Documenti di Didattica
Documenti di Professioni
Documenti di Cultura
discussions, stats, and author profiles for this publication at: https://www.researchgate.net/publication/234841369
CITATIONS
READS
284
4 authors, including:
Zuhaili Idham
14 PUBLICATIONS 38 CITATIONS
SEE PROFILE
SEE PROFILE
176..184
ZUHAILI IDHAM3, IDA IDAYU MUHAMAD1,4, SITI HAMIDAH MOHD SETAPAR3 and MOHD ROJI SARMIDI2
1
Department of Bioprocess Engineering, Faculty of Chemical and Natural Resources Engineering, UTM Skudai, Johor Bahru 81310, Johor, Malaysia
Chemical Engineering Pilot Plant (CEPP), UTM Skudai, Johor Bahru, Johor, Malaysia
3
Centre of Lipid Engineering Applied Research (CLEAR), UTM Skudai, Johor Bahru, Johor, Malaysia
2
ABSTRACT
The stability of roselle anthocyanins was investigated under three different heat
treatments (60, 80 and 98C). The dry red powder from roselle calyces was produced
using spray-drying technique using four different encapsulating agents, i.e., maltodextrin, gum arabic, a combination of maltodextrin and gum arabic, and soluble
starch. The four types of matrices increased the half-life of the pigments during heat
treatment, especially at 98C (P < 0.05), compared with the roselle extract as the
control. Heat treatment results showed that the combination of maltodextrin and
gum arabic had the lowest degradation kinetic rates at 60 and 80C. Arrhenius
parameters results further confirmed that the degradation of anthocyanins was
strongly dependent on the operating temperatures during heat treatment. In this
study, all encapsulating agents, except the soluble starch, largely elongated the halflife of roselle anthocyanins compared with the nonencapsulated anthocyanins.
PRACTICAL APPLICATIONS
A spectrum of natural, red-hue primer colorants is derived from roselle plant
extracts, which is substantially free of alkaloids, enzymes, aroma or solvent residuals,
and is microencapsulated to ensure good stability and shelf life. This study measured
the thermal stability and suitability of the microencapsulated natural colorants. The
colorants are for functional use in the food, pharmaceuticals, cosmetics and other
industries.
INTRODUCTION
Anthocyanins are members of a class of nearly universal,
water-soluble, terrestrial plant pigment that can be classified
chemically as both flavonoid and phenolic. Anthocyanins
provide attractive colors such as orange, red and blue. They
are water soluble, which facilitates their incorporation into
aqueous food systems. These qualities make anthocyanins an
attractive natural food colorant. Besides their color attributes,
anthocyanins have been reported to be beneficial to health as
potent antioxidant and improves visual acuity. They have also
been observed to possess antineoplastic, radiation-protective,
vasotonic, vasoprotective, anti-inflammatory, and chemoand hepatoprotective activities (Duran et al. 2001). Therefore, they have been intensively used as functional food
ingredients and color additives.
176
Journal of Food Processing and Preservation 36 (2012) 176184 2011 Wiley Periodicals, Inc.
Z. IDHAM ET AL.
Extraction Procedure
Pigment extraction method was modified from Laleh et al.
(2006) by maceration of dry powdered calyces with ethanol
with 2% citric acid (50:50) for 24 h at 4C. Then, the extract
was filtered in vacuum using Wattman filter (grade 1,
Whatman, Florham Park, NJ). Plant material was
re-extracted with acidified ethanol until a faint-colored
extract was obtained. Filtrates were pooled and the plant
material was discarded. The ethanolacid was removed with
rotary vacuum evaporator at 40C. Distilled water was added
to make up the remaining aqueous extract to a known
volume. The concentration of roselle anthocyanin extract was
done by adsorption chromatography via Amberlite XAD-16
(Rohm & Haas, Frankfurt, Germany). Amberlite XAD-16 was
slurred in water for 2 h before used (Kammerer et al. 2005).
Glass column was filled with 25 mL of the polymeric resin
and the resin was washed with 50 mL of acidified water. Prior
to application of the samples, the extract was centrifuged (at
3,890 g for 10 min) to remove solid particles. Aliquots of
100 mL of the extracts were applied to the adsorbent resin.
The sample was subsequently rinsed with 125 mL of water
and 50 mL of acidified water (citric acid, pH 2.0) at a flow rate
of 3 mL/min. 200 mL of acidified ethanol was used for elution
of the pigments. Fractions of dark red pigment were collected
during sample application. Then, the solvent was removed in
the rotary evaporator at 40C under vacuum. The pigments
were redissolved in deionized distilled water until Brix was
maintained at 8. Brix was measured using Atago Refractometer (Tokyo, Japan) at 20C. After desorption of phenolic compounds, the resin was reconditioned by rinsing with 100 mL
of sodium hydroxide solution (2.5 mol/L) and 125 mL of
water. All experiments were performed in duplicate. Extracts
were stored at -20C until further treatment.
Journal of Food Processing and Preservation 36 (2012) 176184 2011 Wiley Periodicals, Inc.
177
Z. IDHAM ET AL.
Encapsulation Process
The carrier agents MD DE 11-15, GA, combination of both
maltodextrin and gum arabic (60:40) (MD + GA), and SS
were combined with the pigment extract (8Brix) and stirred
(40C) until all the materials were completely dissolved. A
carrier agent was added subsequently until 20% of the final
solid content was reached, and the pH was maintained at the
range 2.53. Then, the mixtures were vigorously homogenized at 14,000 rpm for 1 h at room temperature. 500 mL of
feed mixtures was prepared for further process. The resulting
feed mixture was fed into the pilot plant spray dryer at a flow
rate 9.5% and was atomized by a centrifugal atomizer. The air
temperatures at the inlet and outlet were 160 and 100C,
respectively. The prepared microcapsules were collected in a
cyclone.
t 1 2 = ln (2) k
(3)
k = e ( Ea
(2)
R) T
(4)
D = ln (10) k
(5)
Q10 = 1010 z
(6)
Heat Stability
The effect of heat treatment on the stability of the encapsulated anthocyanins was investigated under three different
heating temperatures: 60, 80 and 98C. The samples of 0.04%
178
Statistical Analysis
All experimental analyses were done in duplicate. Significant
differences of the means in all the data were analyzed by
Journal of Food Processing and Preservation 36 (2012) 176184 2011 Wiley Periodicals, Inc.
Z. IDHAM ET AL.
Particle Morphology
Dry microcapsules were obtained as red-purple powder
samples. Figure 1 shows the examination of SEM micrographs. The particle size of the spray-dried pigment ranged
from 600 nm to 50 mm approximately, which was presented
in the form of agglomerates. All particles showed spherical in
shape with various sizes, which is typical to materials produced by spray drying. The outer surfaces of the spray-dried
microcapsules are characterized by the presence of dents.
Thermal Stability
Thermal stability is important to determine how long the
anthocyanins can be kept or processed in the thermal temperature. Figure 2 showed that thermal stability in this study
followed the first-order kinetic reaction and showed an agreement with many literature studies such as Yang et al. (2008),
Reyes and Cisneros-Zevallos (2007), Wang and Xu (2007),
and Havlikova and Mikova (1985). The coefficients of
Journal of Food Processing and Preservation 36 (2012) 176184 2011 Wiley Periodicals, Inc.
179
Z. IDHAM ET AL.
180
Journal of Food Processing and Preservation 36 (2012) 176184 2011 Wiley Periodicals, Inc.
Z. IDHAM ET AL.
Temperature (C)
Wall material
k sk (104/day)
R2
Half-life (h)
60
MD
MD + GA
GA
SS
C
MD
MD + GA
GA
SS
C
MD
MD + GA
GA
SS
C
0.0005 0.49a
0.0003 0.54b
0.0006 1.3c
0.0011 1.6d
0.0006 9.12c
0.0019 5.1a
0.0016 1.7b
0.0022 1.59c
0.002 2.1d
0.002 3.1d
0.006 6.14a
0.006 4.85a
0.006 3.76a
0.007 5.48b
0.008 9.51c
0.965
0.929
0.8199
0.929
0.722
0.976
0.958
0.979
0.961
0.933
0.962
0.977
0.985
0.977
0.945
23.1
38.5
19.3
10.5
19.3
6.08
7.22
5.25
5.78
5.78
1.93
1.93
1.93
1.65
1.44
80
98
Means within a column with different letters are significantly different (P < 0.05).
C, control; GA, gum arabic; MD, maltodextrin; SS, soluble starch.
Journal of Food Processing and Preservation 36 (2012) 176184 2011 Wiley Periodicals, Inc.
181
Z. IDHAM ET AL.
Arrhenius Parameter
Heat temperature significantly influences the anthocyanins
degradation rates. The dependence of reaction rates on temperature was characterized by the activation energy value, z
value and Q10. Figure 5 shows the Arrhenius plot for anthocyanins in encapsulated samples and control (roselle extract).
The graph shows, after plotting the ln k versus 1/T, that
encapsulated anthocyanins and control were all fitted to the
Arrhenius equation. The activation energy (Ea) is the energy
needed by a system to initiate a particular process. The activation energy is often used to denote the minimum energy
needed for a specific chemical reaction to occur. The high
activation energy obtained in the control sample shows that
CONCLUSION
182
Journal of Food Processing and Preservation 36 (2012) 176184 2011 Wiley Periodicals, Inc.
Z. IDHAM ET AL.
Temperature
(C)
Activation energy
(kJ/mol)*
Frequency factor,
K0 (1/h)
D value
(day)
z value
(C)
Q10
MD
60
80
98
60
80
98
60
80
98
60
80
98
60
80
98
66.95
(0.978)
1.45E + 07
14
5.18
81.09
(0.985)
1.43E + 06
12.8
6.04
62.4
(0.986)
3.43E + 06
15
4.64
47.51
(0.854)
2.66E + 04
19
3.36
68.67
(0.947)
3.10E + 07
4,605.2
1,211.9
383.8
7,675.3
1,439.1
383.8
3,837.6
1,046.6
383.8
2,093.3
1,151.3
328.9
3,837.6
1,151.3
287.8
13
5.87
MD + GA
GA
SS
ACKNOWLEDGMENT
The authors gratefully thank the Chemical Engineering Pilot
Plant (CEPP), Universiti Teknologi Malaysia, Skudai, for the
financial support through bioentrepreneur program.
REFERENCES
AHMED, J., SHIVHARE, U.S. and RAGHAVAN, G.S.V. 2004.
Thermal degradation kinetics of anthocyanin and visual colour
of plum puree. Eur. Food Res. Technol. 218, 525528.
AL-KAHTANI, H.A. and HASSAN, B.H. 1990. Spray drying of
roselle (Hibiscus sabdariffa L.) extract. J. Food Sci. 55,
10731076.
ANDRADE, I. and FLORES, H. 2004. Optimization of
spray-drying of roselle extract (Hibiscus sabdariffa L.). Drying.
Proceedings of the 14th International-Drying Symposium (IDS
2004), Sao Paulo, Brazil, 597604.
CHIOU, D. and LANGRISH, T.A.G. 2007. Development and
characterisation of novel nutraceuticals with spray-drying
technology. J. Food Eng. 82, 8491.
CLYDESDALE, F.M., MAIN, J.H. and FRANCIS, F.J. 1979. Roselle
(Hibiscus sabdariffa L.) anthocyanins as colorants for beverages
and gelatin desserts. J. Food Prot. 42, 204207.
DUANGMAL, K., SAICHEUA, B. and SUEEPRASAN, S. 2008.
Colour evaluation of freeze-dried roselle extract as a natural
Journal of Food Processing and Preservation 36 (2012) 176184 2011 Wiley Periodicals, Inc.
183
Z. IDHAM ET AL.
184
Journal of Food Processing and Preservation 36 (2012) 176184 2011 Wiley Periodicals, Inc.