Drying Technology

An International Journal

ISSN: 0737-3937 (Print) 1532-2300 (Online) Journal homepage: http://www.tandfonline.com/loi/ldrt20

Encapsulation of Orange Essential Oil in a SpoutFluid Bed Dryer with a Draft Tube on a Bed of Inert
Solids
Claudia Velzquez-Contreras , Guillermo Osorio-Revilla & Tzayhri GallardoVelzquez
To cite this article: Claudia Velzquez-Contreras , Guillermo Osorio-Revilla & Tzayhri
Gallardo-Velzquez (2014) Encapsulation of Orange Essential Oil in a Spout-Fluid Bed
Dryer with a Draft Tube on a Bed of Inert Solids, Drying Technology, 32:14, 1718-1726, DOI:
10.1080/07373937.2014.924525
To link to this article: http://dx.doi.org/10.1080/07373937.2014.924525

Accepted author version posted online: 27

May 2014.

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Date: 10 January 2016, At: 20:18

Drying Technology, 32: 17181726, 2014

Copyright # 2014 Taylor & Francis Group, LLC
ISSN: 0737-3937 print=1532-2300 online
DOI: 10.1080/07373937.2014.924525

Encapsulation of Orange Essential Oil in a Spout-Fluid Bed

Dryer with a Draft Tube on a Bed of Inert Solids
Claudia Velazquez-Contreras, Guillermo Osorio-Revilla, and
Tzayhri Gallardo-Velazquez

Downloaded by [Diego Arroyave] at 20:18 10 January 2016

Escuela Nacional de Ciencias BiologicasInstituto Politecnico Nacional, Mexico City, Mexico

Encapsulation of orange essential oil in modied starch (N-Lok)

was performed in a spout-uid bed dryer with a draft tube (SFB) on
a bed of inert solids under different operating conditions. The essential oil retention and encapsulation efciencies were determined and
compared with those obtained in a spray-drying encapsulation
process. The results showed that, in general, both SFB efciencies
were lower than those obtained in the spray dryer; however, it was
observed that most of the essential oil remaining in the SFB was
encapsulated (94% compared with 70% for the spray dryer). The
formation of particles with thicker encapsulation walls in the SFB
provided better protection of the orange essential oil than that
achieved in spray drying.
Keywords Encapsulation; Inert solids; Orange oil; Spout-uid
bed dryer; Spray drying

INTRODUCTION
Encapsulation or microencapsulation is dened[1] as the
covering of liquids, solids, or gases with a thin, protective
layer or wall of some material, which inhibits volatilization
of the compound in question, thereby protecting it from
chemical deterioration. The term microencapsulation,
when used in the food and pharmaceutical industries, is a
synonym for encapsulation. The encapsulation or microencapsulation process has been applied in the food industry
for various reasons.[2] Various methods have been proposed in the literature to produce microcapsules, and spray
drying is the most commonly used method.[3] One of the
most promising low-cost alternatives to spray drying is
spouted-bed drying on a bed of inert solids.[4] The spouted
bed has been widely used in drying processes and represents an alternative to spray drying to obtain products of
the same quality at a lower cost.[57] Since its introduction
in 1995,[8] this technique has been used in numerous operations, such as the following[9]: drying of granular materials;
granulation; drying of solutions and suspensions; coating
and disinfection of grains and mixing solids.[7,10,11] The
Correspondence: Guillermo Osorio-Revilla, Depto. Ing.
Bioqumica, ENCB-IPN, Prol. de Carpio y Plan de Ayala,
11340 Mexico City, Mexico; E-mail: gosorio@encb.ipn.mx

use of a spouted bed to obtain ne powders from pastes,

suspensions, and solutions was developed by researchers
from the former Soviet Union at the Leningrad Institute
of Technology.[12] To minimize energy costs while drying
suspensions and solutions, it is necessary to use simple,
compact equipment that can be simply controlled, such
as a spouted bed with a bed of inert solids.[13] This type
of dryer offers numerous benets, such as the establishment of a cyclical systematic movement of the solids, good
particle-gas contact, simple construction, and simple maintenance. These characteristics make the spouted-bed dryer
an extremely promising, low-cost alternative to spray drying.[14] However, there are only a few studies available in
the literature regarding the use of this equipment to microencapsulate essential oils and other products. Only three
references were found related to this topic,[4,15,16] where
the authors studied the applicability of the spouted bed
for microencapsulation processes in pharmaceutical products and the drying of aromatic plant extracts; the studies
report that this technique is a promising process because it
forms capsules with harder, thicker walls, which reduces
the release velocity of the encapsulated compounds.
Even though there are no reports on encapsulating
essential oils in spouted beds, the encapsulation phenomenon is similar to that of the pharmaceutical products cited
previously and, therefore, it can be assumed that, based on
these works, encapsulating orange essential oil will yield
similar or better retention, encapsulation efciencies, and
protection to the encapsulated oil during product storage,
compared with processes that encapsulate oil through
spray drying, which is the motivation for this study.
MATERIALS AND METHODS
Materials
The encapsulating wall material used in this work was
modied starch N-Lok supplied by National Starch Food
Innovation (Mexico D. F., Mexico). The orange essential
oil was supplied by Adytec Alimentos (Mexico D. F.,
Mexico), which has a density of 0.843 kg=m3 and a refraction index of 1.473. Toluene, which was used to determine

1718

ORANGE OIL ENCAPSULATION IN SPOUT-FLUID BED DRYER

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the moisture content, was obtained from J.T. Baker

(AvantorTM Performance Materials, Edo. Mexico, Mexico).
Hexane, which was used to determine the supercial volatile
oil (SVO) in the encapsulated product, was obtained
from J.T. Baker (AvantorTM Performance Materials, Edo.
Mexico, Mexico). The essential orange oil components,
which included a-pinene, b-pinene, d-limonene, linalool,
myrcene, and carvone, were used as external standards
and obtained from Sigma-Aldrich (Sigma-Aldrich Co.,
St. Louis, MO, USA).
Emulsion Preparation
Solutions of 20% by weight N-Lok modied starch were
prepared using distilled water and kept overnight to warrant full saturation of the polymer molecules. Orange
essential oil was added in a 1:4 mass ratio (essential
oil:N-Lok) and homogenized for 10 min at 10,000 rpm in
an Ultra-Turrax M45 homogenizer (Ika-werke, Unsingen,
Germany).
Emulsion Drying
Emulsion drying was performed in a spout-uid bed
dryer, which consisted of a cylindrical chamber with a conical base and a short central tube submerged in an inert
solid bed. The content of the encapsulated, supercial
orange essential oil was determined, which will be
explained later. The equipment was described in detail in
previous works.[17,18] In summary, the drying chamber is
made from acrylic with an internal diameter (Dc) of
0.143 m, and the conical base is made from stainless steel
with an internal angle of 60
; the chamber is perforated
throughout its surface to allow additional air to be fed
through the annular region. The short central tube is made
from stainless steel and has a length of 0.088 m, an internal
diameter of 0.03 m, and is located 0.045 m from the air
entry nozzle and 0.01 m below the surface of the bed of
solids to avoid becoming wet by the solution, which is
sprayed from above the bed. The bed of inert solids consists of pellets made from a tetrauoroethylene and hexauoropropylene copolymer (FEP1, DuPont Company,
DE, USA) with an equivalent diameter of 0.0025 m.
Drying runs were performed using a static height of the
inert solid bed of 1 H=Dc, a spray pressure of 0.5 kgf=cm2,
and an inlet air ow velocity to the annular region equivalent to 0.7 Umf (minimum uid velocity) with an inlet annular air temperature equal to the outlet drying temperature
To. The previous operating conditions were used for various inlet air temperatures Ti (125, 140, 155, and 170
C),
outlet drying air temperatures To (80 and 90
C), and inlet
airow velocities through the annulus equivalent to 1.2 and
1.5 Umst (minimum spout velocity with a draft tube).
For comparison purposes, emulsion drying was also performed in a NIRO Atomiser Mobile Minor spray dryer
(Niro, Soeborg, Denmark) using inlet air temperatures

1719

(Ti) of 180, 200, and 220
C and outlet air temperatures

(To) of 110 and 120
C with an air ow rate of 1.57 m3=
min. The dryer consisted of a semi-pilot-scale spray dryer
with a 0.80-m diameter, cylindrical-conical chamber,
equipped with a rotary atomizer. The cylindrical section
was 0.75 m height, and the conical section 0.67 m height.
In addition, the content of the encapsulated, supercial
orange essential oil obtained in this study was compared
with those of two commercial samples that were fabricated
by two of the main avor industries in Mexico. According
to the manufacturers, both samples were prepared by
spray drying; sample 1 used maltodextrin DE-10, and sample 2 used a mixture of maltodextrin-arabic gum as wall
material.
Characterization of the Obtained Product
All measurements were performed in triplicate and are
presented as the mean followed by the standard deviation.
Total Volatile Oil Content (TVO)
The total volatile oil content was determined using
Clevenger traps for light oils, as described by AOAC.[19]
The retention of volatiles in the powder is expressed as
both g of oil per g of the dry encapsulant (N-Lok) and as
a percentage of the volatile compounds originally added
to the mix before emulsication based on the total added
encapsulant dry solids; this value is termed retention
efciency.
Supercial Volatile Oil Content (SVO)
The supercial volatile oil content was determined using
the same previous technique after washing the powder with
hexane.[20,21] The difference observed between the total volatile oil before and after the stage of extraction with hexane
is expressed as g of supercial oil per g of the dry encapsulant (N-Lok) and as a percentage of supercial volatile oil.
The difference between TVO and SVO, related to the initial
quantity of essential oil added per unit mass of dry solid, is
called the encapsulation efciency.
Moisture Content of the Product
The moisture content was determined using the toluene
distillation method as described by the AOAC.[19]
Bulk Density
The bulk density was calculated by determining the
quantity of mass of a loosely packed product required to
occupy a known volume using a 100 ml measuring cylinder.
Emulsion Droplet Size Analysis Before and After Drying
The droplet size analysis of the emulsion before drying
and the reconstituted product was determined using a
Malvern IM026, 2006 series particle size analyzer with a
63 mm lens. Distilled water was used as the dispersant.

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1720

ZQUEZ-CONTRERAS ET AL.
VELA

To determine the change in droplet size during the

encapsulation process in both dryers, the encapsulated
product was reconstituted in distilled water at room temperature at the same solids concentration as the original
emulsion (25%), then mixed with a magnetic stirrer for
30 min, and thus, the orange oil volume mean diameter
(D4,3) and size distribution could be determined.

2
C=min until 120
C was reached, followed by a ramp rate

of 10
C=min until 170
C was reached and nally held at
this temperature for 5 min. The following are the external
standards: a-pinene, b-pinene, d-limonene, linalool, myrcene, and carvone, where carvone was used as an indicator
of the oxidation of d-limonene.

Determination of the Particle Size of the

Encapsulated Product
The particle size of the encapsulated product was determined using a Malvern IM 026, 2006 series particle size
analyzer with a 63 mm lens, which is appropriate to determine particle sizes between 0.6188 mm. The particle size
distribution and the Sauter diameter (D3,2) of the encapsulated products were determined using hexane as a dispersing liquid.

RESULTS AND DISCUSSION

Table 1 lists the physical and dynamic properties of
the inert solids used (FEP1 pellets), which were obtained
using standard procedures.[17,18] The value for Umst was
obtained in the same way as Ums, but in the presence of
the draft tube.
Figure 1 shows the orange essential-oil droplet distribution in the emulsion before drying, compared with that
of the reconstituted encapsulated product obtained in both
the spout-uid bed dryer and in the spray dryer. As seen in
the gure, the distribution curve for the reconstituted
spray-dried product shifted toward a smaller size with a
similar dispersion of that of the emulsion before drying.
This reduction in droplet size, as reported by different
authors,[2325] is due to the large velocity gradient and sharing effect during atomization in the rotating atomizer. This
shift in droplet size, measured by the volume mean diameter, was found to be 2.13 mm in the emulsion before drying
and 1.43 mm in the spray-dried product.
Regarding the distribution curve for the reconstituted
spouted bed-dried product, Fig. 1 shows that a wider dispersion with a bimodal distribution was obtained, which
is caused by the drying process performed in the spouted
bed, characterized by shearing and collisions between the
inert particles themselves and with the dryer wall. As a
result of this, two opposing phenomena occur. First, a portion of the essential oil droplets coalesce, which results in a
large population with a maximum frequency droplet size of

Morphology of the Encapsulated Product by Scanning

Electron Microscopy (SEM)
The encapsulated product was examined in a JEOL
scanning electron microscope, model JSM-58001 V, at
various magnications. The sample was xed with copper
tape, coated in gold, and placed in the interior of the electron microscope. The external and internal structures of
the encapsulated product obtained in both dryers were
observed.
Storage of the Encapsulated Products Obtained by
Spout-Fluid Bed Drying and by Spray Drying
The storage of encapsulated products obtained in the
best operating conditions was accomplished by placing
the powder obtained from each drying technique in amber
glass jars with a screw cap at room temperature in the dark
and analyzing them every 15 days for three and a half
months. The powders were tested for moisture content,
total volatile oil (TVO), supercial volatile oil (SVO), and
retention percent. Morphology by electron microscopy
was examined at the beginning and the end of the threeand-a-half-month storage period. In addition, the powders
were chromatographically characterized.
Chromatographic Characterization
The chromatographic characterization of the orange
essential oil, both immediately after drying and during storage, was performed based on the technique described in the
Mexican Pharmacopeia, code MAG 0241, and the modied
method by Haypek.[22] A Perkin Elmer Clarus 500 gas chromatograph was used with a ame ionization detector (FID)
and an AT-1Heliex column that was 30 m in length and
had an internal diameter of 0.2 mm, which used nitrogen
as the carrier gas. The injector and FID temperatures were
250
C; the temperature program used for the column was
initially set at 60
C for 3 min, followed by a ramp rate of

TABLE 1
Physical properties of the inert solids (FEP1 DuPont)
used in the spout-uid bed dryer
Properties

Measured value

Particle size dp (m)

Particle density (kg=m3)
Sphericity
Bulk density (kg=m3)
Bed porosity
Minimum spouting
velocity (Ums) (m=s)
Minimum spouting velocity
with draft tube (Umst) (m=s)
Minimum uidization
velocity (Umf) (m=s)

0.00259  0.3
2039.6  9.61
0.73  0.15
1214  3.58
0.40  0.003
0.842  0.001
0.554  0.003
0.91  0.02

1721

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ORANGE OIL ENCAPSULATION IN SPOUT-FLUID BED DRYER

FIG. 1. Emulsion size distribution before drying and after reconstituting

the encapsulated powder from the spray-dried product and spout-uid bed
dried product.

approximately 2.7 mm (Fig. 1); and second, part of the

reduction in droplets size is likely due to the attrition
between the inert particles, which results in a smaller population with a maximum frequency droplet size of approximately 1.4 mm (Fig. 1). The volume mean diameter of the
bimodal distribution of the spouted bed product was

2.04 mm, which, on average, is extremely similar to the

droplet size in the emulsion before drying (2.13 mm). These
results show the feasibility of using the spout-uid bed for
encapsulation processes because the integrity of the orange
oil is essentially maintained.
Table 2a presents the results obtained from the characterization of the encapsulated product in the spout-uid
bed, and Table 2b presents the results obtained for the
spray-dried product and for the commercial samples. As
observed in Table 2a, for an equivalent air ow rate of
1.5 Umst, both the total volatile oil (TVO) and the supercial
volatile oil (SVO) increased slightly as the inlet and outlet
drying air temperatures increased until a maximum for both
values was reached at a Ti of 155
C and a To of 80
C; after
reaching these temperatures, these values decreased as Ti
and T0 increased. For an airow rate value through the
spout of 1.2 Umst, the same behavior was observed, where
the maximum values again were at 155
C for Ti and 80
C
for To for both TVO and SVO.
When comparing the characterization results of the
encapsulated product in the spout-uid bed dryer and those
of the spray dryer (Tables 2a and 2b), it can be see that both
the TVO and SVO of the spray-dried product are considerably greater than those obtained in the spout-uid bed
dryer. For the commercial products, Table 2b reveals that
the TVO and SVO values are, in general, less than those
obtained both in the spray dryer and in the spout-uid

TABLE 2A
Characterization of the encapsulated product obtained in the spout uid bed dryer with inert solid
Sample
1.5 Umst
1
2
3
4
5
6
7
8
1.2 Umst
1
2
3
4
5
6
7
8

Ti (
C)

To (
C)

TVO
(g=g N-Lok)

SVO
(g=g N-Lok)

Moisture %

Bulk
density (g=ml)

Particle size
(Sauter diameter) (mm)

170
170
155
155
140
140
125
125

90
80
90
80
90
80
90
80

0.1187  0.0001
0.1245  0.0001
0.1365  0.0030
0.1399  0.0004
0.1365  0.0004
0.1358  0.0001
0.1298  0.0003
0.1279  0.0034

0.0041  0.0002
0.0041  0.0001
0.0117  0.0021
0.0138  0.0002
0.0020  0.0001
0.0031  0.0010
0.0012  0.0008
0.0004  0.0001

1.00  0.01
2.00  0.01
1.25  0.25
1.75  0.25
1.25  0.25
2.50  0.01
2.00  0.01
2.50  0.50

0.36  0.01
0.39  0.01
0.34  0.01
0.35  0.01
0.37  0.01
0.42  0.01
0.36  0.01
0.36  0.01

50.12  0.20
57.25  0.11
43.86  0.96
51.94  1.45
42.49  0.17
64.87  0.72
34.77  0.08
40.36  0.71

170
170
155
155
140
140
125
125

90
80
90
80
90
80
90
80

0.1369  0.0026
0.1373  0.0022
0.1387  0.0001
0.1489  0.0004
0.1412  0.0008
0.1346  0.0004
0.1316  0.0026
0.1301  0.0004

0.0082  0.0041
0.0083  0.0002
0.0082  0.0001
0.0083  0.0002
0.0082  0.0001
0.0083  0.0010
0.0082  0.0001
0.0083  0.0002

1.50  0.01
1.75  0.25
1.00  0.01
0.75  0.25
2.50  0.50
1.75  0.25
1.00  0.01
2.25  0.25

0.36  0.01
0.38  0.01
0.36  0.01
0.37  0.01
0.35  0.01
0.31  0.01
0.35  0.01
0.37  0.01

35.26  0.55
39.51  2.13
27.68  0.55
37.39  1.09
41.10  0.93
41.32  0.38
23.00  0.78
43.00  4.13

TVO: Total volatile oil.

SVO: Supercial volatile oil.

 ZQUEZ-CONTRERAS ET AL.
VELA

1722

TABLE 2B
Characterization of the encapsulated product obtained by the spray-drying process and commercial samples
Sample

Ti (
C)

To (
C)

Spray drying
1
180
2
180
3
200
4
200
5
220
8
220
Commercial samples
Sample 1
Sample 2

110
120
110
120
110
120

TVO
(g=g N-Lok)

SVO
(g=g N-Lok)

Moisture %

Bulk
density (g=ml)

Particle size
(Sauter diameter) (mm)

0.1747  0.0014
0.1775  0.0043
0.1887  0.0029
0.1946  0.0029
0.1847  0.0001
0.1757  0.0043

0.0157  0.0032
0.0177  0.0011
0.0243  0.0011
0.0189  0.0021
0.0296  0.0001
0.0211  0.0021

2.00  0.01
2.00  0.01
2.50  0.01
2.50  0.01
2.00  0.01
2.50  0.01

0.37  0.01
0.35  0.01
0.35  0.01
0.31  0.01
0.34  0.01
0.32  0.01

22.28  0.26
39.51  1.42
27.62  1.52
28.83  1.26
27.84  0.19
27.66  0.12

0.0824  0.0029
0.0889  0.0014

0.0129  0.0021
0.0063  0.0029

5.00  0.01
4.00  0.01

0.24  0.01
0.50  0.01

44.87  1.45
40.48  1.51

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TVO: Total volatile oil.

SVO: Surface volatile oil.

bed dryer, with exception to the SVO of sample 1, which is

higher than that of the product obtained in the spout-uid
bed dryer. This result can be attributed to the type of encapsulation agent used in industry, which is generally maltodextrin (sample 1) or a mixture of maltodextrin and
arabic gum (sample 2), which, as mentioned by Flores,[26]
are not the best encapsulating agents because they cause
greater losses in TVO and SVO.
Tables 2a and 2b show that the moisture content is
less in the encapsulated product from the spout-uid bed
(12.5%) than that in the spray-dried product (23%) and
that of the commercial samples (45%), which is likely
due to the greater retention time of the product in the
spouted bed, which was, on average, 6.8 min.[18] These
same tables indicate that the bulk density of the product
is not affected by the operating conditions or type of dryer;
the bulk density remained essentially constant at approximately 0.350.38 g=ml.
Regarding the particle size of the encapsulated product
(Sauter diameter, D [3,2] Malvern), Table 2a indicates that,
for the spout-uid bed, no uniform trend is observed;
instead, occasionally, both reductions and increases in the
particle size are observed. However, in general, the particle
size is greater than those of the spray-dried samples and
in the commercial samples (Table 2b). These results can
be explained by the drying process performed in the
spout-uid bed, where collisions between the particles
and the fragility acquired by the product adhere to the inert
solids are not a direct function of the operating conditions
and, therefore, particle sizes with a widely dispersed distribution are obtained compared with both the spray-dried
product and the commercial products (Fig. 2). Chen and
zkan[27] and Benelli et al.[15] reported that, in spout-bed
O
drying, the particle size of the obtained product is greater
due to the drying mechanism (drying of lms over inert

solids) compared with that of spray drying (drying of droplets); similar results were obtained in this study.
The retention and encapsulation efciency obtained for
both the spout-uid bed dryer and the spray dryer for all
operating conditions used in this study are shown in
Fig. 3. For the spouted bed dryer, at 1.5 Umst, the retention
efciency increased with increases in the inlet and outlet
drying air temperatures, which obtained the maximum
(56%) at a Ti of 155
C and a To of 80
C; after reaching
these temperatures, the efciency decreased as Ti and T0
increased. The encapsulation efciency exhibited the same
behavior, though the maximum value (54%) was reached
at a Ti of 140
C and a To of 90
C. For a ow rate of
1.2 Umst, the same pattern was observed; however, the
retention and encapsulation efciencies were generally

FIG. 2. Particle size distribution of the product encapsulated by both the

spout-uid bed dryer (1.2 Umst, Ti 155
C, To 80
C) and the spray
dryer (Ti 200
C, To 120
C).

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ORANGE OIL ENCAPSULATION IN SPOUT-FLUID BED DRYER

FIG. 3. Efciency of encapsulation and total retention of the orange

essential oil with respect to the inlet and outlet operation temperatures
for the spout-uid bed dryer and spray dryer.

larger than the values obtained at 1.5 Umst and reached

maximums of 60% and 56% at Ti of 155
C and To of
80
C, respectively.
Figure 3 shows that both the retention and encapsulation efciencies in the spouted-bed dryer are not as high
as those obtained with the spray dryer, which are on the
order of 7078% retention and 6270% encapsulation.
The retention efciency for the spray dryer in the optimal
operating conditions (78%) closely agrees with the 81%
reported by Soottitantawat et al.[28] for the droplet size in
the original emulsion (2.13 mm).
If the encapsulation and retention efciencies obtained
under the optimal operating conditions for both dryers
are related (Ti 155
C, To 80
C and 1.2 Umst for the
spout-uid bed dryer, and Ti 200
C, To 120
C for the
spray dryer), then the results show that, on average, 95%
of the amount of oil retained for the spout-uid bed dryer
is encapsulated compared with 89% for the spray dryer,
which indicates that the encapsulation process in the
spout-uid bed is better in this aspect than that in the spray
dryer.
To perform deterioration tests during storage, the encapsulated product in the best operating conditions for each of
the dryers was packed and stored for three and a half
months. Figure 4 presents the results of the monitored
amounts of retained and encapsulated oil throughout the
storage period. This gure indicates that, as time passed,
the encapsulated oil lessened for both the product encapsulated by spray drying and those encapsulated in the
spout-uid bed dryer, with the total retained oil remaining
essentially constant. As observed in Fig. 4, a greater quantity
of encapsulated oil is lost in the product that was dried by
spray drying because, at the beginning of the storage period,
the ratio of encapsulated oil to total retained oil was 89%

1723

whereas, at the end of the study (three and a half months),

only 78% of the total retained oil remained encapsulated,
which represents a loss of 12.4% of the encapsulated
essential oil. The essential oil diffused to the particle surface
became exposed and began to deteriorate by oxidation in
air. In contrast, the product obtained in the spout-uid
bed dryer, which, at the beginning of storage, had a ratio
of encapsulated oil to total retained oil of 95% and, at the
end of the three and a half months of storage, exhibited a
reduction to 88%, which is a 7.4% loss of the encapsulated
oil. This result agrees with the report of the studies performed by several authors,[4,15,16] which have indicated
that the thicker wall that formed in the encapsulated products in the spouted bed better protected the core material,
which causes a slower release compared with spray drying,
where the wall that forms around the nucleus is thinner.
Figures 5a and 5b show the internal structure of the
encapsulated spray and spout-uid bed dried product,
respectively. As seen in Fig. 5a, the orange essential oil droplets are embedded in the shell (approximately 2 mm thick)
of hollow spheres obtained in the spray-dried product surrounded by a thin wall matrix, very near from the inner
and outer surfaces of the shell. Figure 5b also shows the
essential oil droplets embedded in the wall of the spouted
bed particle, which is ake-shaped; however, the wall thickness of these akes is approximately 20 mm, and the shell
around the droplet is thicker than in the spray-dried product, where most of the droplets are quite far from the surface, which gives more protection to the essential oil than
in the spray-dried product, as explained above.
Figure 5b shows that, although more protection to the
essential oil is given during storage than in the spray-dried

FIG. 4. Variation of the efciency of the encapsulation and total retention of the orange essential oil in the product obtained at the optimal operation conditions for both the spout-uid bed dryer (1.2 Umst, Ti 155
C,
To 80
C) and spray dryer (Ti 200
C, To 120
C) during storage.

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VELA

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FIG. 5. Internal microstructure of the essential orange oil encapsulate in (a) the spray-dried product (Ti 200
C, To 120
C); and (b) spout-uid bed
dried product (1.2 Umst, Ti 155
C, To 80
C).

product, it also shows that when the ake product in the

spout-uid bed dryer is fractured by collisions between
the inert particles and is released from the surface of these,
a large amount of essential oil is exposed to the drying air,
which explains why the total retention oil is lower in the
spouted bed dried product than in the spray-dried product
and why the percentage of the retained oil is higher in the
former (a large amount of droplets embedded in the particle) than in the latter.
Figure 6 presents the SEM electron micrographs of the
products at the beginning and end of the storage period,
where it can be seen that for the product encapsulated in
the spray dryer, at the beginning of storage (Fig. 6a), no

small stains are observed on the surface; however, these

stains are present at the end of the three-and-a-half-month
storage period (Fig. 6b). This result leads us to assume that
the oil was extremely close to the surface of the layer of the
encapsulating agent, which allows the encapsulated oil to
be released from the particle and become part of the
supercial oil.
For the product dried in the spout-uid bed, the SEM
electron micrograph in Fig. 6c shows that, at the beginning
of the storage period, the product was forming thick layers
without oil stains on the surface, and after the three and a
half months of storage, there were still no oil stains on the
surface of the layers. This result indicates that the products

FIG. 6. SEM micrographs of the encapsulated product: (a) and (b) obtained by spray drying (Ti 200
C, To 120
C), and (c) and (d) obtained by
spout-uid bed drying (1.2 Umst, Ti 155
C, To 80
C) at the beginning and after 3.5 months of storage, respectively.

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ORANGE OIL ENCAPSULATION IN SPOUT-FLUID BED DRYER

TABLE 3
Percent abundance of the major components (chromatographic assay) in the distilled original orange essential oil,
spout-uid bed and spray-dried product associated with the oil-retention efciency (% R) at 1.5 and 3.5 months of storage
Description
Original
SFB
SD

Storage time
(months)

a-Pinene

b-Pinene

Myrcene

Limonene

Linalool

Carvone

%R

1.5
3.5
1.5
3.5

0.68
1.03
0.83
0.95
0.92

0.67
0.52
0.49
0.49
0.53

2.62
2.14
2.61
2.79
2.73

94.45
94.86
90.01
95.28
87.97

0.83
0.72
0.60
0.65
0.67

0.10
0.67
0.67
0.79
0.89

56.70
56.13
76.19
74.76

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SFB Spout-uid-bed dried product.

SD Spray-dried product.

thicker wall obtained in the spout-uid bed process delays

the diffusion of oil towards the surface; i.e., it delays the
release of the encapsulated orange essential oil.
Table 3 presents the results obtained from the chromatography assay on the distilled original orange essential
oil used in this study, the encapsulated oil obtained from
the spout-uid bed dryer product (SFB) and the encapsulated oil obtained from the product dried by spray drying
(SD) after 1.5 and 3.5 months of storage. As seen, there
is a lower amount of carvone in the product dried using
the spout-uid bed than in the spray-dried product, which
indicates that the drying process in the spout-uid bed
reduces the exposure of the product to oxidation (represented by the presence of carvone) compared with the case
of spray drying, in which there is a large area of exposed
particles to the drying air. As the storage time progresses
from 1.5 to 3.5 months, the carvone content in the
encapsulated product using the spout-uid bed dryer
remains constant; however, the carvone concentration in
the encapsulated spray-dried product increases with
storage time (Table 3). Again, this result indicates that
the product obtained in the spout-uid bed dryer is more
protected.
Table 3 indicates that the limonene content in the encapsulated orange oil decreases more rapidly in the spray-dried
product because the limonene percentage was reduced to
87.97% at the end of the three-and-a-half-month storage
period compared with the 90.01% that was retained in
the product obtained from the spout-uid bed dryer. Given
that limonene oxidizes to form carvone, this result conrms
that the thick wall formed around the oil globules in the
spout-uid bed dryer favors the protection of the volatile
components of the orange essential oil and protects it from
degradation.
In summary, these results indicate that, even though the
percentage of retained essential oil in the product dried in
the spout-uid bed is lower than that in the spray-dried
product (60% compared with 77%, respectively), a greater
fraction of the retained oil is encapsulated in the

spout-uid bed (approximately 95% compared with 88%

for the spray dryer). In addition, due to the formation of
a thicker layer around the oil globules, drying in the
spout-uid bed better protects the essential oil from oxidation and enables a greater percentage of the encapsulated
oil to be maintained during storage.
CONCLUSIONS
The moisture content, bulk density, and particle size of
the product encapsulated in a spout-uid bed is not affected by the drying temperature or airow rate, and due to
the greater residence time, the product obtained contains
a lower moisture content than the product obtained by
spray drying.
The oil retention efciency of the product dried in the
spout-uid bed is 17% less than the efciency that was
obtained using spray drying. However, the thicker wall
of the encapsulated product provides greater protection to
the orange essential oil because the loss of limonene and
the formation of carvone decrease in the product encapsulated in the spout-uid bed compared with that obtained
by spray drying during storage.
The encapsulation process of essential oils through
spout-uid bed drying has good potential because this process better protects the encapsulated oil and thus slows the
release of oil during storage.
FUNDING
Financial support from the Instituto Politecnico
Nacional Escuela Nacional de Ciencias Biologicas and
CONACyT (Consejo Nacional de Ciencia y Tecnologa)
Mexico for the development of this study is greatly
appreciated.
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