Effect of Spray Nozzle Design on Fish OilWhey

Protein Microcapsule Properties

Jerrad Legako and Nurhan Turgut Dunford

Abstract: Microencapsulation improves oxidative stability and shelf life of fish oil. Spray and freeze drying are widely

E: Food Engineering &

Physical Properties

used to produce microcapsules. Newer spray-nozzles utilize multiple fluid channels allowing for mixing of wall and core
materials at the point of atomization. Sonic energy has also been employed as a means of atomization. The objective
of this study was to examine the effect of nozzle type and design on fish oil encapsulation efficiency and microcapsule
properties. A total of 3 nozzle types, a pressure nozzle with 1 liquid channel, a pressure nozzle with 2 liquid channels,
and a sonic atomizer with 2 liquid channels were examined for their suitability to encapsulate fish oil in whey protein
isolate. Physical and chemical properties of freeze dried microcapsules were compared to those of microcapsules produced
by spray drying. The 2-fluid pressure and ultrasonic nozzles had the highest (91.6%) and the lowest microencapsulation
efficiencies (76%), respectively. There was no significant difference in bulk density of microcapsules produced by ultrasonic
and 3-fluid pressure nozzles. The ultrasonic nozzle showed a significantly narrower particle size distribution than the other
nozzles. This study demonstrated that new nozzle designs that eliminate emulsion preparation prior to spray drying can be
beneficial for microencapsulation applications. However, there is still a need for research to improve microencapsulation
efficiency of multiple channel spray nozzles.
Keywords: fish oil, microencapsulation, whey protein isolate

Practical Application: Since this research evaluates new spray nozzle designs for oil microencapsulation, the information

presented in this article could be an interest to fish oil producers and food industry.

Introduction
It has been recommended to consume 0.2 g/d eicosapentaenoic
acid (EPA [20:5n-3]) and docosahexaenoic acid (DHA [22:6n3]), which may be done by weekly consumption of fatty fish
(Kolanowski and others 2004). However, in many western countries the amount of fish consumed is far below the recommended
servings (Kolanowski and others 2006b). Besides changes in diets,
increased intake of -3 polyunsaturated fatty acids (PUFA) such
as EPA and DHA may be accomplished through consumption of
fish oil supplements or foods enriched with fish oil (Kolanowski
and others 2004). Problems do arise when attempting to enrich
foods with fish oil. Fish oil has a limited storage life because the
PUFA are highly susceptible to oxidation (Cho and others 2003).
Microencapsulation provides a means to convert liquid fish oil
into a more stable and easy to use dry powder. The most common
way to produce microcapsules of fish oil is through spray drying
of an emulsion (Hogan and others 2003; Kolanowski and others
2004, 2006a, 2006b; Tan and others 2005; Augustin and others
2006; Drusch and others 2006; Rusli and others 2006) because
this process is flexible, efficient, and inexpensive (Ashady 1993).
Heinzelmann and others (Heinzelmann and others 2000) were
able to prepare microcapsules by using a freeze drying method.

MS 20100327 Submitted 3/25/2010, Accepted 5/15/2010. Authors are with

Dept. of Biosystems and Agricultural Engineering and Robert M. Kerr Food & Agricultural Products Center, Oklahoma State Univ., OK, U.S.A. Direct inquiries to
author Dunford (E-Mail: Nurhan.Dunford@okstate.edu).
Published with approval of the Director, Oklahoma Agricultural Experiment
Station.

E394

Journal of Food Science r Vol. 75, Nr. 6, 2010

It was hypothesized that freeze drying may have advantages over

spray drying. This is because freeze drying limits fish oil exposure
to high temperatures that are required for spray drying. Furthermore, freeze drying is carried out under vacuum. Therefore, there
is a smaller possibility to catalyze oxidation of fish oil at low temperatures and in the absence of oxygen during the microencapsulation process. Unfortunately, Heinzelmann study (Heinzelmann
and others 2000) did not compare the properties of microcapsules
prepared with freeze drying to those of spray dried samples. Both
spray and freeze drying require preparation of an emulsion prior
to microcapsule production. Emulsion preparation may also lead
to oxidation of fish oil because of exposure of fish oil to oxygen
during the process (Kolanowski and others 2006b).
Conventional 2-fluid (liquid/gas) pressure spray nozzles have 2
concentric channels in which gas and emulsion flow separately. Gas
pressure and centrifugal forces are used to atomize fluids (Klaypradit and Huang 2008). This nozzle type has been shown to have
some disadvantages such as lack of control over droplet size consequently wide distributions of droplet size and clogging (Bittner
and Kissel 1999). Ultrasonic atomizers employ ultrasonic vibrational energy as a means to atomize fluids (Klaypradit and Huang
2008). As their name implies, ultrasonic nozzles employ high frequency sound waves, those beyond the range of human hearing. In
general, high frequency nozzles are smaller, create smaller drops,
and consequently have smaller maximum flow capacity than nozzles that operate at lower frequencies. An important characteristic of ultrasonic nozzles is that they generate a soft spray which
dramatically reduces overspray and minimizes clogging. These
nozzles are recommended when extremely low flow rates are
required. Another advantage of the ultrasonic nozzles is the
R

C 2010 Institute of Food Technologists
doi: 10.1111/j.1750-3841.2010.01708.x

Further reproduction without permission is prohibited

ability to produce droplets with uniform size distribution (Topp

and Eisenklam 1972). Bittner and Kissel (1999) were able to produce microcapsules using an ultrasonic nozzle that had particle
size and encapsulation efficiencies that were within the range of
conventional spray drying nozzles.
There are also pressure and sonic nozzles that are designed for 3fluids (gas/liquid/liquid) and 2-fluids (liquid/liquid), respectively.
When these nozzles are used for microencapsulation applications,
oil and wall material flow in separate channels and do not mix
until they meet at the tip of the nozzle. Utilization of these nozzles eliminates the need for emulsion preparation prior to drying.
Hence oil handling and oxidation can be minimized. To the best of
our knowledge, there is no study examining physical and chemical properties of microcapsules prepared with fish oil-whey protein
isolate by using 2- and 3-fluid pressure and sonication nozzles.
Our hypothesis is that spray drying nozzles where oil is mixed
with wall material at the point of atomization will produce microcapsules with similar or better characteristics than those produced
by freeze drying and conventional spray nozzles. The new nozzle designs will eliminate the need for emulsion preparation prior
to spray drying. Ultrasonic nozzles will produce more uniform
microcapsules compared to pressure atomizing spray nozzles. The
objective of this study was to produce fish oil microcapsules by
different microencapsulation techniques and evaluate the physical
and chemical properties of the microcapsules.
In this study fish oil was encapsulated in whey protein isolate
(WPI) because of its reported health benefits. WPI has been shown
to be an ideal protein supplement for increasing lean muscle while
at the same time helping to reduce fat in humans (Frestedt and
others 2008). It is expected that fish oil encapsulated in WPI will
deliver health benefits of both fish oil and WPI while delivering a
product with extended shelf life. Furthermore, use of WPI eliminates the requirement for addition of a surface active ingredient
to form an emulsion prior to generation of microcapsules because
of the emulsifying properties of proteins. Moreau and Rosenberg
(Moreau and others 1993) stated that WPI exhibited effective microencapsulation properties.

Materials and Methods

Sample characterization and storage
Refined menhaden oil containing 500 mg/kg mixed tocopherols and 200 mg/kg tert-butylhydroquinone was obtained from
a commercial processor. Fish oil was shipped frozen in 4 L jugs.
Once received the fish oil was split into smaller glass bottles and
the head space was filled with nitrogen. The fish oil was then
stored in a 80 C freezer.
Microcapsule preparation
Emulsion preparation. BiPro WPI containing 97.8% 2%
protein was purchased from Davisco Foods Intl. (Eden Prairie,
Minn., U.S.A.). The functional protein groups of the WPI comprised beta-lactoglobulin and alpha-lactalbumin. A 20% (w/w)
solution of WPI in de-ionized water was used for the experiments
because higher concentrations were determined to be too viscous
for spray drying. A 20% WPI solution was also within the wall
material concentration recommended for oil encapsulation, 10%
to 30% (Rosenberg and Young 1993). Fish oil to WPI ratio was
1:2 by weight. First, a polytron electric homogenizer equipped
with a small probe (PowerGen 700, Omni Intl., Marietta, Ga.,
U.S.A.) was used to create a coarse emulsion by homogenizing the
oil protein mixture for three 2 min periods. Then a fine emulsion

was created by using a Misonix Sonicator 3000 sonic probe (output frequency 20 KHz) (Farmingdale, N.Y., U.S.A.). The coarse
emulsion was exposed to sonic energy for three 2 min periods,
allowing the emulsion to cool in between periods. The emulsion
was kept in an ice bath at all times during these processes and
reached a maximum temperature of 22 C.
Freeze drying. The oil-WPI emulsions were frozen at
80 C in an ultra-freezer (Bio Freezer 8517, Forma Scientific,
Waltham, Mass., U.S.A.). After 24 h, the frozen emulsion was
dried for 48 h at 40 C and 0.13 millibar (25 L Sentry Freezemobile, VirTis Co. Inc., Gardiner, N.Y., U.S.A.). The product
was a dry matrix of microcapsules. The cross-links between microcapsules were broken by using a coffee grinder (SmartGrind,
Black&Decker, Towson, Mass., U.S.A.) (5 s grinding periods 5
times shaking) resulting in a free-flowing powder.
Spray drying with 2-fluid pressure nozzle. A Buchi-290
spray dryer (B-290, Flawil, Switzerland) equipped with a 2-fluid
(liquid/gas) Buchi pressure nozzle and in conjunction with the
B-296 de-humidifier (B-296, Flawil, Switzerland) equipped with
a pre-heat exchanger was used for the microencapsulation experiments. The previously prepared emulsion was dried in a nitrogen
environment where compressed nitrogen gas (Airgas, Tulsa, Okla.,
U.S.A.) is circulated through the spray dryer. The evaporated moisture was passed through the de-humidifier and condensed into a
collection bottle. Inlet temperature of nitrogen gas was 180 C.
Outlet temperature, which is dependent on inlet temperature, was
90 2 C. The emulsion was delivered to the nozzle via a peristaltic pump which was built in the spray drying system at 10%
speed (2.75 mL/min).
Spray drying with 3-fluid pressure nozzle. The B-290
spray dryer was equipped with a 3-fluid (gas/liquid/liquid) pressure nozzle (Buchi 46555, Flawil, Switzerland). Whey protein solution and the fish oil were pumped to the nozzle via a peristaltic
and a syringe pump (12-05126, Sono-Tek, Milton, N.Y., U.S.A.),
respectively. The WPI solution was 20% solids (w/w) in water.
The pump rate of the peristaltic pump was 10% (2.75 mL/min).
The ratio of fish oil to WPI was 1:2 (w/w). Fish oil density was
taken as 0.930 g/mL, according to the supplier, for conversion of
fish oil volume to weight. As the previous experiments with 2fluid nozzle the atomized microcapsules were dried in a nitrogen
environment. During these experiments oil, wall material and gas
flow in separate channels and did not mix until they met at the tip
of the nozzle and atomized.
Spray drying with 2-channel ultrasonic nozzle. For these
experiments the B-290 spray dryer was equipped with a 2-liquid
channel 120 kilohertz ultrasonic atomizing nozzle (Sono-Tek,
Milton, N.Y., U.S.A.). The sonic nozzle was powered with a Broad
Ultrasonic Generator (Sono-Tek, 06-05108) at a setting of 5 watts.
The experimental conditions were the same as described in the
previous paragraph. Similar to the experiments described in the
previous section, oil and wall material flowed in separate channels and did not mix until they met at the tip of the nozzle and
were atomized. In these experiments atomization did not require
gas pressure. The sonication was used for this purpose. Nitrogen
gas was circulated through the nozzle to help keep the nozzle
cool. Thermocouple readings indicated that the nozzle reached a
maximum temperature of 50 C during the drying process.
Moisture content and water activity. A Karl Fischer titrator (758 KFD Titrino with 703Ti stand, Metrohm U.S.A. Inc.,
Riverview, Fla., U.S.A.) was used to determine the moisture content of dried powder samples and the fish oil. The instrument
was calibrated using water. For the fish oil approximately 3 g
Vol. 75, Nr. 6, 2010 r Journal of Food Science E395

E: Food Engineering &

Physical Properties

Fish oil encapsulation . . .

Fish oil encapsulation . . .

The following equation was used to calculate microencapsuwas used as the sample size. For dried powder samples 0.4 g was
the sample size used. Samples were dispersed in Hydranal-Solvent lation efficiency (MEE) using the determined total oil and the
CM (Sigma-Aldrich, St. Louis, Mo., U.S.A.) and titrated with surface extractable oil (Jimenez and others 2004).
Hydranal-Titrant 2 (Sigma-Aldrich). Water activity of the samples
MEE = [(total oil extractable oil) 100]/total oil
was measured by using an AquaLab Water Activity Meter at 25 C
(Series 3, Decagon Devices Inc., Pullman, Wash., U.S.A.).

E: Food Engineering &

Physical Properties

Total oil
Soxtec extraction. A Soxtec oil extraction unit (Tecator,
Model 1043 Extraction Unit, Sweden) was used to extract the
total oil from the microcapsules. Approximately 2 g of sample
was weighed into extraction thimbles and mixed with Celite 545
(EMD Chemicals Inc., Gibbstown, N.J., U.S.A.). The thimbles
were loaded onto the instrument along with pre-weighed cups
containing 40 mL of ACS reagent grade petroleum ether (Fisher
Chemical, Fairlawn, N.J., U.S.A.). The thimbles were lowered into
the boiling position for 10 min then raised into the rinse position
for 20 min. The cups were removed and any residual petroleum
ether was dried away. The difference in weight of the cups with
and without oil was recorded as oil extracted. The thimbles were
also dried. Once dried the remaining sample was ground in with
a mortar and pestle and placed back into the extraction thimbles
for a 2nd extraction. The oil extracted from both extractions was
added to equal the total oil.
Solvent extraction. A 2nd method for total oil was used to
confirm the results obtained by Soxtec extraction. Solvent extraction of total oil was done based on the RoseGottllieb method
(GEA 2005). Total of 2 g of encapsulated oil sample was weighed
out into a flask. Total of 20 mL of water were added to disperse the
sample. Then the solution was placed in a water bath for 15 min
at 60 C, shaken occasionally. The mixture was then cooled and
25 mL of petroleum ether was added and mixed for 10 min. The
mixture then was allowed to stand for at least 2 h until the ether
phase was clear and a clear phase separation was observed between
water and petroleum layers. The ether phase was then transferred
into an Erlenmeyer flask and this extraction was performed 2 more
times using the same flask of water phase. After the final transfer
the ether was evaporated using a Rapid-VapC vacuum system
(Model 7900002, Labconco, Kansas City, Mo., U.S.A.). The flask
was allowed to cool under vacuum and weighed.
Total Oil (%, w/w) = (W1 100)/W2
W1 = weight in grams of the evaporation residue.
W2 = weight in grams of the power used.

Surface extractable oil

Surface extractable oil fraction also known as the accessible
or nonencapsulated oil was determined (ModifiedEA Niro
Method A 10a) (GEA 2005). Total of 2 g of encapsulated oil sample
were placed into a 25 mL flask. Total of 10 mL of petroleum-ether
were added. The flask was closed and placed in a shaking device.
The stirring speed was regulated so that the powder was moving but not splashing up on the upper sides of the flask. After
15 min shaking was stopped and the solution was filtered into
a preweighed glass beaker and washed 2 more times with 10 mL
petroleum-ether. Petroleum ether was completely evaporated from
the filtrate under vacuum at 45 C (Rapid-VapC vacuum system
7900002, Labconco, Kansas City, Mo., U.S.A.).
Free oil (%, w/w) = (a 100)/(b)
a = weight of residue in the flask in grams.
b = grams of powder used.
E396 Journal of Food Science r Vol. 75, Nr. 6, 2010

Particle size analysis

A Malvern High Performance Particle Sizer (HPPS 5001,
Malvern Instruments, Ltd, Worcestershire, United Kingdom) was
used to determine the average size of the microcapsules. Dried
microcapsules were dispersed into inert silicone oil (silicone fluid
350 100% pure silicone, Clearco Products Co, Bensalem, Pa.,
U.S.A.) for the analysis. Samples were prepared at a concentration
of 5% (w/v) microcapsules in mineral oil by vortexing at 3000
rpm for 1 min. Measurements were carried out at 25 C. Refractive index of the silicone oil was 1.476. The particle size analyzer
performed 20 scans per sample and displayed an average diameter
value.
Bulk density
The bulk density of the dried powders was calculated by measuring the weight of 15 mL of noncompacted powder in a preweighed
tube. The weight of the sample was divided by the volume to equal
gram per milliliter.
Surface morphology analysis
Samples were mounted on cylindrical stubs which were fitted
with double coated conductive carbon tape. Then a sputter coater
was used to coat the sample with gold atoms. A scanning electron
microscope (FEI Quanta 600, FEI Co., Hillsboro, Oreg., U.S.A.)
was used to analyze the surface morphology of the dried powders. Digital images where obtained at 3 magnifications, 1000,
5000, and 30000.

Statistical Analysis
All analytical tests and microencapsulation experiments were
carried out at least in duplicate and in randomized order with
the mean values being reported and separated by Least Significant
Difference (LSD) at = 0.05. Analysis of variance (ANOVA)
of the results was performed using SAS for Windows (Software
Version 9.1. SAS Insti. Inc., Cary, N.C., U.S.A.).

Results and Discussion

Chemical and physical characteristics of microcapsules
Moisture content and water activity. Moisture content
of microcapsules and WPI used as wall material are shown in
Table 1. The moisture content specified by the WPI supplier was
5% (w/w). However, our laboratory tests showed a higher moisture content, 7.7% (w/w), for this product. Higher moisture of
Table 1 Moisture content of the samples determined by Karl
Fischer Titration.
Sample
Fish oil
WPI
Freeze dried
2-Fluid pressure nozzle
3-Fluid pressure nozzle
Ultrasonic nozzle

Moisture
(%, w/w)

aw A

0.06 4E-4a
7.7 0.2b
4.5 0.2c
2.7 0.03d
5.3 0.1e
4.2 0.08f

0.57 0.01a
0.25 6E-4b
0.21 3E-3c
0.15 3E-3d
0.20 6E-4c
0.15 1E-3d

Means with the same letter within the same column are not significantly different (P >
0.05).

the product might be due to moisture absorption during storage. The food industry has specified that dried powders should
have moisture content between 3% and 4% (Masters 1991). The
moisture content of microcapsules produced by spray drying with
2-fluid pressure nozzle was well below the specified maximum.
Microcapsules produced by freeze drying and spray drying with
the ultrasonic nozzle were near the 4% maximum while the 3-fluid
pressure nozzle microcapsules were higher than the 4% maximum.
Although there were statistically significant differences in moisture
content of encapsulated products the variations were not large for
practical purposes.
Water activity (aw ) is one of the most critical factors in determining quality and safety of the foods and affects the shelf life,
texture, flavor, and smell of foods. Water activity was determined
for the 4 microcapsule products along with WPI and fish oil (Table 1). As expected all the samples had low water activity. Our
findings were in agreement with the literature (Klinkesorn and
others 2006). Sonic and 2-fluid pressure nozzles had the lowest
water activity. High moisture content and water activity of the
product could lead to shorter shelf life and deterioration of food
quality.
Total oil. Total oil describes the percent of oil that makes
up the dried powder. Total 2 oil extraction methods were used
to determine total oil content in microcapsules (Table 2). The

values determined by 2 different extraction methods were not

significantly different. Among the 4 microcapsule products total oil
content in microcapsules obtained by using the ultrasonic nozzle
(about 28%, w/w) was significantly lower than that of other 3
microcapsule products. According to the literature oil content
of microcapsules may vary between 20% and 50% (Drusch and
Schwarz 2005). All the microencapsulated products examined in
this study were within the range reported in the latter study.
Surface extractable oil. The surface extractable oil or free
oil is often defined as the oil that may be extracted with organic
solvents from the surface of unbroken microcapsules. The values
in this study were determined to be significantly different among
all 4 products (Table 3). The pressure nozzle with 2-fluid channels
gave the best results with lowest surface oil, 2.6% while capsules
prepared by using the sonication nozzle had the highest amount
of surface oil, 6.8%. In general free oil contents of the microcapsules examined in this study were similar or lower than the values
reported in the literature (Heinzelmann and others 2000).
Microencapsulation efficiency. MEE is calculated to determine the amount of oil that was successfully encapsulated based
on the values obtained for total oil and surface extractable oil.
Previous research has shown that the MEE can be directly affected
by the materials and process used for production of microcapsules with efficiencies ranging from 0% to 95% (Lin and others
1995; Hardas and others 2000; Heinzelmann and others 2000;
Table 2Total oil content of microcapsules.
Hogan and others 2001; Baik and others 2004; Klinkesorn and
A
Soxtec extraction
RoseGottlieb solvent
Sample
oil (%, w/w)
extraction oil (%, w/w) others 2006; Velasco and others 2006). The values calculated for
this study are displayed in Table 3. There were significant differFreeze dried
31.9 1.1a
31.7 0.5a
ences among MEE of all the products examined in this study. The
2-Fluid pressure nozzle
31.3 0.6a
31.0 0.6a
2-fluid nozzle had the highest (91.6%) while the ultrasonic noza
a
3-Fluid pressure nozzle
31.3 0.8
30.8 0.4
zle had the lowest efficiency (76%). We believe that this was
Ultrasonic nozzle
28.5 0.9b
28.0 1b
A
Means with the same letter within the same column are not significantly different (P > due to inconsistent function of the ultrasonic nozzle. It was ob0.05).
served that ultrasonic nozzle plugged from time to time impeding
Table 3Properties of microcapsules.

Sample

Surface oil
(%, w/w)

MEE
(%)

Average diameter
(m)

Bulk density
(g/mL)

Freeze dried
2-Fluid pressure nozzle
3-Fluid pressure nozzle
Ultrasonic nozzle
WPI

5.3 0.08a
2.6 0.03b
4.4 0.11c
6.8 0.07d

83.3 0.1a
91.6 0.1b
85.8 0.08c
76.1 0.5d

56.2
7.3
12.0
11.3

0.18 0.01d
0.20 3.0E-03c
0.25 0.01ab
0.24 0.01b
0.26 0.01a

Means with the same letter within the same column are not significantly different (P > 0.05).

60
3-Fluid Nozzle

Mean % Intensity

50

Figure 1Particle size distribution plot of

microcapsules.

2-Fluid Nozzle
Ultrasonic Nozzle

40

Freeze Dried
30
20
10
0
5500

14000

24000

34000

44000

54000

Diameter (nm)

Vol. 75, Nr. 6, 2010 r Journal of Food Science E397

E: Food Engineering &

Physical Properties

Fish oil encapsulation . . .

Fish oil encapsulation . . .

atomization briefly during drying. It is likely that lack of atomization lead to higher surface oil on the particles formed right
after atomization re-started. Low encapsulation efficiency can be
attributed improper nozzle function.
Particle size analysis. The average particle size diameter of
the microcapsules was determined (Table 3). Freeze dried microcapsules had the largest average particle size at 56.2 m. Mi-

crocapsules produced with the 2-fluid pressure nozzle were the

smallest at 7.3 m followed by the ultrasonic nozzle and 3-fluid
pressure nozzle at 11.3 and 12.0 m, respectively. A plot of % intensity versus diameter helps show the size distribution around the

E: Food Engineering &

Physical Properties
Figure 2SEM picture of fish oilWPI microcapsules produced by freeze
drying at 3 different magnifications: A: 1000, B: 5000, C: 30000.

E398 Journal of Food Science r Vol. 75, Nr. 6, 2010

Figure 3SEM picture of fish oilWPI microcapsules produced by spray

drying using a 2-fluid pressure nozzle at 3 different magnifications: A:
1000, B: 5000, C: 30000.

Fish oil encapsulation . . .

E: Food Engineering &

Physical Properties

average (Figure 1). The graph indicates that the ultrasonic nozzle This finding supports the hypothesis that the ultrasonic nozzle
microcapsules had the most narrow size distribution, followed by produces more uniform particle size than the other nozzle types.
the 2-fluid nozzle, 3-fluid nozzle, and freeze dried microcapsules.
Bulk density. Bulk density is a very important parameter to
characterize food powders. It may vary with water content in

Figure 4SEM picture of fish oilWPI microcapsules produced by spray Figure 5SEM picture of fish oilWPI microcapsules produced by spray
drying using a 3-fluid pressure nozzle at 3 different magnifications: A: drying using an ultrasonic nozzle at 3 different magnifications: A: 1000,
1000, B: 5000, C: 30000.
B: 5000, C: 30000.

Vol. 75, Nr. 6, 2010 r Journal of Food Science E399

Fish oil encapsulation . . .

E: Food Engineering &

Physical Properties

product, and is dependent on the rate of shrinkage, which in turn

is strongly affected by the drying method (Van Arsdel and
Copley 1964). Spray dried products have to meet bulk density
targets to provide consistent weight during packaging. Bulk density was determined for each of the dried products (Table 3). The
bulk density determined for the powders was considered unpacked
or aerated, because samples were not compacted. Bulk density of
all the microcapsules was lower than that of the WPI. As expected
freeze dried samples had the lowest bulk density followed by capsules produced with ultrasonic nozzle. There was no significant
difference in bulk density of microcapsules produced by ultrasonic
and 3-flluid nozzles.
Surface morphology. The surface morphology of the samples was observed by SEM. Figure 2 through 5 display images
captured for each dried microcapsule product at the same 3 magnifications (1000, 5000, and 30000).
Freeze dried microcapsules were irregular in shape and lacked
uniformity having a wide frequency of microcapsule sizes (Figure 2A to 2C). The surface of freeze dried capsules revealed fairly
large surface cracks at higher magnifications. The microcapsules
produced with the 2-fluid nozzle were more uniform in shape
being round with some surface dents (Figure 3A to 3C), which
may be associated with mid-air collisions during the spray drying
process and improper atomization and drying rate (moisture rate).
Moreau and Rosenberg (Moreau and others 1993) have also observed that some surface dents are present on the surface of whey
derived spray dried powders that have been attributed to improper
atomization and drying rate. Although it was less than the freeze
dried samples, the 2-fluid nozzle microcapsules also showed wide
particle size distribution lacking complete uniformity. The surface
of the 2-fluid nozzle microcapsules did not reveal any observed
surface cracks.
Microcapsules produced from the 3-fluid nozzle revealed round
and some irregular shapes with surface dents (Figure 4A to 4C).
Although the microcapsules were not completely uniform the
frequency of larger to smaller capsules was observed to be less for
3-fluid nozzle in comparison to 2-fluid nozzle. The surface of the
3-fluid nozzle microcapsules did not reveal any observed surface
cracks. There were, however, creases and blisters observed on the
surface.
The ultrasonic nozzle produced round microcapsules with some
irregular shapes (Figure 5A to 5C). It is plausible that irregularly shaped particles were formed when atomization was intermittent due to plugging of the nozzle during the drying process. However, as mentioned earlier the ultrasonic nozzle showed
a significantly narrower particle size distribution than the other
nozzles.

Conclusions
To the best of our knowledge this is the first study to contrast microencapsulation technologies that utilize multiple fluid delivery
and sonic energy with traditional spray and freeze dried emulsion
microencapsulation methods. Comparison of chemical and physical characteristics revealed that ultrasonic nozzle did have one
advantage. With regard to uniformity of size and shape, microcapsules produced by the 2-channel ultrasonic nozzle were observed
to be more uniform in size and shape, determined by particle size
distribution and SEM image comparisons. Disadvantages were also
observed for ultrasonic nozzle microcapsules having lower oil encapsulating efficiency compared to pressure nozzles and freeze

E400 Journal of Food Science r Vol. 75, Nr. 6, 2010

dried microcapsules at the same core to wall ratio. This may be

due to nozzle clogging during the microencapsulation process.
This study demonstrated that new nozzle designs that eliminate
emulsion preparation for microencapsulation applications can be
viable options to conventional nozzles. However there is still a
need for research on process optimization. For example, in this
study the core (oil) to wall material (WPI) ratio was held constant
in all experiments to maintain comparative solids in the final products. Optimization of core to wall solids needs to be investigated
to increase microencapsulation efficiency for ultrasonic nozzles.
Investigations of other wall materials and combinations of wall
materials may reveal wall systems that are better suited for spray
nozzles that encapsulate core materials at the point of atomization.
Solutions to clogging problem observed with sonic nozzles need
to be further examined.

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