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Gianna Et Al-2012-International Journal of Food Science & Technology
Gianna Et Al-2012-International Journal of Food Science & Technology
Original article
Impact of several variables on the microwave extraction of
Chenopodium Quinoa willd saponins
Vicente Gianna,1,2 Juan Manuel Montes,1 Edgardo Luis Calandri1,2 & Carlos Alberto Guzman2,3
1 School of Chemical Engineering. FCEFyN. UNC, Velez Sarseld Av. 1611., 5015 Cordoba, Argentina
2 Institute of Science and Food Technology. FCEFyN. UNC, Velez Sarseld Av. 1611., 5015 Cordoba, Argentina
3 National Council of Scientic and Technical Research (CONICET), Velez Sarseld Av. 1611., 5015 Cordoba, Argentina
(Received 25 August 2011; Accepted in revised form 23 February 2012)
Summary
Despite their possible applications in diverse elds, saponins are still considered to be industrial waste. The
use of saponins, however, would make seed processing more protable and reduce the pollution of
watercourses. In this work, the microwave extraction method of Chenopodium quinoa Willd saponins was
investigated. The eects of variables such as temperature, time of microwave application, solvent
composition and solvent mass seed ratio were investigated. Solvent mixtures (ethanolwater and
isopropanolwater) were used for the extraction. The Taguchi design methodology was employed to
determine the number of experiments and the optimal conditions for dierent extractions. The eciency of
each assay was determined and the results agreed with the best conditions provided by the Taguchi
experimental design for both solvent mixtures. The isopropanolwater mixture eciency was 91.8% in one
extraction step, and for ethanolwater mixture, it was 57.1%, clearly showing the advantage of the rst one.
Keywords
Introduction
doi:10.1111/j.1365-2621.2012.03008.x
2012 The Authors. International Journal of Food Science and Technology 2012 Institute of Food Science and Technology
1593
1594
The eect of water decit level on saponin composition of quinoa was determinate in a eld experiment
conducted in Mexico. The experiment took place during
the development of Sajama and Chucara cultivars. The
saponin content increases during branching, panicle
initiation and in blooming, followed by a decrease
during the grain lling stage, when the plants under
medium water decit recorded the highest saponin
content (Soliz-Guerrero et al., 2002).
The microwave-assisted extraction (MAE) is a relatively new technique but has been growing rapidly in
recent times. Compounds present in the matrix can
interact with a suitable solvent assisted by microwave
energy, which heats the system and allows for better
extraction. Microwaves have advantages over the rate of
heating of the sample and prevent overheating, avoiding
thermolabile substances denaturation. Therefore, with
this method, can achieve good yields in short time.
As mentioned earlier, the objectives of this research
were to evaluate the extraction eciency of saponins
from quinoa seed by solvent extraction, employing
microwaves through an appropriate combination of the
operating variables (% alcohol, time, temperature,
volume solvent gram seeds).
Materials and methods
900 W Litton BGH 16650 microwave (Argentine industry) with a temperature sensor was used during the
experiments.
The extractions in Soxhlet device were performed with
20% ethanolwater or isopropanolwater mixtures in
both cases, in a ratio of 20 mL of solvent per gram of seed.
Extraction procedure with microwave equipment
Saponins in the extracts were derivatised by the LibermannBurchard reaction, mainly based on Monje et al.
(2006) although it was taken into account (Hostettmann
& Marston, 2005) and (Abisch & Reichstein, 1960). The
absorbances were measured at 528 nm with a Perkin
Elmer Lambda 25 spectrophotometer. Calibration
curves were determined with oleanolic acid. Linear
regression of data followed the expression:
A 4:5725 S 0:0164
R = 0.9998
A: measured absorbance, [S]: saponin concentration
(mg mL) and R2: the square correlation coecient of
the calibration curve.
The low quantication limit for eqn (1) is
0.05 mg mL and its linearity limit is 0.65 mg mL.
All measurements were performed at least ve times,
and the Q acceptance criteria applied. The condence
interval was established by the Students t test with a
probability of 95%, resulting 0.011 for extractions
with ethanol and 0.010 for isopropanol.
For the extraction eciency (E), the following equation was used:
E = 100 total mass of saponins [g] mass of seed [g]
Results and discussion
Level
Factor A
Vol. Solvent/g seed
Factor B
Time (min)
Factor C
T (C)
Factor D
% alcohol
I
II
III
IV
15
20
25
30
5
15
20
30
50
60
70
90
20
60
80
95
Experiment
Factor A
Vol. Solvent/g seed
Factor B
Time (min)
Factor C
T (C)
Factor D
% alcohol
Vacancy
Ethanolwater
mixtures
Isopropanolwater
mixtures
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
I(15)
I
I
I
II(20)
II
II
II
III(25)
III
III
III
IV(30)
IV
IV
IV
I(5)
II(15)
III(20)
IV(30)
I
II
III
IV
I
II
III
IV
I
II
III
IV
I(50)
II(60)
III(70)
IV(90)
II
I
IV
III
III
IV
I
II
IV
III
II
I
I(20)
II(60)
III(80)
IV(95)
III
IV
I
II
IV
III
II
I
II
I
IV
III
1
2
3
4
4
3
2
1
2
1
4
3
3
4
1
2
0.765
0.797
1.070
0.339
0.502
0.107
1.555
1.236
0.065
0.749
0.877
0.933
0.742
0.890
0.073
0.722
0.804
1.008
0.477
0.012
0.196
0.015
2.663
1.380
0.002
0.387
0.898
1.568
0.921
1.565
0.000
0.385
0.011
0.011
0.011
0.011
0.011
0.011
0.011
0.011
0.011
0.011
0.011
0.011
0.011
0.011
0.011
0.011
0.010
0.010
0.010
0.010
0.010
0.010
0.010
0.010
0.010
0.010
0.010
0.010
0.010
0.010
0.010
0.010
*Each experiment was performed with factors at the corresponding levels, indicated in roman numbers (see Table 1) and following the proceeding
explained in Materials and Methods.
This table provided the following conditions in the experiment. For example, for the experiment 1: solvent volume is 15 mL g of seeds, applied 5 min
time, temperature 50 C and the percentage of alcohol 20%. The experimentally measured efficiency is 0.804. This value is the average of the efficiencies
of five experiments performed in the same conditions.
1595
Efficiency
(g of saponins per 100 g of seeds)
(a)
3
2.5
2
1.5
1
0.5
0
0
10
15
20
25
30
35
t (min)
3
2.5
2
1.5
1
0.5
0
0
Efficiency
(g of saponins per 100 g of seeds)
(c)
10
15
20
25
% Alcohol
30
35
40
45
3
2.5
2
1.5
1
0.5
0
0
(d)
10
15
20
25
Volume of solvent per gram of seed
30
35
3
2.5
2
1.5
1
0.5
Efficincy
(g of saponins per 100 g of seeds)
(b)
Efficiency
(g of saponins per 100 g of seeds)
1596
2
Stages
0
50
60
70
80
Temperature C
90
100
1597