Food Chemistry Advances 3 (2023) 100507

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Food Chemistry Advances

journal homepage: www.elsevier.com/locate/focha

Studies on the extraction of Jerusalem artichoke tuber phenolics using

microwave-assisted extraction optimized conditions
N.A. Afoakwah a, *, Y. Zhao b, W. Tchabo c, Y. Dong b, *, J. Owusu d, G.K. Mahunu a
a
Department of Food Science and Technology, Faculty of Agriculture, Food and Consumer Sciences, University for Development Studies, P. O. Box 1882, Tamale, Ghana
b
School of Food and Biological Engineering, Jiangsu University, 301 Xuefu Road, Zhenjiang 212013, China
c
Department of Food Science and Nutrition, National Advanced School of Agro-Industrial Sciences (ENSAI), University of Ngaoundere, Ngaoundere, Cameroon
d
Department of Food/Post Harvest Technology, Koforidua Technical University, Koforidua, Ghana

A R T I C L E I N F O A B S T R A C T

Keywords: Microwave-assisted extraction (MAE), which is a known method for the extraction of phenolic compounds from
Jerusalem artichoke tuber plants, was employed to extract the polyphenols in Jerusalem artichoke tuber (JAT) using response surface
Phenolics methodology optimized conditions of microwave power (MP), extraction-time (TE) and temperature (Temp). The
Antioxidant activity
MAE was used to improve polyphenols extraction yield from JAT. The ethanolic extracts of JAT obtained by MAE
Microwave-assisted extraction
Optimized-conditions
were quantitatively analyzed for total polyphenol content (TPC), total flavonoid content (TFC) 2, 2′-diphenyl-1-
picrylhydrazyl (DPPH), and ferric reducing antioxidant power (FRAP). The optimal conditions obtained were as
follows: Temp of 79.18 ◦ C, TE of 11.96 min, and MP of 13.49 W. Based on these conditions, the extraction yield
of TPC, TFC,% DPPH and FRAP could reach 4483.33 mg GAE/kg, 2731.59 mg RE/kg, 82.69 % and 2.65 mmol/L
respectively with a predicted general-desirability value of 0.82. DPPH (r = 0.972) and FRAP (r = 0.982)
significantly (p < 0.05) correlated to TPC suggesting that TPC was the main phenolic contributing to the anti­
oxidant activity. The extraction yield recorded was higher than that of the liquid and ultrasound extraction
methods.

1. Introduction polyphenol–extracts and their antioxidant- capacity depends not only on

Jerusalem artichoke is an agricultural-industrial crop cultivated in
cooler to warmer climates with its tubers found in Europe, North
America, and Asia (Slimestad et al., 2010). The tubers are a potential
source of biomass and a health-promoting food source. Inulin is the main
stored carbohydrate reserve, not starches (Afoakwah et al., 2022;
Afoakwah & Mahunu, 2022). In addition, it is a source of fructose syrups
for the food–industry, more so, its fructans are used for medical purposes
(Afoakwah & Mahunu, 2022; Huang et al., 2012). However, the con­
sumption of Jerusalem artichoke tuber as a pickle or vegetable salad is
becoming popular in China and other parts of the Asian continent partly
because of documented affirmation of its health-beneficial properties
(Afoakwah, 2022) as well as its biologic actions (Afoakwah et al., 2022).
Jerusalem artichoke has a huge dietary and industrial impact,
particularly in the food and pharmaceutical industry, and the present
awareness of the health property of Jerusalem artichoke (Afoakwah
et al., 2022) has motivated the development of innovative extraction
methods for its phenolic compounds-fractions. Undeniably, the value of
the quality of the starting-biomass but on the hi-tech processes involved
during extraction (Li et al., 2013).
Nowadays, a variety of extraction–techniques has been introduced
and studied; nearly all were noted to enhance–efficiency, extrac­
t–quality, extraction-time and solvent- consumption. The promising
method of extraction available are microwave–assisted extraction
(MAE) (Song et al., 2011), ultrasound–assisted–extraction (UAE) (Car­
rera et al., 2012), supercritical–fluid–extraction (Akalın et al., 2013) and
pressurized solvent-extraction (Xiao et al., 2012). MAE in particular has
drawn major research attention in different fields, such as recuperating
of active–ingredients from plant resources. The main advantages of MAE
are the significant–reduction of extraction time compared to conven­
tional solvent–liquid extraction and higher yield of active–substances
(Chan et al., 2011). Several factors (extraction time, temperature, sol­
vent type microwave power and their interactions) have influence on
MAE. As a result, an optimization studies were used for determination of
the optimal operating-conditions using the Response surface method­
ology (RSM) as a statistical tool to generate appropriate quantitative

* Corresponding authors.
E-mail addresses: nafoakwah@uds.edu.gh (N.A. Afoakwah), ydong@ujs.edu.cn (Y. Dong).

https://doi.org/10.1016/j.focha.2023.100507
Received 30 June 2023; Received in revised form 23 October 2023; Accepted 28 October 2023
Available online 29 October 2023
2772-753X/© 2023 The Authors. Published by Elsevier Ltd. This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/).
N.A. Afoakwah et al.
data. The RSM was chosen because it generates a mathematical-model
by taken into account the potential interrelationships among the vari­
ables tested while reducing experimental runs (Song et al., 2011). This
was achieved by employing the Box–Behnken design (BBD) during the
experimental planning, because BBD is among the efficient experimental
methods, and has an advantage for not containing combinations for
which the factors are at the same time being high or at their lowest
levels.
To the best of knowledge, no reports exist on the optimization of
MAE for the extraction of phenolic-compounds from Jerusalem arti­
choke tuber. The objectives of the current study were to investigate, in
the first approach, the effect of temperature, extraction time, and mi­
crowave power as variables on the MAE of Jerusalem artichoke tuber
extract in regards to its phenolic profile such as total phenolic content
(TPC) total flavonoid content (TFC), as well as its antioxidant activity in
terms of 2, 2′-diphenyl-1-picrylhydrazyl (DPPH) radical scavenging ac­
tivity and ferric reducing antioxidant power (FRAP). Further, the study
determined the optimal operating conditions of MAE for the processing
of a rich phenolics Jerusalem artichoke tuber extract with high antiox­
idant properties by means of the response surface methodology. More­
over, the efficiency of MAE was assessed with respect to one
conventional (liquid) and advance (ultrasound) extraction techniques.
2. Experimental
2.1. Sample material and chemical
Tubers of Jerusalem artichoke cultivated in Zhenjiang area of
Jiangsu province in China were obtained during the winter season from
growers. The tubers of Jerusalem artichoke were, washed placed in an
ice-box, and instantly frozen upon-arrival at the laboratory within 1 h of
collecting. The tubers were packed in polythene-bags and kept at − 18 ◦ C
until analysis, which was approximately 6 days. Acetone, formic acid,
methanol, Gallic acid, ascorbic acid and FeCl3 were obtained from
Sinopharm Chemical Reagent (Shanghai, China). TPTZ (2,4,6-tripyr­
idyl-s-triazine), Folin-Ciocalteau and 2, 2-diphenly-1- picrylhydrazyl
(DPPH) were obtained from Sigma (St. Louis, MO, USA). All other
analytical grade chemicals were obtained from Sinopharm. (Shanghai,
China).
2.2. Experimental procedures
2.2.1. Microwave Assisted Extraction (MAE)
Microwave Assisted Extraction (MAE) open vessel technique was
employed using Discover® System S-Class (CEM Cooperation, Smith
Farm Road, Mathews. USA.). On the basis of premilitary laboratory
experiments, a sample of 20 ± 0.001 g of the homogenized Jerusalem
artichoke tuber was mixed with 30 mL of 60 % aqueous ethanol as
solvent and placed into a 50 mL round bottomed flask. A magnetic stirrer
was placed into the round bottomed flask. The round bottomed flask was
placed into the vessel stand of the Teflon tubing. After MAE, the mixture
was centrifuged (5920 g for 30 min) with a Anke GL-20B centrifuged
(Shanghai Anting Scientific Instrument Factory, Shanghai, China), and
the supernatant was concentrated on a rotary evaporator under reduced
pressure at 35 ◦ C.
2.2.2. Liquid extraction
A liquid extraction technique was carried out using acetone-
methanol-water-formic acid (Oszmianski et al., 1988; Youdim et al.,
2002) with slight modifications. In brief, Jerusalem artichoke tuber (20
± 0.001 g) was blend with 50 mL of methanol (40 % v/v), acetone (40 %
v/v), water (20 % v/v) and formic acid (0.1 % v/v) for 5 min. The ho­
mogenates were filtered with filter cloth, and the extract was recovered
as described for MAE.
2
Food Chemistry Advances 3 (2023) 100507
2.2.3. Ultrasound extraction
A ultrasound extraction technique was carried out using ethyl ace­
tate–methanol as solvent (Tchone et al., 2006) with slight modifications.
In brief, fresh tubers (20 ± 0.001 g) were homogenized in a warring
blender with 30 mL of ethyl acetate–methanol for 5 min. The beaker of
the blender was rinsed by adding 10 mL of ethyl acetate–methanol 1:1
(v/v). The homogenate was placed in a treatment chamber of an ultra­
sound equipment (Wuxi Fanbo Biological Engineering, Wuxi, China) set
as a power of 60 W, with pulse durations of 10 s on and 5 s off for 10 min
at a frequency of 28 kHz, with constant temperature of 80 ◦ C. Afterward,
the supernatant obtained after centrifugation (at 5920 g for 30 min) was
kept at 4 ◦ C. The resultant residue was mixed with an additional 30 mL
of extracting solvent and treated as described above. The second residue
was treated in the same way, but using 10 mL of extracting solution. The
extracts were then combined and collected as described for MAE.
2.2.4. Experimental design and data analysis
A 3 level 3 factor Box Behnken-design (BBD) was chosen to evaluate
the effect of MAE on total phenolic, total flavonoid DPPH and FRAP on
Jerusalem artichoke tubers extract (JAE). Following preliminary
extraction through a single factor experiment, Extraction-temperature
(X1), extraction-time (X2) and microwave power (X3) were selected as
the independent variables (supporting result 1). The results of the BBD
experiments as presented as (supporting result 2) were analyzed by the
multiple regression Eq. (1)
∑
3 ∑
3 ∑
2 ∑
3
Y = β0 + β i Xi + βii Xi2 + βij Xi Xj (1)
i=1 i=1 i=1 j=i+1
Y is responses, β0, βi, βii and βij are coefficients-constant of the intercept,
linear, quadratic and interaction terms correspondingly; Xi and Xj are
coded-independent variables of temperature (X1), extraction time (X2),
and microwave power (X3). All the runs were carried out in triplicate,
and the mean results were reported. Design Expert Statistical Software
package 8.0. (Stat Ease, Minneapolis, USA) was used for the data anal­
ysis. The adequacy of the model was confirmed by Fisher’s F test at 5 %
of significance. The predictive potential of the model is explained by it
co-efficient of determination (R2). The analysis of variances (ANOVA)
was employed to examine the fitted-model. The confidence-level of 95 %
was used as the level of significance of the model. The lack-of-fit is
significant at p < 0.05 showing the adequacy of the quadratic-model
chosen.
2.3. Analytical methods
2.3.1. Determination of total polyphenol content
The total phenolic content was performed using the Folin–Ciocalteu
reagent with gallic acid as a standard as described by Hossain et al.
(2013). Briefly, 0.1 mL of extract was mixed with Folin–Ciocalteu re­
agent (0.5 mL) and 5 mL distilled water. It was vortex for 2 min and 5 %
w/v of sodium carbonate solution (0.75 mL) was then added. The
samples were allowed to incubate at room for 2 h. Absorbance was read
using Rayleigh UV–Vis Spectrophotometer 9600 (Shanghai, China) at
765 nm. Results were presented in mg gallic acid equivalent (GAE)/kg.
2.3.2. Determination of total flavonoid content
The determination of the total flavonoid content (TFC) was carried
out using the method described by Hossain et al. (2013). The 0.1 mL
extract was added to distilled water (3 mL) followed by 1.5 mL of NaNO2
(0.05 % w/v). The mixture was made to stand for 6 min, 1 mL of NaOH
(1 M) was then added and after 30 min at room temperature Rayleigh
UV–Vis Spectrophotometer 9600 (Shanghai, China) was used to deter­
mine the absorbance at 510 nm. Results were presented as
rutin-equivalent (RE) /kg.
N.A. Afoakwah et al. Food Chemistry Advances 3 (2023) 100507

2.3.3. Determination of antioxidant activity
2.3.3.1. DPPH radical scavenging activity assay. The 2, 2′-diphenyl-1-
picrylhydrazyl (DPPH) free radical scavenging capacity of the Jerusalem
artichoke tuber extract was determined according to Amarowicz et al.
(2020). DPPH radical solution (1 mL of 0.2 mM) was mixed with 50 µL of
extract, 3.95 mL methanol was added in a test tube. The content in the
test tube was mixed and kept for 30 min in the dark at 27 ◦ C. Rayleigh
UV–Vis Spectrophotometer 9600 (Shanghai, China) was used to quan­
tify the absorbance at 517 nm after 30 min. Methanol was used as a
blank, and the control sample prepared in a similar way except using 50
µL distilled water in place of the extract. The scavenging ability of DPPH
radical was calculated using the following equation:
Inhibition (%) = [(X0 − − X1 ) / X0 ] X 100
The model adequacy-output (Table 1) revealed that, quadratic-
model was very significant (P˂0.0001) for the extraction of all the
phenolic-compounds from JAE. In addition, the quadratic-model
“adjusted R2” as well as, “predicted R2-values were higher than 0.999.
The model fitness adequacy showed a high correlation between the
predicted and the actual (supporting result 3). The interaction-terms of
the model (X1×2, X1×3 and X2×3), the coefficients of the intercept,
linear (X1, X2, X3), and quadratic (X11, X22 and X33) were determined by
least square-technique. The linear, quadratic or interaction-coefficients
effects on the response were tested for significance using analysis of
variance (ANOVA). The significance-level pertaining to the factors are
represented by p-value (Table 1). Moreover, the lack of fit of the model
was non-significant (p > 0.05), signifying the model was satisfactorily
precise for predicting the suitable responses.
(2)

X0 is the absorbance of control and X1 is the absorbance of the tested
sample
2.3.3.2. FRAP method. The ferric reducing antioxidant power (FRAP)
assay was performed according to the FRAP technique as described by
Davey et al. (2000). The FRAP reagent consisted of acetate buffer (0.3
mol/l), TPTZ (10 mmol/l) and FeCl3⋅6H2O (20 mmol/l) in the ratio
10:1:1. 100 μl of JA extract were mixed with 3.0 mL of the FRAP reagent
and allowed to stand at in the dark for 30 min at 37 ◦ C. The absorbance
was read at 595 nm using a Rayleigh UV–Vis Spectrophotometer 9600
(Shanghai, China). Ferrous sulfate was used as a standard, and the re­
sults were expressed in mmol of Fe2+ per liter.
3. Results and discussion
The experimental design was 17 runs with 5 replications at central
points to assess the pure-error (supporting result 2).
3.1. Response surface analysis of total phenolic content
Total phenolic content (TPC) was influenced by linear (X1, X2 and X3;
p < 0.0001), interactive (X1×2 and X2×3; p < 0.05) and quadratics (X11,
X22 and X33; p < 0.0001) terms as shown in Table 2. The optimal-
conditions for extracting phenolic-compounds generated through Eq.
(2) were predicted to be: temperature (Temp) of 71.54 ◦ C, microwave
power (Mp) of 11.18 W, and extraction time (TE) of 12.31 min. Under
these conditions, TPC was achieved at 4544.6 mg GAE/kg. However, the
3D surface-plots (Fig. 1A) showed that TPC of the JA extract increased
significantly between temperature of 50–78.5 ◦ C, but with further in­
crease in temperature to about 110 ◦ C the total phenolic content
decreased. Suggesting that, higher temperature during extraction leads
to thermally induced phenolic degradation. This can be linked to high
temperature (80–110 ◦ C) provoking competing-processes like decom­
position and epimerization (Vuong et al., 2013), but mild (50–78.5 ◦ C)
extracting Temp and a TE of about 12.5 min might make softer the

Table 1
Summary of the statistical analysis of the tested models.
Source Sum of squares DF Mean square F value Prob > F Std. Dev. R2 Adjusted R2 Predicted R2 PRESS Remarks

TPC (mg GAE/kg)

Mean 2.436E+008 1 2.436E+008
Linear 1.081E+006 3 3.602E+005 0.83 0.5021 659.88 0.1603 − 0.0335 − 0.3709 9.242E+006
2FI 3920.90 3 1306.97 2.310E-003 0.9998 752.12 0.1609 − 0.3426 − 1.7035 1.823E+007
Quadratic 5.656E+006 3 1.885E+006 11,093.11 < 0.0001 13.04 0.9998 0.9996 0.998 13,325.37 Suggested
Cubic 794.22 3 264.74 2.68 0.1825 9.94 0.9999 0.9998 Aliased
Residual 395.38 4 98.85
Total 2.504E+008 17 1.473E+007
TFC (mg RE/kg)
Mean 1.165E+008 1 1.165E+008
Linear 1.738E+007 3 5.794E+006 36.27 < 0.0001 399.65 0.8933 0.8687 0.7911 4.064E+006
2FI 1.300E+006 3 4.332E+005 5.58 0.0164 278.70 0.9601 0.9361 0.8552 2.818E+006
Quadratic 7.728E+005 3 2.576E+005 455.43 < 0.0001 23.78 0.9998 0.9995 0.9972 53,734.67 Suggested
Cubic 3293.38 3 1097.79 6.59 0.0500 12.90 1.0000 0.9999 Aliased
Residual 666.00 4 166.50
Total 1.360E+008 17 7.998E+006
DPPH (%)
Mean 6.00E+04 1 6.00E+04
Linear 1.11E+03 3 3.69E+02 0.61 0.6215 24.63 0.1230 − 0.0793 − 0.4971 1.35E+04
2FI 2.12E+02 3 7.05E+01 0.09 0.9628 27.70 0.1466 − 0.3655 − 1.9773 2.68E+04
Quadratic 7.49E+03 3 2.50E+03 94.02 < 0.0001 5.15 0.9793 0.9528 0.7235 2485.615 Suggested
Cubic 152.08 3 50.69 6.01 0.0579 2.90 0.9962 0.9850 Aliased
Residual 33.723 4 8.43
Total 6.90E+04 17 4.06E+03
FRAP (mmol/L)
Mean 61.70 1 61.70
Linear 0.70 3 0.23 0.46 0.7155 0.71 0.0958 − 0.1128 − 0.4800 10.76
2FI 0.07 3 0.022 0.035 0.9909 0.81 0.1051 − 0.4319 − 1.8824 20.95
Quadratic 6.44 3 2.15 242.13 < 0.0001 0.09 0.9915 0.9805 0.9632 0.27 Suggested
Cubic 0.01 3 3.93E-003 0.31 0.8167 0.11 0.9931 0.9723 Aliased
Residual 0.05 4 0.013
Total 68.97 17 4.06

Abbreviations are defined in Section 2: Total phenolics content (TPC), Total flavonoids content (TFC), 2, 2′-diphenyl-1-picrylhydrazyl (DPPH), Ferric reducing ability
potential (FRAP) and Degree of freedom (DF).

3
 N.A. Afoakwah et al. Food Chemistry Advances 3 (2023) 100507

plant-tissue, weaken the cell-wall integrity, hydrolyze the bonds of

<0.0001*

<0.0001*
bound-phenolic-compounds, and enhance phenolics-solubility. Hence,

0.00021*
0.0001*
0.0058*

0.0346*

0.0002*
P-Value

0.1079

0.4931
0.6463

0.8167
more phenolics might distribute to the extracting solvent (Choudhary
et al., 2021; Alara & Abdurahman, 2019). However, increase in TE
caused a decrease in TPC. This might be associated with longer duration
of extraction leading to polyphenols disintegration (Tomasi et al., 2023).
Sum of squares

Microwave output power level had a significant effect (p < 0.05) on

7.21E+00

5.50E+00

7.27E+00
5.30E-01
1.36E-01
3.01E-02

6.07E-02
4.64E-03
2.04E-03

4.27E-01
1.70E-02
6.21E-02
1.18E-02
5.03E-02
the TPC content depending on the temperature. It is important to note
that, microwaves power between 10.0 to about 12.5 min and time of
12.50 min had a positive effect on TPC, which could be associated with
FRAP (mmol/L)

less microwave irradiation time and Mp. In this study, application of a

Coefficient

low-microwave power and a short TE was able to extract phenol from

0.9915
0.9805

27.307
their plant materials. However, other authors combined moderate Mp
− 0.26
− 0.13
− 0.61

− 0.12
− 0.34

− 1.14
− 0.32
− 0.20
0.023
2.69

4.94
with longer time of extraction and realized it was more effective for

Total phenolics content (TPC), Total flavonoids content (TFC), 2, 2′-diphenyl-1-picrylhydrazyl (DPPH) Ferric reducing ability potential (FRAP) and Degree of freedom (DF).
extracting phenolic-compounds (Jokić et al., 2012). Ballard et al. (2010)
reported an increase in extraction efficiency with an increase in TE when
<0.0001*

<0.0001*
0.0010*
0.0288*

0.0308*

0.0438*
0.0331*
P-Value

0.0719

0.6384
0.5187

0.0579

50 % Mp was employed. Though, no prior reports linking to the opti­

mization of this extraction parameter for Jerusalem artichoke tuber was
found. Ballard et al. (2010) reported the effect of MAE on geniposidic
and chlorogenic- acids from E. ulmodies, and indicated that at an
Sum of squares

extraction-time of 10 s, the extraction value of geniposidic-acid was

8.80E+03

7.87E+02
2.00E+02
1.19E+02

1.93E+02
6.40E+00
1.23E+01

6.84E+03
1.60E+02
1.86E+02
1.86E+02
1.52E+02
3.37E+01
8.99E+03

considerably high at 90 %. Nepote et al. (2005) established that TE had a

significant influence on the phenolic-compounds extraction whereas
Alu’datt et al. (2011) showed that prolong TE, total phenolic-compounds
extracted are improved.
Coefficient
DPPH (%)

− 40.29

YTPC = 4536.87 − 313.18X1 − 149.12X2 − 121.53X3 − 20.77X1 X2

0.9793
0.9528

17.290
− 9.92
− 5.00
− 3.86

− 6.95
− 1.27

− 6.16
− 6.65
84.39

1.75

8.67

− 1075.08X12 − 322.50X22 − 188.89X32 (3)

3.2. Response surface analysis of total flavonoid content

<0.0001*

<0.0001*

<0.0001*

<0.0001*
<0.0001*
<0.0001*

<0.0001*
0.0003*

0.0378*
0.0006*
P-Value

0.0500
ANOVA and regression coefficients of the second-order polynomial model for the response variables (actual values).

The effect of TE, Temp, and Mp conditions in MAE on TFC was

studied. Flavonoids are among the major compounds found in the ex­
tracts of Jerusalem artichoke phenolic-extracts. As reported by Heim
Sum of squares

et al. (2002), they have an effect on antioxidant-capacity of plant ex­

1.95E+007

1.00E+007

7.33E+006

3.89E+005
9.10E+005

7.24E+005

1.95E+007

tracts. Table 2 depicts the linear-term of Temp (p < 0.0001), TE (p <

248.12

369.12
201.93
396.38
329.38
666.00

0.001) and Mp (p < 0.0001), which showed a significant outcome on

11.51

flavonoid total content of the extracts. Besides, the interaction between

TFC (mg RE/kg)

Temp and TE (X1×2), interaction between Temp and Mp (X1×3), and

between Temp and Mp (X2×3) indicated a significant (p< 0.0001) effect
Coefficient

− 477.02
2376.22

1119.47

227.703

on TFC. More so, the quadratics of Temp (p < 0.0001), TE (P < 0.05) and
957.25

312.01

414.78

0.9998
0.9995
− 1.70
55.69

29.62
69.09

0.91

Mp (p < 0.001) had a significant influence on the TFC. Applying the

studied-parameters, the TFC of JA extracts ranged from 288.87 to
4477.27 mg RE/kg as shown in Table 1. While the optimal conditions for
<0.0001*

<0.0001*
<0.0001*
<0.0001*

<0.0001*
<0.0001*
<0.0001*

flavonoid content calculated from the quadratic model of TFC (Eq. (4))
0.0153*
0.0171*
P-Value

0.1149

0.8998

were determined at Temp of 109.7 ◦ C, Mp of 14.40 W, TE of 14.20 min,

with predicted-flavonoid content of 4560.98 mg RE/kg. The surface
plots (Fig. 2) showed that total flavonoid content in the extracts
Sum of squares

increased-linearly with an increase in Temp, as well as, with an increase

6.86E+006

7.85E+005
1.78E+005
1.18E+005

4.79E+006
4.17E+005
1.38E+005

6.87E+006

in Mp and TE. As depicted in Fig. 1A and 1B, increasing extraction

temperature may promote solvent-extraction by enhancing both
173.99
164.30
550.61

644.26
794.22
565.04

diffusion-coefficients and the solubility of flavonoid content. Moreover,

TPC (mg GAE/kg)

at higher temperature flavonoid molecules diffuse quickly from the cells

into the extracting agent (Liu et al., 2010). In addition, long duration of
Coefficient

− 1075.08
− 313.18
− 149.12
− 121.53

− 322.50
− 188.89

extraction time at high Mp causes a release in TFC (Fig. 1C). As reported

4536.87

− 20.77
− 20.28

0.9991
0.9979

80.816
11.73

by Wang et al. (2010) microwave-irradiation offers a rapid-transfer of

0.80

indicate 5 % significance level.

energy to the solvent and matrix. That leads to the disruption of

hydrogen-bonds of the raw material and promote the circulation of the
DF

16

solvent. The predicted-equation for the response-surface was deter­

9

1
1
1

1
1
1

1
1
1
7
3
4

mined as a result of the second-order equation shown below:

Adequate precision

YTFC = 2376.22 + 1119.47X1 + 55.69X2 + 957.25 X3 + 312.01X1 X2

− 477.02X1 X3 + 414.78X12 + 29.62X22 + 69.09X32 (4)
Interaction
X1 (Temp)

Pure error
Lack of fit
Quadratic

Residual
X2 (TE)
X3 MP)
Table 2

Source

Adj-R2
Linear
Model

C.V.%
Total
X1×2
X1×3
X2×3

X11
X22
X33

R2

4
N.A. Afoakwah et al. Food Chemistry Advances 3 (2023) 100507

Fig. 1. Response surface plots showing the effect of (A) extraction time (TE) and temperature (Temp); (B) microwave power (Mp) and temperature (Temp); (C)
microwave power (Mp) and extraction time (TE) on total phenolic content (TPC).

3.3. Response surface analysis of antioxidant activity
Polyphenols contents of plants are studied together with its
antioxidant-activity as it enables the elucidation of the antioxidant ca­
pabilities (DPPH and FRAP) of the investigated plant (Kurilich et al.,
2002). The total antioxidant activity (TAC) response of JA extracts ob­
tained by MAE were found to be varied from 20.20 to 88.95 % for DPPH
and 0.75 to 2.85 mmol/L for FRAP (supporting result 2), these were
dependent on the range of the investigated parameter selected. The
ANOVA revealed that, the linear-terms of X1 and X2, interaction terms
(XIX2) and the quadratics-terms were significant (p < 0.05) for both
DPPH and the FRAP of the JA extracts. As illustrated in (Fig. 3A and
supporting result 4), the response-surface plots showed that, TAC
value increased with an increase in TE from 10 min to 12.5 min. Further
increase in TE caused a decline in the TAC value. This result could be
attributed to the degradation of TPC as reported in Fig. 1A. It should be
noted that, the TAC value increased by way of elevating Temp up to
about 80.0 ◦ C, though additional temperature reduced the TAC value.
This result is consistent with previous reports, where the optimum TAC
of the plants extracts was obtained at temperatures below 80 ◦ C (Wan
et al., 2011). The optimal-condition for% inhibition DPPH value and
that of FRAP was predicted to be achieved as follows: Temp (77.52 ◦ C;
77.01 ◦ C), TE (11.48 min; 12.02 min) and Mp (11.66 W; 12.11 W). Based
on the second-order polynomial model (Eqs. (5) and(6)), the predicted%
inhibition DPPH was found to be 86.47 % and the FRAP was 2.72
mmol/L. The interaction effect X1×2 (p < 0.05) on TAC was found to be
similar to those of the TPC. The results obtained proved that the TAC of
the extracts was directly related to the TPC in the JA extracts (Fig. 4). As
depicted, in Fig. 4(B) FRAP of the JA extracts was more correlated (R =
0.989) to the TPC as compared to that of DPPH (r = 0.972) in the ex­
tracts (Fig. 4A). This suggested that TPC was the main phenolic com­
pounds, which contributed to the total antioxidant activity of the JA
extract. This finding is in line with earlier reports (Pavlović et al., 2013).
The second-order polynomial equation of DPPH is:
YDPPH = 84.39 − 9.92X1 − 5.00X2 − 6.95X1 X2 − 40.29X12 − 6.16X22
− 6.65X32 (5)
and that of FRAP was YFRAP = 2.69 − 0.26X1 − 0.13X2 − 0.12X1 X2
− 1.14X12 − 0.32X22 − 0.20X32 (6)
3.4. Optimization of the extraction parameters
The optimal condition of MAE extraction was selected to get the
highest content on total phenolic, flavonoid and antioxidant content.
These optimal conditions are Temp of 79.18 ◦ C, TE of 11.96 min and MP
of 13.49 W. Based the optimum conditions the maximum values of TPC
= 4483.33 mg GAE/kg, TFC = 2731.59 mg RE/kg DPPH = 82.69 % and
FRAP =2.65 mmol/L was predicted with general-desirability value of
0.82 (supporting result 5).

5
N.A. Afoakwah et al.
Fig. 2. Response surface plots showing the effect of (A) extraction time (TE) and temperature (Temp); (B) microwave power (Mp) and temperature (Temp); (C)
microwave power (Mp) and extraction time (TE) on total flavonoid content (TFC).
3.5. Validation of the predictive model
Three experiments were performed using the optimal conditions
with a slight modification taking into consideration the possibility in
production. Temp of 80 ◦ C, TE of 12 min and MP of 14 W were used to
validate the appropriateness of the model to predict the optimum re­
sponses. The experimental results were as follows TPC = 4419.65 ± 104
mg GAE/kg, TFC = 2902.13 ± 67 mg RE/kg, DPPH = 81.95 % and
FRAP = 2.32 mmol/L. Non-significant difference (p > 0.05) was
observed between the experimental and predicted values demonstrating
that, the model was acceptable and precise to predict the responses.
3.6. Comparison between MAE and others extraction methods
Jerusalem artichoke tuber polyphenols were extracted using liquid
and ultrasound extraction techniques as well as by the optimized MAE
method for phenolic, flavonoid, FRAP and DPPH on MAE extraction
effectiveness. The total phenolic of the Jerusalem artichoke tuber ex­
tracts were around 2316.16 ± 0.151 mg GAE /kg, 1199.02 ± 0.11 mg
GAE/Kg, and 4419.65 ± 0.11 mg GAE /kg for Ethyl acetate–methanol
1:1(v/v) extraction, Acetone: methanol: water: formic acid extraction
and MAE, respectively. The results of the total phenolic are presented in
the following order MAE > Ethyl acetate–methanol 1:1(v/v) > Acetone:
6
Food Chemistry Advances 3 (2023) 100507
methanol: water: formic acid extraction. The phenolic contents in the
various extraction methods varied significantly. The value of the TFC of
MAE was around 2902.13 ± 0.25 mg RE/kg, followed by Ethyl aceta­
te–methanol 1:1(v/v) extraction (2182.04 ± 1.90 mg RE/kg) and
Acetone: methanol: water: formic acid extraction (1082.11 ± 0.25 mg
RE/kg). With regards to the DPPH of the JA extracts the following order
was observed: MAE (81.95 %) > ethyl acetate–methanol 1:1 (v/v) ex­
tractions (74.05 %) > Acetone: methanol: water: formic acid extraction
(63.06 %). The following was noted for the FRAP of the JA extracts MAE
(2.32 mmol/L) > ethyl acetate–methanol 1:1 (v/v) extractions (1.02
mmol/L) > Acetone: methanol: water: formic acid extraction (0.95
mmol/L). Moreover, comparing DPPH inhibition potential, with that of
solvent extraction methods using a concentration range of 0.1 to 20 mg/
mL, as expected, MAE extracts showed a higher scavenging ability to
free DPPH-radicals than that of the extracts obtained from the liquid and
ultrasound extraction techniques. The results reported here indicated
that MAE was more capable of extracting Jerusalem artichoke tuber
polyphenols as compared with that of the liquid and ultrasound
extraction techniques (supporting result 6). Salerno et al. (2014) re­
ported that MAE was capable of extracting polyphenols from plant ex­
tracts even when the conventional-extraction time was extended. Zhang
et al. (2008) reported similar results and revealed that MAE was more
effective compared with a conventional technique. Through the
N.A. Afoakwah et al.
Fig. 3. Response surface plots showing the effect of (A) extraction time (TE,) and temperature (Temp); (B) microwave power (Mp) and temperature (Temp); (C)
microwave power (Mp,) and extraction time (TE,) DPPH (2,2-Diphenyl-1-picrylhydrazyl) radical scavenging activity.
utilization of MAE, (Proestos & Komaitis, 2006) extracted phenolic
compounds from aromatic plants employing various solvents. Their
findings revealed that MAE extraction resulted in a higher yield
compared to conventional extraction methods. Furthermore, Laghari
et al. (2011) conducted a study on the extraction, identification, and
antioxidative activities of flavonoids present in the leaves and flowers of
Cassia angustifolia. They employed five distinct techniques for flavonoid
extraction, including MAE, Soxhlet extraction, sonication extraction,
marinating extraction, and reflux condensation extraction. When
various extraction techniques were compared for their ability to extract
total flavonoid content, MAE method emerged as the superior choice.
This method proved to be more effective in terms of both the quantity of
flavonoids extracted and their antioxidant activity. In a study by Yuan
et al. (2018), four commercial brown macroalgae species underwent
phenolic compound extraction using MAE at 110 ◦ C for 15 min. The
results indicated that compared to traditional extraction carried out at
room temperature for 4 h, the compounds extracted via MAE exhibited
higher antioxidant activity and total phenolic content across all algae
species (Yuan et al., 2018). In a comparison of MAE and Soxhlet
extraction for the extraction of phenolic compounds from V. amygdalina
leaves, Alara et al. (2018) discovered that MAE provided a better
extraction yield in a significantly shorter time frame. While Soxhlet
extraction took 480 min to complete, MAE achieved a TPC of 73.54 mg
gallic acid equivalent per gram of dry weight (mg GAE/g d.w) in just 10
min. Furthermore, Choudhary et al. (2021) found that the MAE method
7
Food Chemistry Advances 3 (2023) 100507
outperformed the conventional approach, which involved using a tem­
perature of 50 ◦ C for 18 min to extract plant phenolics from Chenopo­
dium album. Additionally, Kaderides et al. (2019) utilized MAE on
pomegranate peels, resulting in a TPC of 199.4 mg GAE/g with an
extraction duration of just 4 min. The justification of MAE’s high
extraction output could be due to the microwave irradiation-mechanism
(Afoakwah et al., 2012). Microwaves cause rise in temperature in
plant-tissue, which leads to their disintegration and consequently to the
movement of phenolic-compounds to the extracting solvent.
4. Conclusions
In this work, we demonstrated that the tubers of Jerusalem artichoke
are potential-source of polyphenols. Using the Box-Behnken response
surface methodology, a second order statistical-models was developed,
which offered an acceptable explanation of the results. The multiple
regression analyses revealed that TPC in the JA extract was affected by
temperature, extraction time, and microwave power. The same studied
parameters influenced the TFC, DPPH, and FRAP. The optimum condi­
tions, for obtaining higher extractability of polyphenols, and antioxidant
activity were Temp of 79.18 ◦ C, TE of 11.96 min, and MP of 13.49 W.
These conditions give the basics for extracting natural anti-oxidants
from Jerusalem artichoke tuber. In addition, comparing the liquid and
ultrasonic extraction methods with that of the MAE method, the MAE
gave a higher total yield of antioxidants. The use of MAE might be of
N.A. Afoakwah et al. Food Chemistry Advances 3 (2023) 100507

Fig. 4. Correlations between responses: (A) total phenolic content (TPC) and DPPH radical scavenging activity; (B) total polyphenol content and FRAP; (C) DPPH
radical scavenging activity and FRAP.

immense interest to the food and pharmaceutical industries since it is Declaration of Competing Interest
environmentally-friendly and has the potential for higher extraction
yields. The authors have declared no conflict of interest.
Even while conventional procedures are still in use, they have some
drawbacks, such as recovering only small yields, using more extraction Data availability
solvents, taking longer to extract, and producing a large number of
residues. These had sparked the development of unorthodox methods, Data will be made available on request.
such as MAE, to get beyond the limitations of traditional methods. The
demand for novel bioactive substances will increase due to the signifi­
cance of phenolic compounds to humanity, which will further stimulate Acknowledgment
the quest for inventive extraction methods to provide significant re­
covery yields from plant sources. This work was funded by 2012 Agricultural Sci-Tech project of
Zhenjiang (No.: NY2012015) and the Senior Talent Special Fund of
Jiangsu University (No.:1 28136002).

8
N.A. Afoakwah et al.
Supplementary materials
Supplementary material associated with this article can be found, in
the online version, at doi:10.1016/j.focha.2023.100507.
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