Received: 23 May 2018 Revised: 8 November 2018 Accepted: 12 November 2018

DOI: 10.1111/jfpe.12972

ORIGINAL ARTICLE

Curcumin encapsulation by spray drying using Aloe vera

mucilage as encapsulating agent
L. Medina-Torres1 | D. M. Núñez-Ramírez2 | F. Calderas3 | M. J. Bernad-Bernad4 |
J. Gracia-Mora5 | J. Rodríguez-Ramírez6 | R. F. González-Laredo7 | J. A. Gallegos-Infante7 |
O. Manero8

1
Departamento de Ingeniería Química,
Facultad de Química, Universidad Nacional Abstract
Autónoma de México, Ciudad de, México, In this work, curcumin was spray-dried (SD) with Aloe vera mucilage as the encapsulating agent
Mexico
giving particular attention to the effect of the relevant process parameters (feed flow rate,
2
Laboratorio de Biotecnología, Facultad de
atomization speed, and inlet air temperature) on the resulting properties of the SD powders.
Ciencias Químicas, Universidad Juárez del
Estado de Durango (UJED), Durango, Dgo., The powders obtained were analyzed by infrared spectroscopy, scanning electron microscopy,
Mexico rheology, and release profiles. Results show that the best drying conditions are low SD inlet air
3
Laboratorio de Reología y fenómenos de temperature (150  C), low feed flow rate (1.5 L/hr), and high atomization speed (27,500 rpm).
transporte, Unidad Multidisciplinaria de These conditions produced particles with smooth morphologies, preserving the total phenolic
Investigación Experimental (UMIEZ), Facultad
de Estudios Superiores-Zaragoza, Universidad
content (0.0611 μg EAG), with a radical scavenging capacity of 911.48 μmol Trolox/mg. Release
Nacional Autónoma de México, Ciudad de profiles revealed an extended release of encapsulated material with a maximum of about 65% at
México, Mexico 24 hr for these conditions and point out the suitability of encapsulated systems for potential
4
Departamento de Farmacía, Facultad de applications in functional foods, antioxidant systems, pharmaceutical, and organic pigments.
Química, Universidad Nacional Autónoma de
México, Ciudad de México, México Practical applications
5
Departamento de Química Inorgánica y This research presents an optimization method to obtain powders of mucilage (Aloe vera, Av)-
Nuclear, Facultad de Química, Universidad
curcumin (Cu) by spray drying (SD), where the Av was used as wall material to encapsulate Cu
Nacional Autónoma de México, Ciudad de
México, México and obtain the best process conditions (SD) to produce prolonged delivery systems of antioxi-
6
Instituto Politécnico Nacional, CIIDIR Oaxaca, dant compounds that can be used in the food and pharmaceutical industry. The encapsulated
Oaxaca, Mexico systems were analyzed by rheological tests and were supported with other characterizations,
7
Departamento de Ing. Química y Bioquímica, such as antioxidant capacity, morphology (SEM), chemical (FT-IR), and releasing profiles.
Instituto Tecnológico de Durango, Durango,
Dgo., Mexico
8
Departamento de Reología y Mecánica de
Materiales, Instituto de Investigaciones en
Materiales, Universidad Nacional Autónoma de
México, México, Mexico
Correspondence
Fausto Calderas, Laboratorio de Reología y
fenómenos de transporte, Unidad
Multidisciplinaria de Investigación Experimental
(UMIEZ), Facultad de Estudios Superiores-
Zaragoza, Universidad Nacional Autónoma de
México, Batalla 5 de mayo S/N, Ejército de
Oriente, Iztapalapa 09230, Ciudad de Mexico.
Email: faustocg@unam.mx

1 | I N T R O D U C TI O N 1998; Trujillo et al., 2013). It is a labile compound susceptible to deg-

radation by temperature, light exposure, metallic ions, oxygen
Curcumin is an effective antioxidant and a potential safe, anticancer (Mangolim et al., 2014; Paramera, Konteles, & Karathanos, 2011a;
agent (Sampathu, Lakshminarayanan, Sowbhagya, Krishna-Murthy, & Paramera, Konteles, & Karathanos, 2011b; Sowbhagya, Smitha, Sam-
Asha, 2000; Sowbhagya H, Sampathu S, Vatsala C, & Krishnamurthy, pathu, Krishnamurthy, & Bhattacharya, 2005), which restricts its

J Food Process Eng. 2018;e12972. wileyonlinelibrary.com/journal/jfpe © 2018 Wiley Periodicals, Inc. 1 of 12

https://doi.org/10.1111/jfpe.12972
2 of 12
applications in the pharmaceutical and food industries (Hanne,
Mar, & Thorsteinn, 2002; Trujillo et al., 2013). To overcome such
problems, stabilization of labile compounds by microencapsulation
has been considered (Dziezak, 1988; King, 1995). This process
involves the production of particles encapsulated by a coating agent
or embedded in matrices, which renders materials with useful prop-
erties for different applications (Matsuno & Adachi, 1993). Stabiliza-
tion occurs because the wall material provides a physical barrier to
protect the encapsulated particles against molecular oxygen, light,
moisture, and minimizes molecular diffusion (Bimbenet, Bonazzi, &
Dumoulin, 2002; Heinta, Krober, & Teipel, 2001; Kondo, 2001;
Schuck, 2002). Accordingly, the encapsulated products shelf-life is
enhanced and the release rate of the encapsulated particles or drop-
lets can be modified for specific applications. There are different
techniques to produce microencapsulated products (centrifugal
extrusion, spray cooling, lyophilization, spray-drying [SD], extrusion,
molecular inclusion, etc.). However, the SD technique has several
advantages such as low cost, continuous production, availability of
equipment and easy scaled-up, which makes it a popular and widely
used technique (Drusch & Schwarz, 2006; Liu et al., 2001; Paradkar,
Ambike, Jadhav, & Mahadik, 2004; Rosenberg, Kopelman, & Talmon,
1990). Microcapsules stability and SD efficiency depend entirely on
the wall material (Liu et al., 2001; Liu, Zhou, Zeng, & Ouyang, 2004;
Zbicinski, Delag, Strumillo, & Adamiec, 2002).
Attention has been given to curcumin encapsulation with various
wall materials, such as gelatin and porous starch (Wang, Lu, Lv, & Bie,
2009), cyclodextrins (CDs) (Mohan, Sreelakshmi, Muraleedharan, &
Joseph, 2012; Szente, Mikuni, Hashimoto, & Szejtli, 1998; Tønnesen,
Másson, & Loftsson, 2002), liposomes (Li, Braiteh, & Kurzrock, 2005),
cationic micelles (Leung, Colangelo, & Kee, 2008), yeast cells
(Paramera et al., 2011a), and modified starch (Paramera et al., 2011b;
Yu & Huang, 2010). In this context, Aloe vera mucilage has excellent
properties such as water-solubility, film-formation, biodegradability,
edibility, and a capability of forming a dense network when dried
(Brazel, 1999; Gouin, 2004; Medina-Torres et al., 2016; Pérez-Alonso,
Báez-González, Beristain, Vernon-Carter, & Vizcarra-Mendoza, 2003).
However, to establish the best SD conditions, reduction of thermal
degradation is sought to optimize the yield obtaining microcapsules of
appropriate size and form.
The most important process parameters in the SD process are
inlet flow rate, atomizer speed, and inlet–outlet air temperatures
(Augustin, Sanguansri, Margetts, & Young, 2001; Rodríguez-Hernán-
dez, González-García, Grajales-Lagunes, Ruiz-Cabrera, & Abud-Archila,
2005). When the inlet air temperature is increased, droplets size, and
viscosity are reduced (Cervantes-Martínez et al., 2014; Medina-Torres
et al., 2013, 2016; Medina-Torres et al., 2017; Santiago-Adame et al.,
2015). However, high inlet or outlet air temperatures can also degrade
heat-sensitive materials (Cervantes-Martínez et al., 2014). A proper
feed flow rate would cause the sprayed droplets to attain the right
drying levels before reaching the drying chamber surface (Soper &
Thomas, 2001). Cervantes-Martínez et al. (2014) reported that feed
flow rate and temperature of the inlet air are important parameters
affecting the characteristics of the microcapsules. A low inlet air
temperature causes a reduction in the evaporation rate, producing
microcapsules with high water content, high-density membranes,
MEDINA-TORRES ET AL.
poor fluidity, and augmented agglomeration (Mofidi, Aghai-Moghadam, &
Sarbolouki, 2000). Thus, inlet air temperature should be carefully
controlled to preserve the product and generate homogeneous
microcapsules. Outlet air temperature is not generally controlled but
depends on the drying characteristics of the SD material and other
process parameters. The first general approach is to measure and
control the inlet air temperature (Cervantes-Martínez et al., 2014;
Medina-Torres et al., 2013, 2016, 2017; Rodríguez-Hernández et al.,
2005; Santiago-Adame et al., 2015). An optimum outlet air tempera-
ture or the SD of food ingredients has been reported to be in the
range 60–80  C (Gouin, 2004).
Mucilage from Aloe vera (Av) possesses good emulsifying proper-
ties, thus, representing a promising natural encapsulating agent
(Medina-Torres et al., 2013, 2016; Minjares-Fuentes et al., 2016,
2017). Av is used as an additive in the pharmaceutical industry; specif-
ically, it has been applied as a coating to extend the regeneration of
skin tissues (Mangolim et al., 2014). Previous studies have reported
that the mucilage of Aloe vera is a complex mixture of polysaccharides
(Medina-Torres et al., 2016; Sáenz, Sepúlveda, & Matsuhiro, 2004).
One of the properties that limits its applications is the high moisture
content, which has been reduced using specific treatments such as SD
to encapsulate labile compounds (Cervantes-Martínez et al., 2014;
Medina-Torres et al., 2016; Minjares-Fuentes et al., 2016, 2017;
Santiago-Adame et al., 2015).
The rheology of food products subjected to SD is relevant in qual-
ity control, storage processing, and assessment of product stability,
closely related with the texture of SD products (Abu-Jdayil, Banat,
Jumah, Al-Asheh, & Hammad, 2004). In this work, and for the first
time, Aloe vera is used as encapsulating agent of curcumin employing
the SD process. Infrared analysis (FT-IR), scanning electron micros-
copy (SEM), rheology, and release profiles evaluate the effectiveness
of the material to encapsulate curcumin. Microcapsules of Aloe vera
and curcumin as the core encapsulated material represent an interest-
ing option to incorporate color and antioxidant additives in functional
foods and pharmaceutical products, focusing on the best drying condi-
tions to obtain microcapsules with adequate release profiles and pre-
serving their antioxidant capacity.
2 | MATERIAL AND METHODS
2.1 | Materials
Aloe vera leaves were collected in northern Mexico (Durango), in fields
with controlled irrigation. The leaves selected for this study were
bright-green color, growing in the rims of the plant with 24–30 months
in average. In previous works, a concentration of 2  0.1  Brix has
been reported to be the best concentration to encapsulate active
agents (Medina-Torres et al., 2013). Furthermore, the curcumin (active
agent) was used here as the core material.
2.2 | Extraction of the Aloe vera mucilage
The whole leaves of the plant (thorns, tip, base, and bark) were sepa-
rated, washed, and cooled down. Subsequently, semi-frozen pulps
MEDINA-TORRES ET AL. 3 of 12

were placed in a commercial juice extractor (Hamilton Beach Health
Smart 67800, 400 W). The juice produced was clarified and centri-
fuged (Heraeus Labofuge model 400/400 R tabletop centrifuge, 13.4
× 24.6 × 23.6 in.) to remove suspended solids. The clarified juice was
 flow rate (1.5 and 1.7 L/hr) and atomization speed (25,000, 26,500,
stored in sterilized jars at low temperature (at 4 C). pH (AOAC,
1990), 
Brix (EXTECH Instruments, Brix refractometer model RF-

10-CAT, Scale 0–32% Brix, Resolution 0.2%), total soluble solid content
(Standard NMX-F-510-1998) and moisture (OHAUS, thermo-balance
MB27, moisture content presicion of 1 mg/0.01%) were measured.
2.3 | Preparation of curcumin (Cu) dispersions in
Aloe vera mucilage
A sample of 11.25 g Curcumin (Sigma Aldrich, 85% pure) was dis-
solved in 200 ml of Aloe vera mucilage (2  0.1 Brix) at 80  0.1  C
powder collecting glass container of 1,000 ml (with PTFE adapter)
with a rotary atomizer (Minor TS M02/A) were used. To evaluate the
effect of the process parameters, a 23 fractional factorial design was
employed: temperature of inlet air (150, 170, and 190  C), inlet feed
and 27,000 rpm). In each treatment, the constant outlet temperature
was 78 to 80  C; similar conditions were employed in previous studies
(Medina-Torres et al., 2013; Medina-Torres et al., 2016). The drying
conditions for the control sample (middle point used for reference)
were 170  C and 26,500 rpm (see Table 1 for a list of drying condi-
tions of the samples).
2.5 | Moisture content of the SD powders
An infrared thermo-balance (A&D-4714A, resolution 0.1%) was used

with constant stirring in a magnetic stirrer (CLS6795420KIT Sigma, to measure the moisture content of the SD powder, under the follow-

AC/DC input 120 V, 60 Hz, 5–550 C) during 30 min. From this ini- ing conditions: 110  0.1  C for 60 min with an initial weight of 5 g

tial solution, 2 L batches were prepared by continuous dilution up to per sample. All measurements were performed by duplicate. Results

the desired concentration, as described in the following section. are reported as percentage of dry matter (d.b).

Dispersions were prepared using curcumin at a concentration of

0.56% (weight/volume, w/v) of the previous step and adding 1.8 L of
Aloe vera mucilage at 2  Brix adjusted with distilled water. The mixture
was homogenized using magnetic stirring (500 rpm) for 1 hr at 25  C.
Dispersions were dried using a Spray Dryer Niro equipped with a
rotary atomizer. The effect of SD process parameters was studied
according to a fractional factorial design 23 with a central point (see
Table 1). The performance of the SD process was calculated according
to Equation (1):
%Spray Drying Yield, ðSDY Þ ¼ ½ðdried powder weight after spray dryingÞ
=ðweight of initial suspension fed to SD processފ X 100
ð1Þ
2.4 | SD process
A laboratory scale co-current SD was used (Mobile Minor, GEA Niro
Spray Dryer, Copenhagen, Denmark) with compressed gas flow of
5 kg/hr to 15 kg/hr at a pressure of 0.5 to 3.0 bar, maximum flow rate
of 418 L/min with standard tubing, cylinder size diameter, cylindrical
height and cone angle of 793 mm, 645 mm, and 60 , respectively. A
2.6 | Bulk density determination of the powders
10 g of the SD powders were introduced and weighted in a graduated
cylinder class A (Pyrex,  1 ml, height: 33.5 mm, Germany) from which
the bulk volume was measured (NOM-001-SSA1-2010, bulk density).
2.7 | Total phenolic content
To estimate the total content of phenolic compounds (TPC) of Cu and
powders (SDCu), the modified method of Folin–Ciocalteu (Heimler,
Vignolini, Dini, & Romani, 2005) was used. The oxidation–reduction
reactions of the Folin–Ciocalteu reagent for TPC determinations
enable the detection of polyphenols (i.e., curcumin) and almost any
reducing substance. This colorimetric assay is very sensitive, precise
but lack specificity; it may give a relative value of the total reducing
capacity (i.e., antioxidant activity) of a sample besides its phenolic con-
tent. To estimate the TPC values, a calibration curve was prepared with
gallic acid content ranging from 1 to 100 μg/ml (R2 = 0.992). Phenolic
determinations were made almost by triplicate and expressed as gallic
acid equivalents (GAE/mg).

TABLE 1 Yield, moisture, bulk density, total phenolic content, and radical scavenging capacity by ORAC determinations of the spray dried
powders for each of the respective treatments
Inlet air Feed Atomization *Spray drying *Moisture *Bulk *Total phenolic *ORAC,
Sample temperature ( C) flow, (L/hr) speed, (rpm) yield, (%) content, (%, d. b) density, (kg/m3) content, (μg GEA) (μmol Trolox/mg)
C-1 170 1.6 26,500 9.25  0.25ª 7.59  1.06ª 304  8ª 0.1053  0.0080c 934.40  37.62c
b b b ac
T-1 190 1.5 25,000 8.55  0.50 9.02  0.98 320  8 0.1220  0.0033 948.57  35.34ac
b b b ab
T-2 190 1.5 27,500 8.05  0.75 9.45  1.05 330  5 0.0640  0.0076 926.70  72.57ab
b b b a
T-3 190 1.7 25,000 7.95  0.85 9.05  1.50 316  4 0.0485  0.0049 847.33  18.02 a
T-4 190 1.7 27,500 7.22  0.38b 10.7  1.30b 330  5b 0.0472  0.0045a 883.78  59.32 a
a ab
T-5 150 1.5 25,000 9.48  0.72 7.32  0.18ª 300  5ª 0.0613  0.0056 937.97  62.32ab
a ab
T-6 150 1.5 27,500 9.19  0.51 7.38  0.92ª 305  5ª 0.0611  0.0057 911.48  48.10ab
bc
T-7 150 1.7 25,000 9.22  0.28ª 7.90  1.00ª 308  2ª 0.0882  0.0094 915.99  54.83bc
T-8 150 1.7 27,500 8.53  0.57a 7.32  0.28ª 309  6ª 0.0801  0.0069ab 896.97  34.65ab

Note. Means sharing a letter in their superscript are not significantly different at the .05 level.
*Data are expressed as the mean of three essays  SD.
4 of 12
2.8 | Radical-scavenging activity (oxygen radical
absorbance capacity method)
To estimate the antioxidant capacity of the samples, the oxygen radi-
cal absorbance capacity (ORAC) method was used as described by Ou,
Hampsch-Woodill, and Prior (2001) with minor modifications. The
antioxidant trolox was used as a standard at a temperature of 37  C
and pH of 7.4. The oxidative degeneration of the test compound is
quantified by means of a spectro-fluorometer. Absorbance was mea-
sured at 492 nm and 515 nm with a standard curve prepared with dif-
ferent concentration of trolox. The test measures the capacity of
trolox to protect a fluorescent molecule (fluorescein, 1 × 102 M in
PBS) whose intensity decreases after the azo-initiator is added, usually
35 min. Results are reported as trolox equivalents (μmol Trolox/mg).
2.9 | Analysis by infrared spectrometry, (FT-IR)
A FT-IR Nicolet 6,700 with diamond tip (Thermo Fisher Scientific) was
required to perform analysis of Cu, Av, and SDCu. A potassium bro-
mide disc was used and 100 scans were applied with resolutions of
1 cm−1 within a 4,000 cm−1 to 400 cm−1 range.
2.10 | Scanning electron microscopy
Microscopy samples were treated as reported by Medina-Torres
et al. (2016). The samples were fixed to a gold-coated surface and a
vacuum of 10 mbar was applied for 90 s (Model Desk II, Denton Vac-
uum, NJ). A SEM (JEOL Mod. JSM6300 Jeol, Japan) was used to
observe the sample at a 20 kV accelerating voltage.
2.11 | Rheological analysis
Aqueous solutions of SDCu powders with a concentration of
0.06 g/ml (reconstituted powders) were prepared to perform the rhe-
ological characterization of the samples. Tests in continuous steady-
state simple shear flow and small amplitude linear oscillatory flow
were performed in a controlled-stress rheometer model DHR-3 of TA
Instruments. The geometry employed was a concentric cylinder geom-
etry with a Peltier system (Cole Parmer Polystat and Peltier AR- G2)
for temperature control. Samples were dissolved in deionized water

by constant stirring of 300 rpm for 1 hr at 25 C. All tests were per-
formed at 25 C. 
2.12 | Controlled release analysis
Release profiles of SDCu powders were obtained by the dialysis bag
method. The SDCu powder was loaded in a concentration of
0.2 mg/ml in water into a pre-swelled dialysis bag. This dialysis assem-
bly was then suspended in a release medium (100 ml) in phosphate
buffer solution pH 6.5  0.1 at 37.0  1  C to simulate intestinal
fluid during 40 hr in a closed beaker with constant magnetic stirring
(250 rpm). At given intervals, a volume of the release medium was
withdrawn and assayed by UV–VIS spectrophotometry. An equal
amount of fresh medium, which was preheated to 37  C, was added
for compensation after each sample-drawing to maintain sink condi-
tions. All experiments were performed by triplicated.
MEDINA-TORRES ET AL.
spectrophotometric (UV) analysis of AC was carried out at wavelength
of maximum absorbance (λmax = 198.5 nm). The analysis was per-
formed in a S2000 spectrometer using A DT1000 deuteruim light
source, SAD500 serial port interface (Optics, Inc.) and 10 nm path
length quartz cuvette (Prolab) (García Guzmán et al., 2018).
2.13 | Statistical analysis
A 23 fractional factorial design (inlet air temperature: 150, 170, and
190  C, inlet feed flow rate: 1.5, 1.6, and 1.7 L/hr and atomizer speed:
25,000, 26,500, and 27,500 rpm) included three tests for each SD
treatment. These SD conditions are based on previous studies with
Aloe vera as wall material (Cervantes-Martínez et al., 2014; Medina-
Torres et al., 2016; Santiago-Adame et al., 2015). Finally, the data
were analyzed using the ANOVA Tukey test (α = 0.05) with Statistica
7.0 (StatSoft, Tulsa, OK).
3 | RESULTS AND DISCUSSION
3.1 | Powder yield (%), moisture content, and bulk
density
The percentage of yield and moisture content ranged from 7.22 to
9.48 ( 0.11) %, and 7.34 to 10.70% dry basis ( 0.16), respectively
(Table 1). The lowest content was observed in T4, which lies below
the value reported in previous studies with melon and apple extracts
with pomegranates (Ochoa-Martinez et al., 2011; Quek, Chok, & Swe-
dlund, 2007). The bulk density values of the SD powders ranged from
300 to 330 kg/m3.
3.2 | Total phenolic content and antioxidant activity
Table 1 reports on the total phenolic content (TPC) of the samples,
where the highest one corresponds to Samples T1, C, T7, and T8. Phe-
nol concentration TPC in the SD curcumin was lower than that
reported for several Brazilian herbal infusions such as chamomile,
anise, and mint (De Souza, Oldoni, & Alencar, 2008; Trujillo et al.,
2013). With respect to the antioxidant activity, samples were analyzed
for radical scavenging capacity by the ORAC method (Table 1). Results
evidence that the SD process did not affect significantly (p < .05) the
antioxidant capacity of the curcumin, specially for Samples T1, Control
(C), T6, T7, and T8, which show similar values of the TPC. These
values are similar to those reported for the encapsulation processes of
antioxidants by SD at temperatures above 65  C (Gallegos-Infante
et al., 2013; Krishnaiah, Sarbatly, & Nithyanandam, 2012). Chemical
analyses of the microparticles in the powder included characterization
by rheological behavior, molecular spectroscopy (FT-IR) to identify
sample composition, morphology (SEM) and controlled release rate. A
large value of the TPC is associated with lower degradation (according
with the corresponding process parameters) which is used to select
the best conditions of SD. However, a large phenolic content alone
does not ensure that the microcapsules are well formed or that the
release profiles are adequate. The optimum SD conditions expected
for polyphenols as curcumin, are such that the samples containing
A higher phenolic concentration exhibit proportionally higher
MEDINA-TORRES ET AL.
antioxidant activity. The Aloe vera particles with higher or lower TPC
(or curcumin) displayed the correspondingly antioxidant activity level.
It is remarkable that the samples with relatively higher and lower

CTP’s are found at the maximum temperature (190 C), although the
atomization speed and especially the feeding flow determine the qual-
ity of particles and their behavior when releasing their phenolic core.
In this case, for large feed flows rate, the lower the residence time of
samples in the spray dryer; the residence time is thus an important
condition to enhance the production of more efficient particles of Aloe
vera containing a curcumin core. When the phenolic contents of pow-
ders are observed and compared, to show the effect of temperature
(treatments T6 vs. T2, Figure 5b), similar TPC and antioxidant
responses are obtained (Table 1); however, the conformation of parti-
cles and release performance is meaningfully better at lower inlet air
temperature (i.e., 150  C, Figure 5b), which is noticeable during the
first 10 hr of the release experiments. Likewise, particles made at low
temperature show a better release behavior under SD at higher atomi-
zation rate (i.e., 27,500 rpm) as revealed in Samples T7 versus T8
(Figure 5c). In this case, the retention time of curcumin and Aloe solu-
tion in SD is also a key factor to display a better release pattern of the
bioactive component (T4 vs. T2, Figure 5a).
3.3 | Spectrometry analysis (FT-IR)
Samples of Cu-Av (those fed to the drying process) and SDCu (Spray
dryed curcumin powders) were characterized by FT-IR-spectra analy-
sis. In Table 2, the characteristic wavelengths (corresponding to chem-
ical bonds) are shown. The bands at 1,110 cm−1, 1,300 cm−1, and
1,602 cm −1
are associated with aromatic compounds having phenyl
bonds such as flavonoids which are polyphenolic compounds
(Heneczkowski, Kopacz, Nowak, & Kuźniar, 2000; Schulz & Baranska,
2007). Similar absorption bands revealing the presence of phenolic
TABLE 2 The infrared peaks wavelenghts of curcumin and Aloe vera
main components
Raw material Peak assignment
Curcumin (cm−1)
856 γ(CH) of aromatic and structure of CCH
1,110 δ(CCH) of aromatic rings and δ(C OH) of
the enolic group coupled to d(C CH) in
the inter-ring chain
1,300 δ(CH) of C CH, ν(CCH) of the aromatic
ring in the enolic side of the molecule
1,580 ν(C O), δ(CCC) and δ(CC O)
1,602 ν(C C) of aromatic rings
Aloe vera (cm−1)
810 Mannose absorption
875 Piranoside ring absorption (C H ring
vibration)
1,040 Mannopyranose component, glucan units
1,240 o-Acetyl ester (C O C) stretching
1,590 Carboxyl groups (asymmetrical COO −
stretching vibration); C O
3,280 OH hidroxyl groups
According to: Kolev et al., 2005 and Mohan et al., 2012; Mangolim et al.,
2014; Yan et al., 2002; Nejatzadeh-Barandozi and Eferadi, 2012.
5 of 12
compounds in herbs and aromatic plants were reported elsewhere
(Lu, Ross, Powers, & Rasco, 2011; Ragupathi Raja Kannan, Arumu-
gam, & Anantharaman, 2011). Figure 1a–d shows different FT-IR
spectra corresponding to the raw materials and SD samples. In
Figure 1a, the FT-IR spectra of the pure compounds is shown (Aloe
vera and curcumin). Figure 1b,c illustrate various SD samples and the
pure curcumin spectra included as reference. In Figure 1a, a typical
absorption band is shown at a wavelength of λ = 3,280 cm−1, charac-
teristic of the hydroxyl group (-OH, see Table 2) in the pure Aloe vera
sample (dotted line). The fact that this band is significantly reduced
for the SD samples is related to the quality of the drying process, since
this band indicates the water content of the sample. Curcumin typical
absorption bands lie in the interval from 856 cm−1 to 1,602 cm−1 (see
Table 2). These signals are present in the SD samples (SDCu), but with
reduced magnitude (Figure 1b,d), which reveals a good encapsulation.
As in previous reports (Cervantes-Martínez et al., 2014; Medina-
Torres et al., 2013; Medina-Torres et al., 2016; Medina-Torres et al.,
2017; Santiago-Adame et al., 2015), the signal of the wall material is
the predominant signal in the SD powders. If the core material is
encapsulated inside the particles, the band is overshadowed by that
of the wall material, caused by the dramatic reduction in the concen-
tration of the core material contained inside the particles. If the mate-
rial to be encapsulated is not located inside the particles, its signal will
not be reduced in the powders spectra. The mucilage shows a typical
band at 1,040 cm−1 (Figure 1a) which corresponds to the mannopyra-
nose component (see Table 2). This band is predominant in all encap-
sulated samples. Accordingly, samples dried at 150  C with 1.5 L/hr
feed rate (Sample T6, see Table 1) show the best curcumin encapsula-
tion profile on comparison of the FT-IR-spectra in Figure 1b–d.
3.4 | Scanning electron microscopy
The configuration of the SD powder microparticles is shown in
Figure 2. Micrographs of the curcumin powders obtained by SD
(Figure 2b,f ) and the sample of mucilage without curcumin (Figure 2a)
are shown. In Figure 2a, irregular capsule shapes are attributed to par-
ticle shrinkage and collapse during the SD process. The shape of the
particles is determined by the drying process conditions, that is, the
atomization speed determines the diameter and number of particles
(Porowska et al., 2016). The feed flow rate establishes the residence
time of the material in the drying chamber and the inlet air tempera-
ture controls the evaporation rate of the droplets and the external
shape of the particles (De Prisco, Maresca, Ongeng, & Mauriello,
2015). When biopolymers are employedd as wall material, it is com-
mon to observe smooth particles, with few collapsed particles. The
predominant microstructure will tend to spherical particles or
deflated-ballon like particles, as reported by Dolly, Anishaparvin,
Joseph, and Anandharamakrishnan (2011). They argue that the inter-
nal (liquid) and external (solid) particle pressure difference produces
an adiabatic evaporation process in which the rate of diffusion of
water vapor is higher through the particle wall than in the particle sur-
face itself. Another possible explanation according to Liu et al. (2016)
deals with the occurrence of phase separation when biopolymers are
employed as wall materials. Polymer network formed through hydro-
gen bonds, hydrophobic interactions or van der Waals forces, induce a
6 of 12 MEDINA-TORRES ET AL.

FIGURE 1 Infrared analysis: (a) raw materials curcumin and Aloe vera; (b) inlet air temperature effect at 1.5 L/hr and 27,500 rpm (T2, 190  C and
T6, 150  C; (c) feed flow rate effect at 150  C and 27,500 rpm (T6, 1.5 L/hr and T8, 1.7 L/hr); (d) atomization speed effect at 150  C and 1.5 L/hr
(T5, 25,000 rpm and T6, 27,500 rpm)

diffusion of biopolymer molecles and water to the particle surface,
due to differences in dehydration of the first layers of polymer
attached to the particle surface and those formed afterwards.
Similar morphologies have been reported for microcapsules of
cactus pear crops (Opuntia lasiacantha), pigments encapsulated with
maltodextrin (Sánchez, López, Kerstupp, Ibarra, & Scheinvar, 2006),
Opuntia ficus indica and Aloe vera mucilages (Medina-Torres et al.,
2013, 2016), maltodextrin encapsulated amaranthus (Cai & Corke,
2000), and β-carotene encapsulated with maltodextrin and modified
tapioca starch (Loksuwan, 2007). Smooth spherical microcapsules
were observed in maltodextrin encapsulated black carrot pigments
Daucuscarota L. (Ersus & Yurdagel, 2007). Gharsallaoui, Roudaut,
Chambin, Voilley, and Saurel (2007) reported a direct relationship
between morphology configurations and SD inlet air temperature.
Figure 2b shows the C-1 sample where capsules collapsed with irregu-
lar shapes. Micrographs of the SD samples with curcumin (Figure 2c,f )
show more dispersed microcapsules. For enhanced intermolecular
mucilage-curcumin interactions, reduction of aggregates size is evi-
dent, especially at 150  C and 1.5 L/hr, which is independent of the
atomization speed (Figure 2c,d, T5 and T6 samples, respectively).
Agglomeration is revealed in Samples T7 (Figure 2e) and T8
(Figure 2f ) corresponding to SD conditions of 150  C and 1.7 L/hr
feed flow rate, independently of the atomization speed. In Figure 2,
we observe the effect of increasing the feed flow rate from 1.5
(Figure 2e) to 1.7 L/hr (Figure 2f ) and keeping all other parameters
constant (150  C and 25,000 rpm). The effect of the increasing feed
MEDINA-TORRES ET AL.
FIGURE 2 SEM images at 1000 X of the powder particles of SD Aloe vera—curcumin aqueous extracts: (a) pure Av mucilage at the same SD
conditions as Sample T6, (b) C1, (c) T5, (d) T6, (e) T7, and (f ) T8
flow rate is to produce collapsed particles with rugged surfaces. A
possible cause is the presence of large shear stresses due to the
increase in feed flow rate. This is also observed in Figure 2d (1.5 L/hr)
and 2f (1.7 L/hr) at different atomization speeds for both samples

(27,500 rpm) at a temperature of 150 C.
A combination of low inlet air temperatures with low feed flow
rates seems necessary to obtain a good particle morphology. In the
middle point (Sample C1 170  C, 1.6 L/hr) particle morphologies are
not fine. Irregular shape capsules are attributed to deficiencies in
water removal in the SD process. At higher SD temperatures (and
higher evaporation rates) smoother and well-defined surfaces in
microcapsules are reported by Alamilla-Beltran, Chanona-Perez,
Jimenez-Aparicio, and Gutierrez-Lopez (2005). They found that at low
inlet air temperatures in the SD process, irregularly shaped microparti-
cles with creased surfaces are formed. In contrast, with high inlet air
temperatures, more defined and smoother microparticles were
7 of 12
obtained. In the case of the present study, a low temperature in the
SD process (150  C) in combination with low feed flow rate (1.5 L/hr)
led to more spherical and defined microparticles, with fewer collapsed
particles and with reduced particle agglomeration. Tonon et al. (2009)
reported similar results for maltodextrin encapsulated açai juice,
where smooth, irregular, and spherical-semispherical particle configu-
rations were observed.
3.5 | Rheological behavior of the reconstituted
powder
The mechanical spectra in simple shear flow present three different
regions: a near Newtonian behavior (constant viscosity plateau) at low
shear rates and a well-defined shear thinning response (n < 1) at high
shear rate (Figure 3), with an intermediate transition region at moderate
shear rates (1–10 s−1). Figure 3a shows the effect of the feed flow rate
8 of 12
FIGURE 3 Viscosity-shear rate curves: (a) feed flow rate effect at
150  C and 27,500 rpm (T6, 1.5 L/hr and T8, 1.7 L/hr); (b) inlet air
temperature effect at 1.5 L/hr and 27,500 rpm (T2, 190  C and T6,
150  C; (c) atomization speed effect at 150  C and 1.5 L/hr (T5,
25,000 rpm and T6, 27,500 rpm)
(1.5 and 1.7 L/hr, Samples T6 and T8, respectively) for samples pro-
cessed at 1.5 L/hr and 27,500 rpm. The sample with the largest feed
flow rate (T8) shows the highest viscosity, due to the fact that a high
feed flow rate is related with low residence time in the SD chamber
and, thus, thermal degradation of the mucilage by chain scission is
reduced. Thermal degradation is associated with molecular weight
decay and thus, viscosity decreases with increasing thermal degradation
MEDINA-TORRES ET AL.
FIGURE 4 Oscillatory flow curves: (a) feed flow rate effect at 150  C
and 27,500 rpm (T6, 1.5 L/hr and T8, 1.7 L/hr); (b) inlet air
temperature effect at 1.5 L/hr and 27,500 rpm (T2, 190  C and T6,
150  C; (c) atomization speed effect at 150  C and 1.5 L/hr (T5,
25,000 rpm and T6, 27,500 rpm)
(Medina-Torres et al., 2017). Accordingly, rheological measurements
can be related to the thermal degration occurring inside the drying
chamber. This is the reason why the best SD conditions are sought to
prevent structure degradation of the encapsulated compound (Medina-
Torres et al., 2016). Figure 4b shows the effect of inlet air temperature
on the viscosity of samples processed at 150  C and 27,500 rpm. The
sample processed at the highest temperature (190  C, T2) shows the
lowest viscosity, which is attributed to thermal degradation (Tuyen,
MEDINA-TORRES ET AL.
FIGURE 5 Comparison of release profile: (a) feed flow rate effect at 190  C and 27,500 rpm (T2, 1.5 L/hr and T4, 1.7 L/hr); (b) inlet air
temperature effect at 1.5 L/hr and 27,500 rpm (T2, 190  C and T6, 150  C; (c) atomization speed effect at 150  C and 1.7 L/hr (T7, 25,000 rpm
and T8, 27,500 rpm)
Nguyen, & Roach, 2010). This is consistent with results of the sample

processed at the lowest temperature (150 C, T6) which shows a high
viscosity. Finally, Figure 3c shows the effect of the atomization speed
for samples processed at 150  C and 1.5 L/hr feed flow rate (Samples
T5 and T6 at 25,000 and 27,500 rpm, respectively). The sample with
the highest atomization speed (27,500 rpm, T6) shows the largest vis-
cosity. A high atomization speed is related to large shear stresses,
which promote particle disaggregation and particle-size reduction aug-
menting the viscosity of the system (Grabowski, Truong, & Daubert,
2008; Hill & Carrington, 2006; Medina-Torres et al., 2013; Medina-
Torres, Brito-De La Fuente, Torrestiana-Sanchez, & Katthain, 2000).
In Figure 4, we show the effect of the SD process conditions on
the storage (G0 ) and loss (G00 ) modulus as a function of the oscillatory
frequency in SDCu-reconstituted samples. Results depict a predomi-
nant viscous behavior (empty symbols) over the elastic one (filled sym-
bols). No crossover point was found along the frequency range. In
general, the moduli follow Maxwellian terminal slopes of 1 and 2 for
G” and G’, respectively.
9 of 12
Figure 4a illustrates the variation of feed flow rate (1.5 and 1.7 L/hr,
Samples T6 and T8 respectively) for samples processed at 150  C and
27,500 rpm. Results confirm the effect observed in the viscosity
(Figure 3a), namely, a high feed (1.7 L/hr) increases the value of both
moduli (G’ and G”) indicating low thermal degradation. Figure 4b shows
the effect of temperature on the viscoelastic moduli for samples pro-
cessed at 1.5 L/hr and 27,500 rpm, confirming that high temperatures
have a negative effect on the viscoelastic moduli by thermal degradation
inside the drying chamber: Sample T2 processed at 190  C shows the
lowest moduli (G’ and G”). Finally, Figure 4c shows the effect of the
atomization speed of samples processed at 150  C and 1.5 L/hr feed
flow rate (Samples T5 and T6 at 25,000 and 27,500 rpm, respectively).
Results confirm that high atomization speeds lead to a positive effect on
the moduli (Sample T6 processed at 27,500 rpm shows larger moduli
than Sample T5 processed at 25,000 rpm). Other works using carbohy-
drates as encapsulating agents have reported similar results (León-Martí-
nez, Rodríguez-Ramírez, Medina-Torres, Lagunas, & Bernad-Bernad,
2011; Medina-Torres et al., 2013).
10 of 12
3.6 | Controlled release analysis
Controlled release analysis of microencapsulated systems is very
important to estimate the quality of the microencapsulation process
and the encapsulated compound release evolution for specific applica-
tions. Stability of the encapsulated system is also assessed by this
analysis. SDCu did not show problems of solubility in aqueous media
(electric potential, pZ > 30 mV). The release conditions for the pro-
files presented here are designed to emulate the conditions inside the
digestive tract. The release of antioxidants during a large release
period is sought, since enhanced absorption of the curcumin antioxi-
dants is promoted with large residence times. Figure 5 shows different
release profiles and in particular, Figure 5a illustrates the effect of
feed flow rate of curcumin SD samples at 190  C and 27,500 rpm. At
these conditions, the release profiles for both samples (T2 and T4, 1.5
and 1.7 L/hr, respectively) are practically overlapped, indicating no
effect of the feed flow rate on the release profile. However, these
samples show a quasi-steady release profile of curcumin, which is
reached at approximately 8 hr with a maximum release of about 45%
at 36 hr. These systems are not very effective since the percentage
release is below 50% and they stabilize after 36 hr, leaving most of
the content inside the capsules. This effect may be related to micro-
capsule excesive aggregations which impede the core material to be
released properly. This is confrmed by the presence of agglomerated
microcapsules in the micrographs of Figure 2e,f. Figure 5b shows the
effect of temperature on the release profile of SD-curcumin samples
at 1.5 L/hr feed flow rate and 27,500 rpm atomization speed. The
sample dried at low temperature (T6, 150  C) depicts the major exten-
sion and most complete release profiles, reaching a maximum above
60% (~70%) of curcumin at 24 hr. This system is very effective
because most of the encapsulated curcumin is released over a period
of 24 hr. Finally, Figure 5c shows the effect of atomization speed on

the release profile of samples processed at 150 C and 1.7 L/hr feed
flow rate. The sample processed at high atomization speed (T8,
27,500 rpm) shows the fastest release profile of all samples with
almost 65% release reached at 12 hr, while the sample processed at
low atomization speed (T7, 25,000 rpm) shows an extended release
profile with a maximum of 55% at 24 hr. The release profile depicted
an initial rapid release period during 12 hr, followed by a slower
release rate up to 24 hr. The results at 150  C, 1.5 L/hr and
27,500 rpm (T6) suggest that the SDCu microparticles allow the maxi-
mum percentage of prolonged release in the intestinal regions (37  C
and pH~6.0) where the curcumin could possibly be absorbed more
efficiently. These release profiles would allow the manufacture of
tailor-made delivery systems, depending on the release period sought
and curcumin doses for each situation.
4 | CO NC LUSIO NS
Curcumin was encapsulated by SD using Aloe vera mucilage as the
encapsulating agent, at different process conditions of inlet air tem-
perature, feed flow rate, and atomization speed.
The morphology of the encapsulated curcumin powders depicts
quasi-spherical particles with considerable particle aggregation.
MEDINA-TORRES ET AL.
Smoother particle morphologies were found in samples processed at
low temperature (150  C) and low feed flow rate (1.5 L/hr).
FT-IR analysis confirmed that the curcumin was effectively
encapsulated by the Aloe vera mucilage. The rheological behavior of
rehydrated powders evidenced shear-thinning behavior (n < 1) with
a tendency to a Newtonian constant viscosity at low shear rates.
The most significant effect in the flow curves was observed at low
feed flows, which caused lower viscosity than at high feed flow
rate. This result is associated to high sample degradation due to
longer residence time.
A high inlet air temperature caused lower viscosities as expected,
and atomization speed had a small influence on the mechanical behav-
ior of the samples. This was confirmed by linear oscillatory flow data.
Release profiles were obtained at similar conditions as those
found in the human digestive tract (37  C and pH~ 5.6). This study
revealed that the best encapsulating conditions were found in Sample
T6 (an extended release profile with a maximum release of about 65%
at 24 hr). Different release profiles were obtained under various pro-
cessing conditions, which allows for the possibility of preparing tailor-
made encapsulated systems depending on the preferred release
period and adequate doses for specific applications, such as antioxi-
dant systems, functional pharmaceutical, and organic pigments.
Further studies may include evaluation of the particle size of the
microcapsules, storage stability of the powders, scale-up to pilot and
industrial plants, study the release profiles on real digestive tract con-
ditions, and others.
ACKNOWLEDGMENT
For the handling and treatment of the samples by SEM to Prof. Ivan
Puente (Facultad de Química, USAI, Universidad Nacional Autónoma
de México, México).
ORCID
L. Medina-Torres https://orcid.org/0000-0002-9963-821X
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How to cite this article: Medina-Torres L, Núñez-
Ramírez DM, Calderas F, et al. Curcumin encapsulation by
spray drying using Aloe vera mucilage as encapsulating agent.
J Food Process Eng. 2018;e12972. https://doi.org/10.1111/
jfpe.12972