Study On Microencapsulation of Curcumin Pigments by Spray Drying PDF

Eur Food Res Technol (2009) 229:391396
DOI 10.1007/s00217-009-1064-6
ORIGINAL PAPER
Study on microencapsulation of curcumin pigments by spray

drying
Yu Wang Zhaoxin Lu Fengxia Lv
Xiaomei Bie
Received: 13 November 2008 / Revised: 25 March 2009 / Accepted: 30 March 2009 / Published online: 18 April 2009
Springer-Verlag 2009
Abstract Curcumin has strong coloring power, safety

and innocuity, comprehensive pharmacological function,
but its low stability and water insoluble limit its application. Curcumin microcapsules were prepared by spraydrying process using porous starch and gelatin as wall
material here. Results showed optimal condition as follows: the ratio of core and wall material of 1/30, embedding temperature of 70 C, embedding time 2 h, inlet gas
temperature of 190 C, feed flow rate 70 mL/min and
drying air flow 70 m3/h, at which the microencapsules had
good encapsulation efficiency. The stability of microencapsulation curcumin against light, heat, pH was effectively improved and its solubility was increased greatly.
This study would be helpful to the industrial application of
curcumin.
Keywords Curcumin Pigment Microencapsulation
Spray drying Stability
Introduction
Natural pigment is a vital quality attribute of foods, and
plays an important role in sensory and consumer acceptance of products [8, 28, 29].Curcumin is an important
permitted natural colorant used in food, nutritious and
pharmaceutical preparations among others [22, 26]. It is a
fat soluble pigment, while it is insoluble in aqueous medium [10]. It is susceptible to oxidants, light and heat, which
can be easily deteriorated when exposed to such factors as
Y. Wang (&) Z. Lu F. Lv X. Bie
College of Food Science and Technology, Nanjing Agricultural
University, 210095 Nanjing, China
e-mail: joywangyu@sina.com
pH, temperature, light, metallic ions, enzymes, oxygen, and

ascorbic acid [27]. Because of its low stability, it cannot
really be widely used in the food processing industry [10].
Microencapsulation has been widely used for the stabilization of labile compounds [7, 13]. It is defined as a
process in which tiny particles or droplets are surrounded
by a coating, or embedded in homogeneous or heterogeneous matrix, to give small capsules with many useful
properties [17, 21]. In systems, stabilization occurs because
the wall material acts as physical and a permeability barrier
for molecular oxygen and other molecular diffusion [3, 11,
14, 23], consequently, the shelf life of the encapsulated
products could be prolonged.
Various kinds of microencapsulation techniques such as
spray drying, spray cooling, extrusion, centrifugal extrusion, freeze drying, molecular inclusion among others,
have been developed, among which, spray drying is the
most commonly used one due to its low cost, available
equipment, continuous production and easiness of industrialization, solid dispersions of curcumin in different ratios
with PVP prepared by spray drying can improve its bioavailability such as its limited aqueous solubility and
degradation at alkaline pH, but it give no further research
for its property study, which limits its industrialization[1, 6,
16, 20].
Microencapsulation efficiency and microcapsules stability are largely dependent on wall material composition
[15, 16, 30]. Wall materials can be selected from a wide
variety of natural and synthetic polymers such as natural
gum, proteins and maltodextrins. Among them, gelatin is a
good choice due to its good properties of film-formation,
water-solubility, edibility, biodegradation and a tendency
to form a fine dense network upon drying, results of study
indicate that microencapsulation using gelatin simple
coacervation method can reduce the color staining effect
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392
and enhance the stability of curcumin, but it give no

technological parameter for its industrialization [5, 9, 12,
19].
Optimal spray-drying conditions must also be considered. Among the main factors that must be optimized are
feed temperature, feed rate, air inlet temperature, low rate
and air outlet temperature [2].
When the feed temperature is increased, viscosity and
droplets size should be decreased but high temperatures
can cause volatilization or degradation of some heat-sensitive ingredients. The rate of feed is adjusted to ensure that
each sprayed droplet reaches the desired drying level
before it comes in contact with the surface of the drying
chamber [25].
Air inlet temperature and flow rate is important. When
the air inlet temperature is low, the low evaporation rate
causes the formation of microcapsules with high density
membranes, high water content, poor fluidity, and easiness
of agglomeration [18]. The air inlet temperature which can
safely be used without damaging the product or creating
operating hazards and the comparative cost of heat sources.
Air outlet temperature depends on the drying characteristics of the material. The ideal air outlet temperature for the
microencapsulation of food ingredients such as flavors has
been reported to be 5080 C [24].
The objective of this study is to develop a spray-drying
method for preparation of curcumin microcapsules using
gelatin as wall materials and to determine the effects of
different spray-drying operational variable on the curcumin
microcapsules to evaluate the effects on the properties of
spray-dried powders and their stability, which are valuable
for the advancement of drying technology and give technological parameter for its industrialization in the food
industry.
dissolve in acetone (solution concentration is 10%), was

dripped into the aqueous solution by stirring to form a
coarse emulsion at the following conditions (shown in
Table 1): embedding temperature, Tet, 60, 70, and 80 C;
embedding time, tet, 1, 1.5 and 2 h.
Spray-drying process
The emulsion were carried out on a Model YC-105 Spray
Dryer (Pilotech Instrument & Equipment Co., Ltd,
Shanghai, China) equipped with a spray-drying chamber
with dimensions of 150 cm height and 80 cm diameter, a
high-speed centrifugal atomizer, a cyclone separator, plus a
hot air blower and an exhaust blower. The emulsion was
then fed to the spray dryer at the following conditions
(shown in Table 2): feed flow rate of microencapsulating
composition, Wff, 60, 70, and 80 mL/min; inlet gas temperature, Tgi, 180, 190, and 200 C; drying air flow, Waf,
50, 60 and 70 m3/h. Samples of the spray-dried particles
were collected during the experiments.
Analysis
The encapsulation efficiency
The encapsulation efficiency (EE) was calculated as follows [4, 27]:
EE(% )
CE
100
CT
where CT refers to total added curcumin mass and CE refers

to the mass of curcumin in the microencapsulated.
Materials and methods
Table 1 Orthogonal design for the optimization of curcumin

microencapsulation
Wall and core materials
Number
Tet (C)
Mc/Mw
tet (h)
EE (%)
(1) 60
(1) 1:20
(2) 1.5
75.0
(1) 60
(2) 1:30
(1) 1
83.5
(1) 60
(3) 1:40
(3) 2
94.4
(2) 70
(1) 1:20
(1) 1
92.1
(2) 70
(2) 1:30
(3) 2
96.1
(2) 70
(3) 1:40
(2) 1.5
93.8
(3) 80
(1) 1:20
(3) 2
67.8
(3) 80
(2) 1:30
(2) 1.5
73.2
(3) 80
(3) 1:40
(1) 1
57.6
K1
252.9%
234.9%
243.4%
K2
282.0%
252.8%
241.9%
K3
Range
208.8%
73.2%
256.0%
21.1%
258.3%
16.4%
Wall materials used here included edible gelatin (G200,

Shanghai Chemical Reagent Corporation, China) and porous starch (Chongqing Taiwei Ecoagriculture Ltd, China).
Core materials used here were curcumin samples
(Hangzhou Lvtian Biotechnology Ltd, China).
Microencapsulation process
Gelatin (purity 96%) and porous starch (purity 98%) were
dissolved in hot distilled water, being stirred, to form an
aqueous solution containing different ratios of gelatin and
porous starch (mass ratio of core to wall material, Mc/Mw,
1/20, 1/30, and 1/40). Curcumin sample, preheated to
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393
Table 2 Orthogonal design for the optimization of spray-drying

operation conditions
Number
Tgi (C)
Wff (mL/min)
Waf (m3/h)
EE (%)
(1) 180
(1) 60
(1) 50
73.3
(1) 180
(2) 70
(2) 60
88.1
(1) 180
(3) 80
(3) 70
77.8
(2) 190
(1) 60
(2) 60
86.8
(2) 190
(2) 70
(3) 70
98.4
(2) 190
(3) 80
(1) 50
92.2
7
8
(3) 200
(3) 200
(1) 60
(2) 70
(3) 70
(1) 50
90.9
93.0
(3) 200
(3) 80
(2) 60
88.1
K1
239.1%
251.0%
258.4%
K2
277.34%
279.4%
263.0%
K3
272.0%
258.0%
267.1%
Range
38.3%
28.4%
8.7%
Quantification of curcumin
Twenty milligrams of microcapsule sample was dissolved
in absolute alcohol to form homogeneous solution (solution
concentration is 20%). Its absorbance and mass was
determined by a Model 752 UV spectrophotometry
(Shanghai jinghua Instrument Ltd, China) at
kmax = 425 nm. Curcumin concentration in the sample
was calculated using absorption value of the standard
solution.
Ten milligram of pure curcumin was dissolved in
absolute alcohol and up to 100 mL constant volume, from
which 10 mL solution was fetched. When it was up to
100 mL constant volume again, the standard curcumin
solution was obtained. In all, 1.0, 2.0, 3.0, 4.0, and 5.0 mL
standard solutions were up to 10 mL constant volume,
respectively, whose absorbances were determined by the
752 UV spectrophotometry at kmax = 425 nm. Its standard
curve and regression equation were then achieved, by
which the mass of curcumin in the encapsulated was
calculated.
The solubility of curcumin
The curcumin solubility in water was determined as follows. The mixture of the powder in the water solution
(0.3% w/v) was gently stirred until solid solubilization. The
powder was considered soluble when the time of solubilization was not greater than 5 min.
The time necessary for complete microcapsule solubilization was recorded. The results were conducted in
triplicate.
Evaluation of the curcumin stability

Effect of heating temperature and heating time on heat
resistance stability
The mixture of the powder in the water solution (0.5% w/v)
was prepared. Ten-milliliter solutions were heated 10 min
at a certain temperature, Th, 0, 60, 70, 80, 90 and 100 C,
respectively, the absorbance value of them were determined by the spectrophotometry at kmax = 425 nm.
Ten-milliliter solutions were kept at 100 C for a certain
heating time, tht, 10, 20, 30, 40 and 50 min, respectively,
the absorbance values were also determined by the
instrument.
Effect of pH on acid fastness stability
Curcumin can easily be deposited at the acidity condition,
which restricts its application in acid food. Improvement of
its acid fastness is necessary. When it is in alkali condition,
its color turns into russety, the alkali fastness stability have
not studied because of it.
The mixture of the powder in the water solution (0.5%
w/v) was prepared. Ten-milliliter solutions were regulated
to pH 1, 2, 3, 4,5, 6 and 7 with 1 mol/L hydrochloric acid,
respectively, the absorbance values of them were determined at 425 nm.
Effect of illumination time on light stability
The mixture of the powder in the water solution (0.5% w/v)
was prepared, 100 mL solutions were exposed in daylight
for certain days (illumination time), ti, 1, 4, 6, 8, 12, 16 and
30 days. Absorbance values were determined using the
previously described technique.
Experimental design and results

The standard curve is shown in Fig. 1. Its regression
equation was as follows:
Y 12:278X 0:3281
where X referred to the absorbance value and Y referred to

the concentration of curcumin. Furthermore, its R2 was
0.9998.
Optimization of curcumin encapsulation process
To determine the optimal condition of curcumin encapsulation process, the results of its orthogonal system was also
shown in Table 1. The best of EE 96.1% is in the
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394
The solubility of curcumin
curcumin concentraiton (mg/L)
7
6
In the water-solubility experiment, free curcumin was not

solved with water as solvent at normal temperature while
encapsulated curcumin was resolved immediately after
4 min. There was no deposit in solution, whose color and
luster of solution was vivid and transparent.
When encapsulated curcumin turned into powders after
spray-drying process, powders was immediately resolved
after 2 min. The solubility of encapsulated curcumin has
further improved.
y = 12.278x + 0.3281
2
R = 0.9998
5
4
3
2
1
0
The stability of curcumin

0.0
0.1
0.2
0.3
0.4
0.5
Effect of heating temperature and heating time on heat

resistance stability of curcumin
aborbance value (A)

Fig. 1 The standard curve of curcumin solution
experiment number 5, so the optimal condition was as

following: Tet, 70 C; Mc/Mw, 1/30; tet, 2 h.
Furthermore, compared their K1, K2, K3 and range, it
demonstrated that the embedding temperature was the best
important factor which effected on the encapsulation, while
mass ratio of core to wall material and embedding time was
relatively minor.
Optimization of curcumin spray-drying process
The results of spray-drying operation condition were
shown in orthogonal table (Table 2). The best of EE 98.4%
was in the experiment number 5, the optimal condition was
Tgi = 190 C, Wff = 70 mL/min and Waf = 70 m3/h.
Compared their K1, K2, K3 and range, the best important
factor was inlet gas temperature, the second was feed flow
rate, drying air flow was minor.
0.276
0.274
absorbance value (A)
0.272
0.270
0.268
0.266
0.264
microencapsulated curcumin before spray drying
primary curcumin
microencapsulated curcumin after spray drying
0.262
0.260
0.258
Effects of heating temperature for 10 min on the stability

of free curcumin, micro-encapsulated curcumin before and
after spray drying were shown in Fig. 2.
For three forms of curcumin, when heating temperature
was below 70 C, the variation of temperature had no
effect on curcumin stability. Along with increasing temperature, absorbance values of free curcumin fell off rapidly while those of microencapsulated curcumin before and
after spray drying declined tardily. Compared their absorbance values variation of curcumin at the temperature from
0 to 100 C, the reducing ratio of absorbance value for free
curcumin was 6.2%, while these for microencapsulated
curcumin before and after spray drying were 1.2 and 0.8%,
respectively.
Effects of heating time at temperature 100 C on the
stability of free curcumin, microencapsulated curcumin
before and after spray drying were shown in Fig. 3.
For curcumin, when heating temperature was 100 C,
along with increasing heating time, absorbance values of
free curcumin decreased rapidly while those of microencapsulated curcumin before and after spray drying leveled
off. Compared their absorbance values variation of curcumin from 10 to 50 min, the reducing ratio of absorbance
value for free curcumin was 25.9%, while these for microencapsulated curcumin before and after spray drying
were 5.9 and 2.8%, respectively.
When curcumin was microencapsulated, the heat resistance stability had been improved obviously, microencapsulated curcumin had better heat resistance stability.
0.256
Effect of pH on acid fastness stability
0.254
0.252
0
20
40
60
80
heating temperature ( )
Fig. 2 Effect of heating temperature on curcumin stability
123
100
Effects of pH on the stability of free and microencapsulated

curcumin before and after spray drying were shown in
Fig. 4. When their solutions were in condition from pH 6 to
pH 1, their orange color and lustre were stable. From pH 6
395
0.24
0.26
0.25
0.22
0.24
0.23
0.22
0.21
0.20

primary curcumin
0.18
0.16
0.19
0.20
primary curcumin
0.18
10
20
30
40
50
0.14
0
heating time (min)
10
15
20
25
30
illumination time (day)
Fig. 3 Effect of heating time on curcumin stability at temperature

100 C
Fig. 5 Effect of illumination on light stability of curcumin
absorbance values of free curcumin decreased rapidly, the

whole reducing ratio from 1 to 30 days was about 17.4%,
while those of microencapsulated curcumin before and
after spray drying were minor, which were 1.4 and 0.9%.
Microencapsulation of curcumin also had better stability to
illumination for a long time.
0.30
0.29
0.28
primary curcumin
0.27
0.26
0.25
0.24
0.23
1
pH
Fig. 4 Effect of pH on acid fastness stability of curcumin
to pH 4, absorbance value of free curcumin was invariable,

while from pH 4 to pH 1, it cut down. From pH 6 to pH 1,
the reducing ratio of absorbance value for microencapsulated curcumin before and after spray drying were 3.3 and
2.6%, while that of free curcumin is 15.7%. Microencapsulation of curcumin had better acid fastness stability.
Effect of illumination time on light stability
Effects of illumination on the stability of free curcumin,
microencapsulated curcumin before and after spray drying
were shown in Fig. 5. When their solutions were exposed
to light, orange color was stable. From 1 to 15 days,
absorbance value of free curcumin kept stable, along with
increasing illumination time from 15 to 30 days,
Conclusion
Curcumin microcapsules were successfully prepared by a
spray-drying method using a wall system consisting of
gelatin and porous starch. EE were significantly affected by
the ratio of core to wall materials, embedding temperature,
inlet gas temperature and feed flow rate. The optimal
condition was determined as follows: the ratio of core and
wall material of 1/30, embedding temperature of 70 C,
embedding time of 2 h, inlet gas temperature of 190 C,
feed flow rate of 70 mL/min and drying air flow of 70 m3/
h, at which microencapsulated curcumin before and after
spray drying showed good solubility and stability, such as
heat resistance stability, acid fastness stability and light
stability. This study would be helpful to promote the
application of curcumin and the food industry.
Acknowledgments This work was supported by the Youthful Scientific Innovation Foundation of Nanjing Agricultural University(no.
29972020).
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Eur Food Res Technol (2009) 229:391396