 6.3–52.2 J/mol K.
8.5 25 2.34 10−10 18.56 2.54 10−10 18.20
8.5 40 2.94 10−10 24.91 2.87 10−10 23.99
The free energy values lie between 0.14 and 2.44 kJ/
8.5 55 3.16 10−10 24.82 3.22 10−10 25.17 mol. This shows that the energy required to break the
solute–solute and solvent–solvent interactions are less
than the energy released in solute–solvent interactions.
Effective diffusivity values can be strongly affected by
conditions under which the extraction process is carried
out. Temperature, for instance, was reported to signifi-
cantly increase diffusivity [24]. The results show that the 4 Conclusions
effective diffusivity values were 2.34 10−10 m2 s−1–3.22
10−10 m2 s−1. Extraction of gum from native seeds and its use in
Table 3 also represents the Thiele modulus calculate the formulation of food products has recently become
for the wild sage seed gum solution at 30:1 and 40:1 very attractive. Wild sage seed has practical amounts of
water/seed ratio at temperature 25–55°C and pH of 5.5, gum with good functional properties which is compar-
7 and 8.5. Thiele modulus ranges between 15.41 and 26.3. able with commercial food hydrocolloids. In this study
The value of Thiele modulus indicates water diffuses with the effect of extraction temperature (at three levels, 25, 40
reacting. The reaction increases the internal mass transfer and 55°C), pH (at three levels, 5.5, 7 and 8.5) and the ratio
diffusion limitation [13]. However, the system was of water to seed (at two levels, 30 to 1 and 40 to 1) on
affected by the mass transfer within the seed. This was mass transfer kinetics of wild sage seed gum extraction
due to the value of the Thiele modulus, which was >10. was studied. The results showed that increasing the tem-
perature from 25 to 55°C, increased the gum extraction
about 9.4%. With increasing the ratio of water to seed,
3.5 Thermodynamic parameters the rate of extraction of gum was also increased. The
maximum value of gum obtained from extraction of
Table 4 shows the values of equilibrium constant and wild sage seed was 12.5% at 55°C, pH ¼ 7 and water to
thermodynamic parameters for the gum extraction seed 40 to 1.
Table 4 Thermodynamic parameters for gum extraction process of wild sage seed
1:30 1:40
pH T (K) F ΔH, kJ/mol ΔS, kJ/mol K ΔG, kJ/mol F ΔH, kJ/mol ΔS, kJ/mol K ΔG, kJ/mol
5.5 298 2.57 0.57 6.30 10−3 −2.33 1.77 3.59 1.61 10−2 −1.41
5.5 313 1.72 −1.42 1.51 −1.07
5.5 328 1.73 −1.49 2.03 −1.93
7 298 1.10 14.99 5.22 10−2 −0.24 2.54 0.52 9.47 10−3 −2.31
7 313 2.23 −2.09 2.56 −2.44
7 328 1.89 −1.74 1.79 −1.58
8.5 298 1.06 13.49 4.56 10−2 −0.14 1.36 10.04 3.63 10−2 −0.77
8.5 313 1.30 −0.68 1.69 −1.36
8.5 328 1.75 −1.52 1.98 −1.87
In this study, the experimental data were fitted to a value shows that the gum extraction was affected by the
mathematical model of mass transport and equations mass transfer within the particle.
constants were obtained. The K (h−1) value varies from The ΔH, ΔS and ΔG values were 0.52–14.99 kJ/mol,
4.7 to 16.9. Statistical results indicated that the model 6.3–52.2 J/mol K and 0.14–2.44 kJ/mol, respectively,
used in this study will be able to predict the gum extrac- which show that the extraction process was spontaneous,
tion from wild sage seed adequately and is probably irreversible and endothermic based on thermodynamic
useful for other gum-containing seeds. Thiele modulus parameters.
References
1. Salehi F, Kashaninejad M, Behshad V. Effect of sugars and response surface methodology. LWT – Food Sci Technol
salts on rheological properties of Balangu seed (Lallemantia 1994;27:363–9.
royleana) gum. Int J Biol Macromol 2014;67:16–21. 15. Singthong J, Ningsanond S, Cui SW. Extraction and
2. Williams PA, Phillips GO. Introduction to food hydrocolloids. In: physicochemical characterisation of polysaccharide gum from
Phillips GO, Williams PA, editors. Handbook of hydrocolloids. yanang (Tiliacora triandra) leaves. Food Chem 2008;114:1301–7.
New York, NY: CRC Press, 2000:1–19. 16. Wu Y, Cui SW, Tang J, Gu X. Optimization of extraction process
3. Salehi F, Kashaninejad M. Effect of different drying methods on of crude polysaccharides from boat-fruited sterculia seeds by
rheological and textural properties of Balangu seed gum. response surface methodology. Food Chem 1605;2007:1599–.
Drying Technol 2014;32:720–7. 17. Eikani MH, Golmohammad F, Homami SS. Extraction of
4. Razavi SM, Mohammadi Moghaddam T, Emadzadeh B, Salehi pomegranate (Punica granatum L.) Seed oil using superheated
F. Dilute solution properties of wild sage (Salvia macrosiphon) hexane. Food Bioprod Process 2012;90:32–6.
seed gum. Food Hydrocolloid 2012;29:205–10. 18. Mazza G, Biliaderis CG. Functional properties of flaxseed
5. Farahnaky A, Shanesazzadeh E, Gh M, Majzoobi M. Effect of mucilage. J Food Sci 1989;54:1302–5.
various salts and pH condition on rheological properties of 19. Vinogradov EV, Brade L, Brade H, Holst O. Structural and
Salvia macrosiphon hydrocolloid solutions. J Food Eng serological characterisation of the O-antigenic polysaccharide
2013;116:782–8. of the lipopolysaccharide from acinetobacter baumannii strain
6. Bostan A, Razavi SM, Farhoosh R. Optimization of hydrocolloid 24. Carbohydr Res 2003;338:2751–6.
extraction from wild sage seed (Salvia macrosiphon) using 20. Yin G, Dang Y. Optimization of extraction technology of the
response surface. Int J Food Properties 2010;13:1380–92. lycium barbarum polysaccharides by box–behnken statistical
7. Pinelo M, Sineiro J, Núñez MJ. Mass transfer during continuous design. Carbohydr Polymers 2008;74:603–10.
solid– liquid extraction of antioxidants from grape byproducts. 21. Ye CL, Jiang CJ. Optimization of extraction process of crude
J Food Eng 2006;77:57–63. polysaccharides from Plantago asiatica L. By response surface
8. Amid BT, Mirhosseini H. Optimisation of aqueous extraction of methodology. Carbohydr Polymers 2011;84:495–502.
gum from durian (Durio zibethinus) seed: a potential, low cost 22. Sepulveda E, Sanez C, Aliaga E, Aceituno C. Extraction and
source of hydrocolloid. Food Chem 2012;132:1258–68. characterization of mucilage in Opuntia spp. J Arid Environ
9. Sulaiman S, Aziz AR, Aroua MK. Optimization and modeling of 2007;68:534–54.
extraction of solid coconut waste oil. J Food Eng 2013;114:228–34. 23. Bendahou A, Dufresne A, Kaddami H, Habibi Y. Isolation and
10. Liauw MY, Natan FA, Widiyanti P, Ikasari D, Indraswati N, structural characterization of hemicelluloses from palm of
Soetaredjo FE. Extraction of neem oil (Azadirachta indica Phoenix dactylifera L. Carbohydr Polymers 2007;68:601–8.
A. Juss) using n-hexane and ethanol: studies of oil quality, 24. Loncin M, Merson RL. Food engineering. Principles and
kinetic and thermodynamic. ARPN J Eng Appl Sci 2008;3:6. selected applications. New York, NY: Academic Press,
11. Palumbo SA, Komanowsky M, Metzger V, Smith JL. Kinetics of 1979:494.
pepperoni drying. J Food Sci 1977;42:1030–3. 25. Ibemesi J, Attah J. Temperature effects on the extraction of
12. Schwartzberg HG, Chao RY. Solute diffusivities in leaching rubber and melon seed oils. J Am Oil Chem Soc
processes. Food Technol 1982;36:73–86. 1990;67:443–5.
13. Giri CC, Sharma DK. Mass-transfer studies of solvent 26. Meziane S, Kadi H. Kinetics and thermodynamics of oil extraction
extraction of coals in N-methyl-2-pyrrolidone. Fuel from olive cake. J Am Oil Chem Soc 2008;85:391–6.
2000;79:577–85. 27. Amin S, Hawash G, El Diwani G, El Rafei S. Kinetics and
14. Cui W, Mazza G, Oomah BD, Biliaderis CG. Optimization thermodynamics of oil extraction from jatropha curcas in
of an aqueous extraction process for flaxseed gum by aqueous acidic hexane solutions. J Am Sci 2010;6:8.