Japan Journal of Food Engineering, Vol. 16, No. 1, pp. 37 - 52, March.

2015

◇◇◇ Review ◇◇◇

Encapsulation of Hydrophilic and Hydrophobic Flavors by Spray Drying

1 2 3 3,†
Apinan SOOTTITANTAWAT , Riitta PARTANEN , Tze Loon NEOH , Hidefumi YOSHII
1
Department of Chemical Engineering, Chulalongkorn University, Pathumwan, Bangkok 10330, Thailand
2
Bioprocessing, VTT Technical Research Centre of Finland, P.O. Box 1000, 02044 VTT, Espoo, Finland
3
Department of Applied Biological Science, Kagawa University, 2393 Ikenobe Miki-chi, Kita, Kagawa 761-0795, Japan

The encapsulation of flavors is the important process in food industry. The encapsulation of flavors
with spray drying and the flavor release from spray-dried powder were reviewed. The hydrophobic
flavor was in the form of emulsion before spray dr ying. Therefore, the researches were mainly
related to the forming of emulsion which wall material containing emulsifier properties are required.
On the other hands, the hydrophilic flavor was mainly related to the antioxidant and coloring flavor
powder. The hygroscopicity of powder and their stickyness during the spray dryer were important
points to improve which the remaining of hydrophilic flavors were less concerned. The morphologies,
and flavor release behavior are important physical properties of the flavor encapsulated powder.
Especially, the correlation equations for the flavor release are summarized in the relation with
Avrami or Weibull equation. The glass transition temperature is important to estimate the collapse
of the powder and the permeation of the powder matrix to flavor compounds. The flavor release
(mass transfer of flavor) rate is affected by temperature difference (T- Tg ). In this review, recent
researches are summarized in the flavor encapsulation in spray drying, especially for tropical flavor
encapsulation.
Keywords: flavor, encapsulation, spray drying, powder, controlled release

1. Introduction
Tropical fruits are of increasing interest to consumers
worldwide. Fabiano et al reviewed the drying of exotic
tropical fruits and indicated the drying method affected
the quality of fruits such as the content of vitamins [1].
The tropical fruits are exotic in flavor. Flavor contents in
the fruits were affected also by the drying conditions and
method. Flavor (aroma) is one of the most important
attributes that affects the consumption of fruit from the
tropics and subtropics. In food industr y, various core
compounds, such as volatile compounds, essential oils,
and oleoresins, are encapsulated with some specific con-
cerns, such as safety usage of solvent and wall material.
The most common and economical way to carr y out
microencapsulation to retain and protect chemically reac-
tive or flavor compounds is spray drying so that it is
widely used in commercial scale. Many research works
related to encapsulation of liquid flavors by spray drying
have been reported [2- 5]. Several researchers investi-
gated the volatile flavor constituents of tropical fruits and
flavor behaviors at storage. Pino and Marbot [6] investi-
gated the volatile constituent of acerola fruits. Tietel et
(Received 17 Jan. 2015: accepted 23 Feb. 2015)
† Fax: 087-891-3021, E-mail: foodeng.yoshii@ag.kagawa-u.ac.jp
al. [7] evaluated the flavor and quality of ‘Or’ and ‘Odem’
mandarins after 4 weeks of storage. Rouseff et al. [8]
reviewed historical review of citrus flavor research dur-
ing the past 100 years. Bicas et al. [9] investigated vola-
tile constituents of exotic fruits from Brazil. They pointed
the flavor in these fruits was a very important factor.
Perez-Cacho and Rouseff [10] reviewed processing and
storage effects on orange juice aroma. They indicated
the flavor compounds were labile compounds and unsta-
ble during the storage. One method is the encapsulation
to form stable flavor form. Madene et al. [4] reviewed the
flavor encapsulation and controlled release. They sum-
marized the flavor release mechanism from the powder
with diffusion, swelling, melting and degradation. Gibbs
et al. [11] reviews also the encapsulation in the food
industry. They showed encapsulation in foods is also uti-
lized to mask odours or tastes. Various techniques are
employed to form the capsules, including spray drying,
spray chilling or spray cooling, extrusion coating, fluid-
ized bed coating, liposome entrapment, coacer vation,
inclusion complexation, centrifugal extrusion and rota-
tional suspension separation. Powder formation of these
flavors is one interesting process of food industr y.
Zuidam and Heinrich [12] edited the book of
“Encapsulation Technologies for active food ingredients
and food processing”. The aroma encapsulation were
38 Apinan SOOTTITANTAWAT, Riitta PARTANEN, Tze Loon NEOH, Hidefumi YOSHII
summarized in the book. Spray drying has been playing
a vital role in the encapsulation and microencapsulation
of functional compounds in food.
The losses of both hydrophilic and hydrophobic fla-
vors during the spray drying were reported in each step
of process. The losses of flavors were occurred first dur-
ing the atomization step. The flavors and water are evap-
orated with the hot inlet air at initial period of drying.
The loss of flavors especially the high volatile flavors
(with low boiling point temperature) was expected in this
period with the temperature of droplet increase. In the
second step with the constant drying periods, the forma-
tion of crust was occurred. The crust was the selective
membrane allows the higher diffusion rate of water than
the flavors resulted the higher remaining of flavor in the
droplet. However, the high solubility flavor as well as
hydrophilic flavor was lost in the higher amount than in
the hydrophobic flavor. The dissolved flavors were loss
during the drying as the water molecule. After the solid
droplets were formed, the loss of flavors was expected to
occur with the change of powder morphology. However,
the losses in this step were less amount comparing to the
first and second steps.
In this paper, the hydropobic and hydrophilic flavors
encapsulation focusing on tropical flavor by spray drying
especially the work published in last decade were
reviewed including the flavor release mechanism as well
as the oxidation of encapsulated flavors.
2. The encapsulated hydrophobic flavors
To encapsulate the hydrophobic flavors by spray dry-
ing, the emulsion of flavors will first to produce under
the wall materials solution. Therefore, the wall materials
with emulsifier properties or the additional of surfactant
are required. Then the flavor emulsion is spray dried to
form the encapsulated flavors powder. The flavor is in the
form of droplet inside the shell wall of powder as the
multi core encapsulated powder. In the past decade, the
research works are studied the effects of each factors on
the flavor retention during spray drying. During the stor-
age with various conditions, the water, oxygen and flavor
itself can diffuse through the shell wall. The stability of
encapsulated flavors during the storage is also widely
investigated.
2.1 Wall materials
Wall materials are one of the most important factors on
the properties of encapsulated flavor powder. The widely
used of wall materials to encapsulated hydrophobic flavor
by spray drying is gum arabic (also known as arabic gum
or acacia gum) and n- octenyl succinic anhydride (OSA)-
modified starch since both of them have the emulsifier
properties. The maltodextrin was also used to blend with
the emulsifier wall materials as the drying aid which was
also prevent the losses of flavor during the spray drying
process. The higher solid content increased the flavors
retention because the rate of crust formation around the
atomized droplet as the selective diffusion membrane for
the flavors is increased. The surfactants were also added
to stabilize the emulsion with less used methods. The
used surfactants are mostly in the form of viscous and
sticky liquid affected to the physical properties as well as
the yield of product. The surfactant can stabilize the
emulsion but it cannot cover the flavor droplet during the
drying periods.
There are some of works that reported the new wall
materials with the emulsifier properties comparing to the
conventional materials of gum arabic and OSA- modified
starch. Drusch [13] reported a novel emulsifying wall
component of sugar beet pectin. Beristain et al. [14- 15]
showed the application of mesquite gum with the high
retention. Xie et al. [16] reported the addition of peach
gum in the emulsion system resulted the smooth surface
of spray dried powder. Hogan et al. [17] used the whey
protein concentrate to encapsulate the soya oil. The
whey protein concentrate offered the surface active prop-
erties required to stabilize emulsion. Hogan et al. [18]
showed the encapsulation with sodium caseinate/matlo-
dextrin blends. Charve and Reineccius [19] evaluated the
potential of selected proteins (sodium caseinate, whey
and soy protein isolates) as alternative materials for fla-
vor comparing to the gum arabic and modified starch.
The highest flavor retention in gum arabic was reported
but protein materials effectively limited limonene oxida-
tion. Calvo et al. [20] studied the microencapsulation of
extra - virgin olive oil by spray - dr ying with proteins
(sodium caseinate and gelatin), gum arabic and malto-
dextrin. A better microcapsule yield, ef ficiency, and
internal- external fat ratio were achieved when a combi-
nation of proteins and polysaccharides was used as the
wall component. Liu et al. [21] used the soybean soluble
polysaccharide to encapsulate the hydrophobic flavors.
The increasing of flavor retention with addition of gelatin
to the emulsion was also reported. The volatile com-
pounds were retained in dry emulsions stabilized by pea
protein isolate/pectin complex. The pectin was able to
preserve the β- sheet secondary structure of pea protein
 Encapsulation of Hydrophilic and Hydrophobic Flavors by Spray Drying
when pea globulins/pectin complexes are heated.
Drusch et al. [22] and Gharsallaoui et al. [23] described
the fundamental physical characteristics of spray-dried
carrier matrices based on sodium caseinate and casein
hydrolyzate. Surface accumulation of proteins at the air-
water interface led to a modified surface composition of
spray-dried carrier matrix particles for microencapsula-
tion. However, the interfacial elasticity was markedly
altered when using hydrolyzed casein as emulsifier,
which is related to a decrease in microencapsulation effi-
ciency. Lipid oxidation during storage of the microencap-
sulated oil increased with the protein content in the for-
mulation. Excess protein led to an increase in free vol-
ume elements and is suspected to increase oxygen diffu-
sion.
Klinkesorn [24] used the two- layered interfacial mem-
branes of lecithin–chitosan to emulsified the tuna oil
combination with the maltodextrin as drying aid materi-
als. The high oil retention levels (>85%) was obtained.
Loksuwan [25] showed the modified tapioca starch as
potential wall material for encapsulation of β-carotene.
The efficacy of pullulan as stabilizer to achieve a stable
emulsion of turmeric oleoresin and its subsequent micro-
encapsulation was investigated. Kshirsagare et al. [26]
and Yang et al. [27] used the konjac glucomannan
(KGM) which have the excellent film forming capability
to encapsulate orange oil. The KGM was hydrolyzed
before used to decrease the viscosity of carrier solution.
Because of the lack of emulsifier properties, the surfac-
tant or gum arabic or OSA-modified starches have to add
in the system.
Furthermore, the combination of encapsulation meth-
ods between the inclusion complex and spray dr ying
were also reported. The cyclodextrins and their deriva-
tives was used to form the inclusion complex of hydro-
phobic flavor and then following by spray drying to form
the dry products. Liu et al. [28] showed the encapsulated
of menthols in β, α and γ- cyclodextrin following with
the single droplet drying process to simulate the loss of
flavor during spray drying process. Kawakami et al. [29]
showed the encapsulation of rice flavor in α-cyclodextrin
and highly branched cyclic dextrin by spray drying.
2.2 Type of hydrophobic flavors
Numerous of works have reported the encapsulation of
flavors as well as the tropical flavors in both of model fla-
vors and natural extracted flavors. Bylaitë et al. [30]
encapsulated the caraway essential oil in mixtures of
whey protein concentrate and malodextrins matrix by
39
spray drying. Partanen et al. [31] reported the microen-
capsulation of caraway extract in β - cyclodextrin and
modified starches. The inclusion complex seemed to pro-
tect volatile substances more efficiently during storage,
whereas microcapsules with modified starches as wall
material were more heat tolerant. Encapsulation of
extracted sea buckthorn kernel oil and the stability of
the products were also investigated. Encapsulation of
extracted sea buckthorn kernel oil in maltodextrin and
emulsifying starch derivative and the stability of the
products were investigated [32]. Teixeira et al. [33]
encapsulated swiss cheese flavor in conventional wall
materials of gum arabic and maltodextrin. The rose oil
which composed of 2 - phenylethanol (50.22%), nerol
(22.34%) and citronellol (19.40%) was also encapsulated
gum arabic and maltodextrin wall materials. The yield of
encapsulated rose oil varied with wall materials (64–70%)
[34]. The model flavor of menthol was also encapsulated
in gum arabic and modified starch. The re- crystallize to
form whisker of menthol during storage was discussed
[35]. Krishnan et al. [36] reported the microencapsula-
tion of cardamom oleoresin using binar y and ternar y
blends of gum arabic, maltodextrin, and OSA- modified
starch as wall materials. Bixin was encapsulated by
spray - dr ying with gum arabic or maltodextrin [37].
Dzondo - Gadet [38] reported the encapsulation of safou
pulp oil in maltodextrins(DE=6). Baranauskiene et al.
[39] reported the encapsulation of natural flavorings of
oregano, citronella and marjoram into skimmed milk
powder and whey protein concentrate. Vaidya et al. [40]
reports on the microencapsulation of cinnamon oleoresin
by spray drying using binary and ternary blends of gum
arabic, maltodextrin, and modified starch as wall materi-
als. Shaikh et al. [41] reports on microencapsulation of
black pepper oleoresin (piperine) by spray-drying, using
gum arabic and OSA- modified starch as wall materials.
The encapsulation of peppermint oil in modified starch
was also reported with the encapsulation efficiency about
80 percent [42]. About 60 percent encapsulation effi-
ciency of cold pressed avocado oil using whey protein
and maltodextrin was reported [43]. Bae et al. [43] and
Jimenez et al. [44] reported the encapsulation of conju-
gated linoleic acid in whey protein concentrate and gum
arabic. Ahn et al. [45] studied the encapsulation of high
oleic sunflower oil. The lipid oxidation of encapsulated
sunflower oil was remarkable decreased with the addi-
tion of the mixed natural antioxidants extract to the sys-
tem. Natural Canthaxantin was encapsulated in soybean
soluble polysaccharides. The results showed the oxida-
40 Apinan SOOTTITANTAWAT, Riitta PARTANEN, Tze Loon NEOH, Hidefumi YOSHII
tion was more suppressed for the microcapsules pre-
pared from the emulsion having smaller droplets [46].
Touré et al. [47] reported the microencapsulation of gin-
ger oil in maltodextrin(DE=18)/whey protein isolate
with the application of the higher pressure homogeniza-
tion. The best conditions for higher retention at 93 per-
cent were found. The influence of some process condi-
tions on the microencapsulation of flaxseed oil (vegeta-
ble sources of ω- 3) in gum arabic by spray drying was
reported [48]. Rodea- González [49] reported the encap-
sulation of chia essential oil in whey protein concentrate-
polysaccharide matrices. Ko et al. [50] produced the
encapsulated allyl isothiocyanate (AITC) in gum arabic
and chitosan materials via spray drying. Lim et al. [51]
investigated the influence of the composition of the wall
material on the encapsulation and stability of microen-
capsulated red- fleshed pitaya seed oil by spray dr ying.
The study on oil retention revealed that sodium casein-
ate > whey protein > gum arabic as effective wall materi-
als for pitaya seed oil encapsulation. Rubilar et al. [52]
prepared the formulation of soup powder enriched with
ω- 3 fatty acids of linseed oil in gum arabic/maltodex-
trin mixture. Recently, the encapsulation of multiflavors
bergamot oil in gum arabic and modified starch were
studied. The transformation among each flavor to give
the retention higher than 100 percent was discussed
[53].
3. The encapsulated hydrophilic flavors
To encapsulate the hydrophilic flavors, the aqueous
solution of flavor and carrier solid was prepared. Then,
the aqueous mixture was spray dried. The flavors are dis-
persed and encapsulated in the dried carrier solid in the
form of matrix type.
The researches work is now aim to improve the physi-
cal properties of the powder. The main problem of the
natural hydrophilic flavors is the content of the soluble
solid as low molecular of saccharide in the extract aque-
ous flavor which is a cause of the stickyness and the high
hydroscopicity. Therefore, the research is aim to
improve the hygroscopicity of product as well as to
decrease the sticky of obtained powder during the spray
drying. The maltodextrin was normally used as the dry-
ing aid agents to the system. The higher maltodextrin
content decreased the stickyness and hygroscopicity of
the product. The gum arabic was also used because of its
excellent film forming properties even the emulsifier
properties are not required in this system. However, the
quality of the product as the flavor concentration in dry
basis was decreased. Numerous works was done to
improve these problems rather than the retention of fla-
vor in the powder products.
3.1 Wall materials
Some new wall materials and wall materials systems
were applied to solve the stickyness and hygroscopic
properties problems with high flavor content. Oliveira et
al. [54] showed the potential using of cashew tree gum to
partially replace the conventional maltodextrin as drying
aid agent in spray dr ying of cashew apple juice. The
retention of ascorbic acid was increased with the
decreasing of powder hygroscopicity especially when the
ratio of cashew tree gum to maltodextrin is higher than
50%.
Recently, the protein compounds were added to the
feed solution in the small amount to increase the hygro-
scopic proper ties instead of adding high content of
maltodextrin. Jayasundera et al. [55] reported the pow-
der recover y up to 80% of amorphous fructose and
sucrose powder with the addition of sodium caseinate at
7.89% and 0.13% respectively. The protein compounds in
the emulsion were reported to form the film and crust
around atomized droplet during the drying process. Kim
et al. [56] reported the surface composition of spray
dried of milk powder. The results showed that the sur-
face composition is very much different from the bulk
composition of powders. A maltodextrin/apple pectin
based matrix was used to encapsulate the plant extracts.
The bioactive polyphenols and moisture content of the
particles or the antioxidant activity appeared significantly
modified [57].
3.2 Type of hydrophilic flavors
There are numerous of works reported the encapsu-
lated hydrophilic flavors such as juice powder and colo-
rant powder. In general, for the hydrophobic and hydro-
philic flavors which have the close molecular weight
and normal boiling point, the retention of hydrophilic
flavors during the spray dr ying are lower than the
retention of hydrophobic flavors as the mechanism
explained above. However, the low amount of remaining
flavor in the powder is enough for the application of
juice powder as well as the colorant product. As men-
tion before, almost of the works done in encapsulate
hydrophilic flavor the stickyness and hygroscopicity of
product are concerned with a few reported of colorant
retention. Amaranthus betacyanin extracts were spray-
 Encapsulation of Hydrophilic and Hydrophobic Flavors by Spray Drying
dried using a range of maltodextrins (DE10- 25) and
starches (native/modified) as car rier and coating
agents. Adding maltodextrins and starches significantly
reduced the hygroscopicity of the betacyanin extracts
and enhanced storage stability [58]. The extracted 2-ace-
tyl-1- pyrroline odor of rice flavor was encapsulated in
gum arabic and maltodextrin [59]. Shiga et al. [60] devel-
oped the encapsulated extracted shiitake flavors powder
by spray drying. The mixture between cyclodextrin and
maltodextrin was used as carrier. A heat treatment to
increase the lenthionine before the spray drying was rec-
ommended. Cactus pear juice powder was produced with
maltodextrin with different DE values. The retention of
vitamin C as well as the powder properties was also
reported [61]. Cano- Chauca et al. [62] investigated the
induction of crystallization on powder mango juice dur-
ing the process of spray drying and the correlation of the
microstructure of the powder obtained with the func-
tional properties of stickiness and solubility. The malto-
dextrin, gum arabic and waxy starch were used as wall
materials with the additional of cellulose. They reported
that the cellulose as a substance that induces crystalliza-
tion of sugar is not suitable. Immature acerola juice pow-
der was prepared by spray drying with maltodextrin and
gum arabic. The ratio of juice solid to carrier was 1:1.
The glass transition temperature and the stickiness of
the powder was discussed [63]. The raisin juice powder
was produced with maltodextrins as drying aid agents. It
was shown that the lower the DE of the maltodextrin
used, the lower the temperature of drying air at the inlet
and the lower the concentration of drying aid in the feed
were required for successful powder production [64].
The watermelon powder was produced with maltodex-
trin. Addition of maltodextrin reduced the stickiness of
the products and altered the physicochemical properties
of the spray-dried powders. The loss of lycopene and
carotene occurred at higher inlet temperatures [65].
Microencapsulation of anthocyanin pigments of black
carrot by spray drying with maltodextrin (DE 10, 20, 30)
was reported. The highest anthocyanin content powder
was found in DE20 of maltodextrin. The higher air inlet
temperature the higher anthocyanin losses [66]. Gong et
al. [67] produced the instant bayberry powder by spray
drying following with the agglomeration process. Tonon
et al. [68] studied the influence of spray drying condi-
tions on the physicochemical properties of açai powder
with maltodextrin DE 10 as carrier. The curcumin pig-
ments was also produced by spray drying using porous
starch and gelatin [69]. A powder food colorant was
41
obtained by spray dr ying of puntia stricta fruit juices
with glucose syrup (DE 29) as drying aid. Color was
retained during the drying process (>98%) and drying
yield was high (58%) [70]. Moreira et al. [71] assessed
the impact of some processing parameters on moisture
content, flowability, hygroscopicity and water solubility
of spray dried acerola pomace extract using maltodextrin
and cashew tree gum as drying aids. Bakowska-Barczak
and Kolodziejczyk [72] prepared the encapsulated black
currant berries in maltodextrin (DE 11, 18 and 21) and
inerlin by spray drying. The retention of black currant
polyphenol compounds and their antioxidant activity was
investigated. The DE11 of maltodextrin had not only
higher drying yield but also offered better protection for
phenolics during storage. Pomegranate bioactive com-
pounds (polyphenols and anthocyanins) of juice were
encapsulated with maltodextrin or soybean protein iso-
lates by spray dr ying. The polyphenols encapsulating
efficiency was significantly better in soybean protein iso-
lates matrix whereas for anthocyanins was in maltodex-
trin matrix [73]. Kha et al. [74] reported a good quality
gac powder in terms of colour, carotenoid content and
total antioxidant activity can be produced by spray dry-
ing at low inlet temperature (120 ºC) and adding malto-
dextrin concentration at 10% w/v. Chin et al. [75]
reported the stability of encapsulated durian powder by
spray drying. Gum arabic, maltodextrin and N-Lok were
used as wall materials. The retention of maker volatile
compounds (two esters and two sulfides) was investi-
gated during spray drying and storage. The retention of
flavors was in the rage of 20- 70%. The study demon-
strated that volatiles with larger molecular weight tended
to retain better during spray drying. However, the stabil-
ity during storage was still low. Nayak and Rastogi [76]
reported that maltodextrin is an effective drying aid for
production of microencapsulated anthocyanin from gar-
cinia indica. Addition of gum acacia and tricalcium phos-
phate fur ther reduced the hygroscopicity as well as
increasing the stability of the pigments. Goula and
Adamopoulos [77] investigated the development a new
technique for spray dr ying orange juice concentrate
using dehumidified air as drying medium and maltodex-
trin as drying agent. They indicated the hygroscopicity
and degree of caking decrease with an increase in inlet
air temperature and maltodextrin concentration and a
decrease in maltodextrin dextrose equivalent and the
combination of maltodextrin addition and use of dehu-
midified air as drying medium seems to be an effective
way of producing a free-flowing orange powder. The pro-
42 Apinan SOOTTITANTAWAT, Riitta PARTANEN, Tze Loon NEOH, Hidefumi YOSHII
duction of bayber r y polyphenols powder with MD
(DE10) by spray drying with the retention of phenolic
content and total anthocayanins after spray dr ying at
about 95% was reported [78]. The water extract of the
mountain tea was spray- dried by using β- cyclodextrin,
gum arabic and maltodextrins as carrier materials. The
product yield increased with the addition of the carrier
materials whereas decreased at higher drying tempera-
tures [79]. Suhaimi et al. [80] carried out to determine
the effect of different ratios of pineapple juice to malto-
dextrin as a carrier agent. These results suggested that
the ratio of pineapple juice solid to maltodextrin at 40:60
produced the highest powder output at 84.85% recovery.
Yousefi et al. [81] reported the pomegranate juice was
diluted to 12° Brix and carriers (maltodextrin, gum ara-
bic, waxy starch) were added with varying concentra-
tions of cellulose before being reduced to powder by
spray dr ying. The gum arabic still showed the most
effective carriers. The production of pomegranate juice
powder with DE6 of maltodextrin was also investigated.
The results showed that inlet temperature had a great
influence on the physicochemical proper ties of the
spray- dried powders. The antioxidant capacity of the
sample increased with increasing air inlet temperature.
However, the total phenolics content of the samples was
not affected by temperature [82]. Furthermore, also to
produce the pomegranate juice powder, Vardin and Yasar
[83] showed the optimization of pomegranate juice
spray-drying as affected by temperature and maltodex-
trin content. Solval et al. [84] developed a cantaloupe
juice powders from fresh cantaloupe fruit by spray dry-
ing. The 10 wt% maltodextrin solution was used as a car-
rier. The results indicated that the inlet air temperature
of the spray dryer can affect vitamin C and β-carotene
contents of cantaloupe juice powders. Caparino et al.
[85] showed the effect of dr ying methods (refractance
window dr ying, freeze dr ying, drum dr ying and spray
dr ying) on the physical properties and microstructures
of mango powder. The maltodextrin was used as carrier
for the spray dr ying technique. The higher porosity or
lower bulk density in spray- dried mango powder was
due to the addition of maltodextrin. The spray dried
powder showed the least hygroscopic comparing to
other types of dr ying. Wang and Zhou [86] character-
ized of spray- dried soy sauce powders using maltodex-
trins. Maltodextrin concentration and DE value greatly
influenced the caking strength of the soy sauce pow-
ders.
4. Effects of related factors on the retention of
the flavor and properties of encapsulated powder
The properties of wall materials, flavors, emulsion as
well as the spray drying parameters have been reported
to affect the retention and properties of obtained encap-
sulated flavor powder. In this paper, some of the works
that reported to each property were reviewed. Mongenot
et al. [87] showed the ultrasound emulsification on
cheese aroma encapsulation. The use of ultrasound is
particularly effective to obtain a stable emulsion with
maltodextrin as support, which is known for poor emulsi-
fication properties. Buffo et al. [88] study the effect of
agglomeration process of fluidization on the retention of
flavor in the powder. Flavors retention was not adversely
affected by the secondary processing as long as agglom-
eration did not promote structure collapse. Finney et al.
[89] report the effects of type of atomization and process-
ing temperatures on the physical properties and stability
of spray-dried flavors. Type of atomizer and inlet air tem-
perature did not af fected to the total oil content.
However, the centrifugal atomizer gave the higher sur-
face oil content than spray nozzle type. This study added
factual evidence to strengthen the hypothesis that shelf
life depends primarily on the porosity of dried particles
and confirmed that surface oil is not a significant deter-
minant of shelf life. Cho and Park [90] showed the dou-
ble encapsulation of limonene powder by coating the
powder with wax oil. The double encapsulated limonene
was consistently stable without the oxidation.
Soottitantawat et al. [91] reported the effect of flavor
emulsion size on their retention after spray drying. The
large emulsion size gave the low flavor retention in both
of non- soluble and partly- soluble flavors because the
droplet was sheared during the atomization process.
However, for the small emulsion size give the higher
retention of non-soluble flavor but give the lower reten-
t i o n i n t h e c a s e o f p a r t l y - s o l u b l e f l a v o r.
Microencapsulation by spray dr ying of multiple emul-
sions containing carotenoids was reported to improve
their properties [92]. Turchiuli et al. [93] investigated
the feasibility of encapsulation of a vegetable oil used as
a model into a mixture of maltodextrin and acacia gum.
Encapsulation was completed in three stages, i.e. emulsi-
fication, spray dr ying and fluid bed agglomeration.
Agglomeration did not change oil encapsulation proper-
ties of the spray - dried powder but considerably
improved its wettability. Chegini and Ghobadian [94]
investigated the effects of the feed ratio, atomizer speed,
 Encapsulation of Hydrophilic and Hydrophobic Flavors by Spray Drying
and inlet air temperature on properties of spray-dried
orange juice powders basing on a full factorial experi-
mental design. Tan et al. [95] reported the effect of
marine oil loading on the encapsulation efficiency when
modified starch was used as wall materials. The higher
oil loading increased the droplet size of emulsions
formed resulted the higher surface content and lower
production yield. The encapsulation of vegetable oil as
the model in MD and GA was studied. The direct
agglomeration process was used to increase the size of
the particle to improve the flowability and wettability
[96]. A cool chamber wall spray dr yer was used to
increase the production of yield of lime juice powder
because of the decreasing of particles stickiness on the
wall [97]. The different emulsifying ingredients (Tween
20, modified starch or whey protein concentrate) were
used to produce sub- micron emulsions by high pressure
homogenizer. The biopolymers were not efficient ingre-
dients to produce ver y small emulsion droplets com-
pared with small molecule surfactants because of their
slow adsorption kinetics [98]. However, it was not possi-
ble to produce a fairly stable microfluidized emulsion
with surfactants for encapsulation purposes. The influ-
ence of par ticle morphology of spray dried powders
obtained by using different carriers on the efficiency of
microencapsulation of rosemary aroma is investigated.
The efficiency of encapsulating aroma inside the cap-
sules depended on the size of obtained particles and the
apparent density of powders. An increase in the average
diameter and decrease in the apparent density of pow-
ders decreased the quantity of microcapsulated aroma
[99]. Serfert et al. [100] investigate the impact of the
emulsifying carrier matrix constituent, n- octenylsucci-
nate derivatised (OSA)- starch, and process conditions
on physical characteristics and oxidative stability of
microencapsulated fish oil. The highest oxidative stabil-
ity was observed for fish oil microencapsulated in OSA-
starch with the lowest average molecular weight. In
terms of spray-drying under inert conditions and in the
presence of air, lipid oxidation of microencapsulated fish
oil was rather attributed to oxygen availability in the feed
emulsion than in the drying gas. The present study indi-
cates that also discrete air inclusion may accelerate lipid
oxidation of microencapsulated oils. To produce low-salt
fish sauce powder, the effect of electrodialysis pretreat-
ment on physicochemical properties and morphology of
powder was investigated. Without the additional carrier
materials, the lower hygroscopicity of the low salt fish
sauce powder with the low product recover y was
43
reported. The salt concentration of not lower than 14 wt%
was recommended [101]. Paramita et al. [102] developed
the high content of encapsulated of d- liomonene powder.
The medium- chain triglyceride was mixed to the d-Limo-
nene to make the emulsion in the OSA-modified starch
carrier solution before spray drying. Goula et al. [77,
103] reported an effective way of increasing lycopene
encapsulation and reducing residue formation of spray
dried orange juice concentrate by using dehumidified air
as the drying medium.
5. Morphology of spray - dried powder
Spray drying is the process by which a solution or
slurry is transformed into a dry powder by spraying the
fluid feed material into a hot drying medium. The mor-
phology of the spray- dried particle has been studied
extensively by Walton and Mumford [104] and Walton
[105] using a suspended droplet drying techniques. They
classified the morphology of the droplet into 3 catego-
ries; agglomerate, skin-forming, and crystalline. Figure
1 shows four powder photos of scanning electron micro-
scope, milk proteins (a), spray- dried fat with maltodex-
trin (b) , mannitol (c) and α-cyclodextrin (d). Several
spray-dried powders have aggregates as shown in Fig.
1(a), which were formed at the outlet gas temperature
above glass transition temperature. The cr ystalline in
spray -dried powder with mannitol and cyclodextrin were
observed. Higher content fat in wall material could be
observed smooth surface in spray-dried powder.
Morphologies of the powder particle by spray drying
Fig. 1 Morphologies of spray-dried powders.
(a) Spray-dried milk powder (x140), (b) Spray-dried powder
with maltodextrin and fat (x800), (d) spray- dried mannitol
(x1500), (d) Spray-dried α-cyclodextrin
44 Apinan SOOTTITANTAWAT, Riitta PARTANEN, Tze Loon NEOH, Hidefumi YOSHII
affects upon the porosity, the surface integrity and flow
properties of spray dried powder. Figure 2 shows dex-
trose equivalent (DE) of maltodextrin affects the surface
integrity. Surface crinkle structure might depend on the
drying rate. The powders produced with higher malto-
dextrin concentrations were less hygroscopic and had a
lower moisture content after drying.
Hecht and King [106] investigated the morphology
changes of the particle by using single droplet. Rogers et
al. [107] investigated particle shrinkage and morphology
of milk powder made with a monodisperse spray dryer.
They suggest the surface crust (initially spherical) is vis-
coelastic and deforms in response to dr ying stresses.
They also investigated the modelling of the formation of
insoluble material for a monodisperse spray dr yer.
Alamilla-Beltrán et al. [108] investigated the morphologi-
cal changes of particles during spray drying and con-
cluded the particle changes are related to moisture con-
tent of the material and operating drying temperatures.
Abadio et al. [109] investigated physical properties of
powdered pineapple (ananas comosus) juice in the effect
of maltodextrin concentration and atomization speed.
They showed the powder density could be correlated
with atomizing speed and maltodextrin concentration.
Bhandari et al. [110] investigated spray drying of concen-
trated fruit juices. They obtained the optimal ratio of
maltodextrin to the juice. In the morphology of the spray
dried powder, the coagulation of the particles is impor-
tant to evaluate the powder properties. The stickiness
problem of sugar products such as fruit juices has been
related to their low glass transition temperature (Tg ) and
water-induced plasticization..
Fig. 2 Surface morphologies of spray-dried particle with various DE of maltodextrin.
6. Release of flavor from spray- dried powder
Spray drying is the most commonly used technique for
the production of dr y flavorings. Zuidan and Heinlich
[111] summarized encapsulation of aroma. Morphologies
of the encapsulant depend on the flavor release behavior
as well as wall material. The release mechanism compari-
son may be carried out using model independent or
model dependent methods [112]. In order to investigate
the release mechanism, several different models have
been employed for outlining the release mechanism from
matrices. The analysis of flavor release from spray-dried
powder is complex and difficult, since the phenomena of
flavor release take place with intrinsically overlapping
mechanisms, mainly by dissolution and subsequent diffu-
sion of flavors and water as well as flavor oxidations. The
release rates, that are achievable from single microcap-
sule, are generally 0, 0.5, or 1st order. Zero -order release
relation can be used to describe the flavor release of sev-
eral types of modified release flavor dried powders, as in
the case of some transdermal systems, as well as matrix
particles with low soluble flavor, coated forms, osmotic
systems, etc., When the core is a pure material and
release through the wall of the reservoir microcapsule as
a pure material, the release rates might indicate the
zero- order. Half order release kinetics occurs with
matrix particles. Diffusion is controlled by the solubility
of a flavor in the matrix and the diffusivity of the flavor
through the matrix [113]. A simple equation of Avrami
equation has been proposed for the correlation of the
release time- course of a spray- dried ethyl- n- butylate
powder during storage [5]
 Encapsulation of Hydrophilic and Hydrophobic Flavors by Spray Drying 45

tion kinetics. Table 1 shows the proposed equation for

(1)
Where R is the retention of flavor in the powder, t is
the storage time, kR is the release rate constant, n is a
parameter representing the release mechanism. This
equation is also called the Weibull distribution function,
which has been successfully applied to describe the
shelf-life failure. A general empirical equation described
by Weibull [114] could be adapted to the dissolution/
release process. Figure 3 shows the release time-course
of ethyl butyrate from spray- dried powder with the mix-
ture of gum arabic and maltodextrin, and soluble soy-
bean polysaccharides and maltodextrin. The mechanism
values of n depend also on the wall material. The release
time-course of ethyl butyrate fitted well to the Avrami’s
equation. This Avrami equation is essentially analogaous
to the equation of Kohlraush - Willian - Watt (KWW)
[115]. Taking a logarithm of both sides of equation 1, we
can get the parameter n as slope by plotting ln[-ln R] vs.
ln t and release rate constant k from the interception at ln
t = 0. For n of value, n = 1 represents the first- order
reaction, n = 0.54 represents the diffusion- limiting reac-
various n values. Flavor release rate are strongly affected
by the environmental humidity and temperature since
the humidity as water vapor pressure influence the
degree of plasticization of wall material and emulsion sta-
bility in spray -dried powder. Soottitantawat et al. [116]
showed the release of d-limonene from emulsified d-lim-
onene in spray-dried powder was closely related to water
activity of the powder.
7. Collapse of spray - dried powder
Most amorphous carbohydrate systems are not in
equilibrium and can be metastable with slow kinetics for
changes, or unstable with physical changes occurring on
practical time scale. Dried fruits and vegetable juices are
convenience foods that have long storage life at ambient
temperature. However, environmental humidity affected
the physical structure of the powder. Stickiness is a
major reason that limits the spray dr ying of various
sugar- rich food products. The main constituents of fruit
juices are low molecular weight sugars such as sucrose,

Fig. 3 Ef fect of gelatin on the release time - course of ethyl butyrate. (○●, MD
conc.=20% (w/w); △▲, 30% (w/w). GA or SSPS concentration=10% (w/w). Closed
symbols refer to the addition of gelatin. Solid lines are the correlation cur ves
obtained by Eq. (1)). [5]

Table 1 Comparison of mechanism value of n with the release model equation in Avrami equation.

Value of n Release mechanism Model equation

0.54 Diffusion controlled (sphere)

0.57 Diffusion controlled (cylinder)

0.62 Diffusion controlled (tablet)
1.00 First-order mechanism
1.07 Moving interface mechanism (sphere)
1.11 Moving interface mechanism (disk)
1.24 Zero-order mechanism
46 Apinan SOOTTITANTAWAT, Riitta PARTANEN, Tze Loon NEOH, Hidefumi YOSHII

Table 2 The theories linked with the physical state of carbohydrate matrix affecting oxidation of matrix-embedded flavors and lipids.

Observation Theory Uncertainties/Limitations

1. Aw affects lipid oxidation rate Monolayer theory – best stability at Assumption of equilibrium, sorption the only mate-
monolayer moisture rial property considered

2. Oxygen is needed for hydroper- Oxygen transfer is rate-limiting for Shown for glassy system at ambient/ high tem-
oxide formation oxidation perature, but may depend on oil susceptibility

3. Diffusion of small molecules is Glass transition theory Diffusion not coupled with viscosity in the transi-
facilitated due to plasticization tion region

4. Dry starch is a good oxygen Role of water as solvent, solubility of Solubility data only for solutions of sugar alcohols,
barrier O2 in dry carbohydrate limits perme- extrapolated to low-water systems
ation

5. Average volume of the voids Glassy state swelling affects diffusion Also molecular packing affects as demonstrated
between polymers increases of small permeants in carbohydrate for glucose syrup in comparison to maltose as
gradually with increasing water matrices length of jump distances
content

6. Oxidative stability of oil in carbo- More intense structural re-organiza- Antioxidativity of proteins at high humidity may
hydrate and protein matrices is tion of the protein matrix in the pres- affect oxidative stability
oppositely affected by water ence of water due to hydrophobicity

glucose, fructose, and some organic acids. Jaya and Das
[117] investigated the glass transition and sticky point
temperatures and stability/mobility diagram of fruit pow-
ders. They showed glass transition temperature of the
fruit powders were interpreted in terms of the Gordon-
Taylor model (Eq(2)) for verification and glass transition
and sticky point temperatures were compared by plotting
them in a graph against moisture content.
(2)
where Tgm, Tgs, and Tgw are the glass transition tempera-
ture (℃) of the mixture, solids, and water respectively, Xs
and Xw are the mass fraction of solids and water (wet
basis), and k is the Gordon–Taylor parameter. In the
equation, the value of ‘k’ depends on moisture content
and the empirical equations derived for ‘k’ of three differ-
ent fruits were different from each other. The empirical
constant ‘k’ of power equations for different fruit pow-
ders are [117]:
(3)
where a and b are parameters for powder (a=0.548,
0.642, and 1.294 for mango, pineapple, and tomato pow-
der, b=0.628, 0.5571, and 0.4474 for mango, pineapple,
and tomato powder, respectively). Foster et al. [118]
investigated glass transition related cohesion of amor-
phous sugar powders and indicated the rate of cohesive-
ness development is proportional to the (T–Tg ) value,
that is, the greater the temperature above the Tg , the
quicker the powders will develop liquid bridges which
may result in caking. Mosquera et al. [119] investigated
the water content–water activity–glass transition temper-
ature relationships of commercial spray - dried borojó
powder, as related to changes in color and mechanical
properties. They showed the changes in the mechanical
properties of borojó powder related to collapse develop-
ment started when the sample moved to the rubber y
state and began to be significant at about 10℃ above Tg .
Collapse has been found to occur in amorphous system
above Tg , where its rate affected by temperature differ-
ence (T-Tg ) [120]. Soottitantawat et al. [116] indicated
the flavor release rates and oxidation rate of d-limonene
from spray-dried powder could be correlated with the
temperature difference (T- Tg ). In their results, flavor
release rate constant increased with an increase in T- Tg
and reached a maximum at roughly (T- Tg ) equals to
zero, which is analogous to the oxidation rate constant.
Moisture sorption properties of dry food products and
ingredients are critical in their overall processing, stor-
age stability, and application performance. Dronen and
Reineccius [121] investigated rapid analysis of volatile
release from powders using dynamic vapor sorption
atmospheric pressure chemical ionization mass spec-
trometry and indicated the system demonstrated differ-
ences in volatile release as a function of volatile com-
pound, relative humidity, and food polymer. Mortenson
and Reineccius [122] investigated dynamic real- time
analysis to determine how carrier material affects men-
thol release characteristics from various spray- dried
powders. They showed DVS - P&T–GC methodology
proved to be a useful screening tool to select samples for
the more precise DVS–PTR–MS analysis.
 Encapsulation of Hydrophilic and Hydrophobic Flavors by Spray Drying
Recent advances in understanding the nano - scale
structures, and thus packing, of carbohydrate matrices
[123, 124] should lead to better control over diffusion of
small permeants in glassy state. Also the role of water
has been re- assessed not only affecting as plasticizer,
but also as a solvent e.g. to oxygen [125, 126]. The theo-
ries linked with the physical state of carbohydrate matrix
affecting oxidation of matrix- embedded lipids and the
permeation of small components are briefly summarized
in Table 2.
8. Conclusion
The microencapsulation of tropical flavors by spray
drying is reviewed with the recently published papers.
Spray drying is a useful method to encapsulate extracted
flavors or liquids of the tropical fruits in powder form.
The selection of wall materials and emulsifier, as well as
the process conditions are very important to form the
suitable powder in food industr y. The stability and
release of flavor are affected with the glass transition
temperature of the wall materials, and presumably by the
nano - scale structure of the formed powder matrix.
Storage conditions have a major role in both physical and
chemical stability of the powders. Basic mass- transfer
phenomena of flavor release and stability during spray
drying and storage at different humidity conditions are
currently under investigation using the latest analytical
instruments.
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 「日本食品工学会誌」, Vol. 16, No. 1, p. 53, March. 2015

◇◇◇ 和文要約 ◇◇◇

噴霧乾燥による親水性，または疎水性フレーバーの包括粉末化
1 2 3 3
スーチンタワット アピナン ，リッタ パータネン ，ネオ ツー ルーン ，吉井英文
1
チュラロンコン大学工学部化学工学科， 2 フィンランド国立技術研究所，
3
香川大学農学部生物応用科学科

食品の香りのコントロールは，食品素材の付加価値 係わる事項として，貯蔵中に賦形剤の相変化，粉末か
を大きく高める技術として注目され，フレーバーの徐 らのフレーバーの移動，酸化，賦形剤中の酸素移動，
放制御特性などの新しい機能を付与した機能性粉末を 水分の移動といった諸現象の経時変化がある．フレー
作製する研究が行われている．食品工業において，フ バー粉末の徐放性に関する研究のほとんどは，恒温恒
レーバーの包括粉末化は重要なプロセスである．本総 湿環境下（静的方法）における粉末からのフレーバー
説において，噴霧乾燥によるフレーバーの包括粉末化 徐放特性から評価されている．乳化フレーバー粉末や
と噴霧乾燥粉末からのフレーバー徐放挙動についてま フレーバー包接シクロデキストリンからのフレーバー
とめた．疎水的フレーバーは，一般的にオイルにフレー 徐放挙動は，次式のアブラミの式で良好に相関できる．
バーを溶解させたもの，またはフレーバーオイルその n
R=exp (－(kt) ) （1）
ものを，界面活性剤，賦形剤を溶解した溶液に添加後
乳化した溶液を噴霧乾燥機で粉末化する．親水性フレー ここで，R は粉末中のフレーバー残留率（ - ），k は徐
-1
バーは，噴霧乾燥粉末内に均一に分散するため包括率 放速度定数（s ），t は時間（s），n は徐放機構定数（ - ）
は賦形剤に大きく依存する．これらのそれぞれの粉末 である，このアブラミ式（Weibull 式）は，結晶成長を
作製における賦形剤，フレーバーのタイプについて， 相関する速度式で多くの事象を解析するのに用いられ
既往の研究をまとめた．噴霧乾燥粉末は，粉末が凝集 ている．異なる n の値を用いて，多くのフレーバー徐
したものや，凸凹のしわが多い粉末，粉末内部が中空 放機構に対応しフレーバー徐放挙動を相関できること
や結晶が析出したものといった様々な形態の粉末があ から，この式は非常に有用な相関式である．フレーバー
る，この粉末の形態は，粉末内機能性物質の安定性や 粉末が球で賦形剤中の拡散速度によりフレーバー徐放
粉末の流動性に大きく影響する．食品粉末のフレーバー 速度が決まる場合は，徐放機構定数 n は 0.54 付近の値
の保持，徐放特性は，粉末の品質の点から非常に重要 をとる．アブラミ式を用いて噴霧乾燥粉末からのフレー
である．フレーバーの徐放に関して多くの研究が行わ バー徐放速度定数の湿度依存性（ガラス転移温度依存
れており，粉末からのフレーバー徐放特性が貯蔵温度 性）をみた結果，ガラス転移温度 Tg と徐放環境温度 T
における相対湿度と密接に関係していることが報告さ の差（T- T g ）に依存していた．
れている．乳化フレーバー噴霧乾燥粉末の緩和現象の

（受付 2015 年 1 月 17 日，受理 2015 年 2 月 23 日）

〒761- 0795　香川県木田郡三木町池戸2393
Fax: 087-891-3021, E-mail: foodeng.yoshii@ag.kagawa-u.ac.jp