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

誌名誌名 日本食品工学会誌 = Japan journal of food engineering

ISSNISSN 13457942

著者著者

Soottitantawat, A.Partanen, R.Neoh, T.L.吉井, 英文

巻/号巻/号 16巻1号

掲載ページ掲載ページ p. 37-53

発行年月発行年月 2015年3月

農林水産省 農林水産技術会議事務局筑波産学連携支援センターTsukuba Business-Academia Cooperation Support Center, Agriculture, Forestry and Fisheries Research CouncilSecretariat

J apan J ournal of Food Enginee出 g，Vol. 16， No. 1， pp. 37 -52， March. 2015

。く〉く>Reviewく〉く〉く〉

Encapsulation of Hydrophi1ic and Hydrophobic Flavors by Spray Drying

Apinan SOOTIITANTAW.Nザ， Rii仕aPARTANEN2， Tze Loon NEOH3， Hidefumi YOSHII3，t

1 Department 01 Chemical Engineering， Chulalongkorn Universiか"Pathumwan， Bangkok 10330， Thailand 2 Bioprocessin，ιV1T Technical Research Centre 01 Finland， P.O. Box 1000， 02044 VTT， Espoo， Finland

3Department 01 ApPlied Biological Science， Kagawa University， 2393 lkenobe Miki.一chi，Kita， Kagawa 761-0795， Japan

τ'he encapsulation of flavors is the important process in food indus仕y.The encapsulation of flavors

with spray drying and the flavor release企omspray-dried powder were reviewed.τ'he hydrophobic flavor was in the form of emulsion before spray drying. Therefore， the researches were mainly related to the forming of emulsion which wall material containing emulsi:fier properties are required. On the other hands， the hydrophilic flavor was mainly related to the antioxidant and coloring flavor powder.τ'he hygroscopicity of powder and their stickyness during the spray dryer were important points to improve which the remaining of hydrophilic flavors were less concerned.τ'he 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.τ'he 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-九).In this review， recent researches are summarized in the flavor encapsulation in spray drying， especially for仕opicalflavor

encapsulation. Keywords: flavor， encapsulation， spray drying， powder， con仕olledrelease

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仕opicalfruits 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 industry， various core

compounds， such as volatile compounds， essential oils，

and oleoresins， are encapsulated with some spec坦ccon-

cerns， such as safety usage of solvent and wall material.

The most common and economical way to carry 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血evola泊leflavor constituents of tropical fruits and

flavor behaviors at storage. Pino and Marbot [6] investi-

gated血evolatile constituent of acerola fruits. Tietel et

(Received 17 Jan. 2015: accep匝d23 Feb. 2015)

t Fax: 087-891-3021， E-四国1:ioodeng.yosbii@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.τ'hey 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.τ'hey 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.τ'hey 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 en仕apment，coacervation，

inclusion complexation， cen仕出galextrusion and rota-

tional suspension separation. Powder formation of these

flavors is one interesting process of food industry.

Zuidam and Heinrich [12] edited the book of

“Encapsulation Technologies for active food ingredients

and food processing". The aroma encapsulation were

38 Apinan SOOTII'L必，TAWAT，Rii仕耳 PARTANEN，τ'zeLoon 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.τ'he 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.τ'he 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 pape巳thehydropobic 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

wi出 emulsifierproperties 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 wi仕1various conditions， the water， 0勾rgenand flavor

itself can diffuse through the shell wall.τ'he 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 ofwall 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.τ'he 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.

τ'here 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.日7]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-drying with proteins

(sodium caseinate and gelatin)， gum arabic and malto-

dextrin. A better microcapsule yield， efficiency， 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.τ'he pectin was able to

preserve the β-sheet secondary structure of pea protein

Encapsulation of HydrophiIic and Hydrophobic Flavors by Spray Drying 39

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 partic1es 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 0刃gend江fu-

slOn.

K1inkesorn [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.

1ρksuwan [25] showed the modified tapioca starch as

potential wall material for encapsulation of s-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 inc1usion complex and spray drying

were also reported.τne cyc10dextrins and their deriva-

tives was used to form the inc1usion complex of hydro-

phobic f1avor and then following by spray drying to form

the dry products. Liu et al. [28] showed the encapsulated

of menthols inβ，αand y-cyc1odextrin following with

the single droplet drying process to simulate the loss of

f1avor during spray drying process. Kawakami et al. [29]

showed the encapsulation of rice f1avor in α-cyc1odextrin

and highly branched cyc1ic dextrin by spray drying.

2.2 Type of hydrophobic flavors

Numerous of works have reported the encapsulation of

f1avors as well as the仕opicalf1avors in both of model f1a-

vors and natural extracted f1avors. Bylaite et al. [30]

encapsulated the caraway essential oil in mixtures of

whey protein concentrate and malodextrins matrix by

spray drying. Partanen et al. [31] report疋dthe microen-

capsulation of caraway extract in β-cyc1odextrin and

modified starches.τne inc1usion complex seemed to pro-

tect volatile substances more efficient1y 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 f1avor in conventional wall

materials of gum arabic and maltodextrin.τne rose oil

which composed of 2-phenylethanol (50.22%)， nerol

(22.34%) and citronell01 (19.40%) was also encapsulated

gum arabic and maltodextrin wall materials. The yield of

encapsulated rose oil varied with wall materials (6←70%)

[34]. The model f1avor 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仕lemicroencapsula-

tion of cardamom oleoresin using binary and ternary

blends of gum arabic， maltodextrin， and OSA-modified

starch as wall materials. Bixin was encapsulated by

spray-drying 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 f1avorings 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幽

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.

τne 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

]imenez 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 sunf10wer oil. The lipid oxidation of encapsulated

sunf10wer oil was remarkable decreased with the addi-

tion of the mixed natural antioxidants ex仕actto the sys-

tem. Natural Canthaxantin was encapsulated in soybean

soluble polysaccharides. The results showed the oxida-

40 Apinan SOOTIITANTAWAT， Rii伽 PARTANEN.τzeLoon NEOH. Hidefumi YOSHII

tion was more suppressed for the microcapsules pre- quality of the product as the f1avor concentration in dry

pared from the emulsion having smaller droplets [46]. basis was decreased. Numerous works was done to

Toure et al. [47] reported the microencapsulation of gin- improve these problems rather than the retention of f1a-

ger oi1 in maltodextrin(DE=18)/whey protein isolate vor in the powder products.

with the application of the higher pressure homogeniza-

tion. The best conditions for higher retention at 93 per-

cent were found. The inf1uence of some process condi-

tions on the microencapsulation of f1axseed oi1 (vegeta-

ble sources ofωー3)in gum arabic by spray drying was

reported [48]. Rodea-Gonzalez [49] reported the encap-

sulation of chia essential oi1 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 inf1uence of the composition of出ewall

material on the encapsulation and stability of microen-

capsulated red-f1eshed pitaya seed oi1 by spray drying.

The study on oi1 retention revealed that sodium casein-

ate > whey protein > gum arabic as effective wall materi-

als for pitaya seed oi1 encapsulation. Rubi1ar et αl. [52]

prepared the formulation of soup powder enriched with

ω-3 fatty acids of linseed oi1 in gum arabic/maltodex-

trin mixture. Recently， the encapsulation of multif1avors

bergamot oi1 in gum arabic and modified starch were

studied. The transformation among each f1avor to give

the retention higher than 100 percent was discussed

[53].

3. The encapsulated hydrophilic flavors

To encapsulate the hydrophilic f1avors， the aqueous

solution of宜avorand carrier solid was prepared.τ'hen，

the aqueous mixture was spray dried.τ'he f1avors are dis-

persed and encapsulated in the dried carrier solid in the

form of matrix type.

τ'he researches work is now aim to improve the physi-

cal properties of the powder. The main problem of the

natural hydrophilic f1avors is the content of the soluble

solid as low molecular of saccharide in the extract aque-

ous f1avor 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.τ'he maltodextrin was norma11y used as the dry-

ing aid agents to仕lesystem.τ'he higher maltodextrin

content decreased the stic均nessand hygroscopicity of

the product. The gum arabic was a1so used because of its

excellent film forming properties even the emulsifier

properties are not required in this system. However， the

3.1 Wall materials

Some new wall materials and wall materials systems

were applied to solve the stickyness and hygroscopic

properties problems wi仕1high f1avor content. Oliveira et

al. [54] showed the potential using of cashew仕eegum to

partially replace the conventional maltodextrin as drying

aid agent in spray drying of cashew apple juice.百le

retention of ascorbic acid was increased with the

decreasing of powder hygroscopicity especially when the

ratio of cashew tree gum to ma1todex仕inis higher than

50%.

Recent1y， the protein compounds were added to the

feed solution in the sma11 amount to increase the hygro-

scopic properties instead of adding high content of

maltodex仕in.]ayasundera et al. [55] reported the pow-

der recovery 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 mi1k powder.τ'he results showed that the sur-

face composition is very much different企omthe bulk

composition of powders. A maltodextrin/ apple pectin

based matrix was used to encapsulate the plant extracts.

τ'he bioactive polyphenols and moisture content of the

partic1es or the antioxidant activity appeared signi宣cant1y

modified [57].

3.2 Type of hydrophilic flavors

There are numerous of works reported the encapsu-

lated hydrophilic f1avors such as juice powder and colo-

rant powder. In general， for the hydrophobic and hydro-

philic f1avors which have the c10se molecular weight

and normal boiling point， the retention of hydrophilic

f1avors during the spray drying are lower than the

retention of hydrophobic f1avors as the mechanism

explained above. However， the low amount of remaining

f1avor 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 f1avor 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 41

dried using a range of maltodextrins (DEI0-25) and

starches (native/modified) as carrier and coating

agents. Adding maltodextrins and starches significant1y

reduced the hygroscopicity of the betacyanin extracts

and enhanced storage stability [58]. The extracted 2-ace-

tyl-l-pyrroline odor of rice f1avor was encapsulated in

gum arabic and maltodex仕in[59]. Shiga et al. [60] devel-

oped the encapsulated extracted shiitake f1avors powder

by spray drying.τne mixture between cyc10dextrin 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

ma1todextrin 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.τne malto-

dextrin， gum arabic and waxy siarch were used as wall

materials with the additional of cellulose. They reported

that the cellulose as a substance白紙 inducescrystalliza-

tion of sugar is not suitable. Immature acerola juice pow-

der was prepared by spray drying with maltodextrin and

gum arabic.百leratio of juice solid to carrier was 1:1.

The glass transition temperature and the stickiness of

the powder was discussed [63].τne raisin juice powder

was produced with maltodextrins as drying aid agents. It

was shown that the lower the DE of the maltodex仕in

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].

τne watermelon powder was produced with maltodex-

trin. Addition of maltodextrin reduced the stickiness of

the products and a1tered the physicochemical properties

of the spray-dried powders.τne loss of lycopene and

carotene occurred at higher inlet temperatures [65].

Microencapsulation of anthocyanin pigments of black

carrot by spray drying wi仕1maltodextrin (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 inf1uence of spray drying condi-

tions on the physicochemica1 properties of acai powder

with maltodextrin DE 10 as carrier. The curcumin pig-

ments was a1so produced by spray drying using porous

starch and gelatin [69]. A powder food colorant was

obtained by spray drying 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 ma1todextrin (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 beiter 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 drying. The polyphenols encapsulating

efficiency was significant1y beiter 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 materia1s. The retention of maker volatile

compounds (two esters and two sulfides) was investi-

gated during spray drying and storage. The retention of

f1avors was in the rage of 20-70%. The study demon-

S仕ated仕latvolati1es with larger molecular weight tended

to retain beiter during spray drying. However，仕lestabil-

ity during storage was stilllow. 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 further reduced the hygroscopicity as well as

increasing the stabi1ity of the pigments. Goula and

Adamopoulos [77] investigated the development a new

technique for spray drying 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 ma1todextrin addition and use of dehu四

midified air as drying medium seems to be an effective

way of producing a仕ee-f1owingorange powder.τne pro-

42 Apinan SOOTIITANTAWAT， Rii抗aPARTANEN，τzeLoon NEOH， Hidefumi YOSHII

duction of bayberry polyphenols powder with MD

(DE10) by spray drying with the retention of phenolic

content and total anthocayanins after spray drying at

about 95% was reported [78]. The water extract of the

mountain tea was spray-dried by using s-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

白eeffect 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% recover手

Yousefi et al. [81] reported the pomegranate juice was

diluted to 120 Brix and carriers (maltodextrin， gum ara-

bic， waxy starch) were added wi白 varyingconcentra-

tions of cellulose before being reduced to powder by

spray drying. 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 properties 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 s-carotene

contents of cantaloupe juice powders. Caparino et al.

[85] showed the effect of drying methods (re仕actance

window drying， freeze drying， drum drying and spray

drying) on the physical properties and microstructures

of mango powder. The maltodextrin was used as carrier

for the spray drying 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 drying. 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

τ'he properties of wall materials， flavors， emulsion as

well as白espray 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.τ'he 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 affected 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 signi宣cantdeter-

minant of shelf life. Cho and Park [90] showed the dou-

ble encapsulation of limonene powder by coating the

powder with wax oil.τ'he 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-

tion in the case of partly-soluble flavor.

Microencapsulation by spray drying 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 drying 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 Orying 43

and inlet air temperature on properties of spray-dried reported. The salt concentration of not lower than 14 wt%

orange juice powders basing on a full factorial experi- was recommended [101]. Paramita et al.日02]developed

mental design. Tan et al. [95] reported the effect of the high content of encapsulated of d-liomonene powder.

marine oil loading on the encapsulation efficiency when The medium-chain triglyceride was mixed to the d-Limo-

modified starch was used as wall materials. The higher nene to make the emulsion in the OSA-modified starch

oil loading increased the droplet size of emulsions carrier solution before spray drying. Goula et al. [77，

formed resulted the higher surface content and lower 103] reported an effective way of increasing lycopene

production yield. The encapsulation of vegetable oil as encapsulation and reducing residue formation of spray

the model in MD and GA was studied. The direct dried orange juice concentrate by using dehumidified air

agglomeration process was used to increase the size of as the drying medium

the particle to improve the f10wability and wettability

[96]. A cool chamber wall spray dryer was used to 5. Morphology of spray-dried powder

increase the production of yield of lime juice powder

because of the decreasing of particles stickiness on the

wall [97]. The di仔'erentemulsifying 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 very 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 microf1uidized emulsion

with surfactants for encapsulation purposes. The inf1u-

ence of particle 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

emulsiちringcarrier 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 recovery was

Spray drying is the process by which a solution or

slurry is transformed into a dry powder by spraying the

f1uid 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 crystalline 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 a-cyclodextrin

44 Apinan SOOTTITANTAWAT，脳出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.τ'he 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.日07]investigated particle shrinkage and morphology

of milk powder made with a monodisperse spray dryer.

τ'hey suggest the surface crust (initially spherical) is vis-

coelastic and deforms in response to drying stresses.

τ'hey also investigated the modelling of the formation of

insoluble material for a monodisperse spray dryer

Alami1la-Beltran 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仕uitjuices. They obtained the optimal ratio of

maltodextrin to the juice. 1n the morphology of the spray

dried powder， the coagulation of the particles is impor-

tant to evaluate the powder properties.τ'he stickiness

problem of sugar products such as fruit juices has been

related to their low glass transition temperature (九)and

water-induced plasticization..

6. Release of flavor from spray-dried powder

Spray drying is the most commonly used technique for

the production of dry flavorings. Zuidan and Heinlich

[111] summarized encapsulation of aroma.Morphologies

of the encapsulant depend on the flavor release behavior

as well as wall material.τ'he release mechanism compari-

son may be carried out using model independent or

model dependent methods [112]. 1n order to investigate

the release mechanism， severaldifferent models have

been employed for outlining the release mechanism from

matrices. The analysis of flavor release from spray-dried

powderiscomplexanddifficult， since the phenomenaof

flavor release take place with intrinsically overlapping

mechanisms， mainly by dissolution and subsequent diffu-

sion of flavors and water aswell 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 d江釦sivityof 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]

Fig. 2 Surface morphologies of spray-dried particle with various DE of maltodextrin.

Encapsulation of Hydrophilic and Hydrophobic Flavors by Spray Drying 45

Rニ仰[-(kRtl] (1)

Where R is the retention of f1avor 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日141could 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.τ'he mechanism

values of n depend also on the wall material.τ'he release

time-course of ethyl butyrate fitted well to the Avrami' s

equation. This Avrami equation is essentially analogaous

to the equation of Kohlraush-Wil1ian-Watt (KWW)

[1151. Taking a logarithm of both sides of equation 1， we

can get the parameter n as slope by plotting ln[-ln R1 vs.

ln t and release rate constant k from the interception at ln

t = O. For n of value， n = 1 represents the first-order

reaction， n = 0.54 represents the diffusion-limiting reac-

1.0 0

帽

忌0.82 a

z0.6 0

20.4 0

~ 0.2 由

0::

0 0 10 20 30 40

Time (h) 50 60

tion kinetics. Table 1 shows the proposed equation for

various n values. Flavor release rate are strongly affected

by the environmental humidity and temperature since

the humidity as water vapor pressure inf1uence the

degree of plasticization of wall material and emulsion sta-

bility in spray-dried powder. Soottitantawat et al. [1161

showed the release of d-limonene企omemulsified d・lim-

onene in spray-dried powder was c10sely 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企uitsand vegetable juices are

convenience foods白athave 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 drying of various

sugar-rich food products. The main constituents of fruit

juices are low molecular weight sugars such as sucrose，

1.0 0

‘' 団長 0.8コJJ

~ 0.6 -由句・

20.4 0

-・4~ 0.2 0 0::

5 10 15 20 Time (h)

Fig.3 Effect of gelatin on the release time-course of ethyl butyrate. (0・， MD

conc.=20% (w/w);ム企， 30% (w/w). GA or SSPS concentration=10% (w/w). Closed

symbols refer to the addition of gelatin. Solid lines are the correlation curves obtained by Eq. (1)). [5]

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

Valueofn

0.54

0.57

0.62

1.00

1.07

1.11

1.24

Release mechanism

Diffusion con仕olled(sphere)

Diffusion con仕olled(cy駈lder)

Diffusion con仕olled(句blet)

First-order mechanism

Moving interface mechanism (sphere)

Moving interface mechanism (disk)

Zero-order mechanism

Modelequation

[1_Rl13]2=kt

R ln R + 1-R = kt

(1-R)2 = kt

-lnR =kt

1-R1/3 =kt

1-R1/2 =kt

1-R=kt

46 A.pinan SOOTTITANTAWAT，問i出 PARTANEN，Tze Loon NEOH， Hidefumi YOSHII

Table 2 The theories linked with the physical state of carbohydrate ma廿ixaffe氾出goxidation of ma凶x-embeddedflavors and lipids.

Obs e r v a t i o n τ be⑪ry Uncertainties/Limitations

1. Aw affects lipid 0長idationrate Monolayモrtheory -best stability at Assumption of equilibrium， sorption仕leonly mate-monolayer moisture rial property ∞nsidered

2. Oxygen is needed for hydroper- Oxygen回 nsferis rate-limiting for Shown for glass子野批matambientノhightem-oxide formation oxidation p告'raturモ， but may depend on oil susceptibility

3. Diffusion of small molecules is Glass transition出eory Diffusion not coupled with viscosity in the仕組si-facilitated due ωplasticization tion region

4. Dry starch is a good oxygen Role of water as sol問 nt，solubili匂Tof Solubility da也 onlyfor solu世!onsof sugar al∞hols， barrier O2 in dry carbohydrate limits perm仔 のぽapola舵dωlow~明atersystems

a世.on

5. Average volume of the voids Glassy sta民 swellingaffects diffusion Also molecular packing affects as dβmons仕百tedbe回目npo恥nersincreases of small perme叩 tsin carbohydrate for glucose syrup in comparisゅnωmaltoseas graduallywi白 increasingwater m直凶C四 leng仕1of jump distances content

6. Oxidative stability of oil in carbo- More intense structural re-org皿 iza- An世oxidativityof proteins at high humidity may hydrate and protein matrices is 世onof出eproteinma仕ixin the pres- affect 0氾 dativestability oppositely affected by water ence of water due to hydrophobicity

glucose， fructose， and some organic acids. ]aya and Das the water content-water activity-glass transition temper-

[117] investigated the glass transition and sticky point ature relationships of commercial spray-dried borojo

temperatures and stability/mobility diagram of fruit pow- powder， as related to changes in color and mechanical

ders. They showed glass transition temperature of the properties. They showed the changes in the mechanical

fruit powders were interpreted in terms of the Gordon- properties of borojo powder related to collapse develop-

Taylor model (Eq (2)) for verification and glass transition ment started when the sample moved to the rubbery

and sticky point temperatures were compared by plotting state and began to be significant at about lOoC above 九.

4EL n

ρlV

4EL n

ゆ

w-

E

'

g一

町川一

w

ux一x

i

k

一k

・時+一十

剛弘一九

叫ん一

-m

一一mth

hR1』

p

a

rA gb

na n

--m

砕しh

4EL

(2)

where 1ふ，九"and九叩 arethe glass transition tempera-

ture CC) 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.τ'he empirical

constant 'k' of power equations for different企uitpow-

ders are [117]:

k=αX才 (3)

where a and b are parameters for powder (α=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.日18]

investigated glass transition related cohesion of amor-

phous sugar powders and indicated the rate of cohesive-

ness development is proportional to the (T一九)value，

that is， the greater the temperature above the 九， the

quicker the powders will develop liquid bridges which

may result in caking. Mosquera et al. [119] investigated

Collapse has been found to occur in amorphous system

above 九， where its rate affected by temperature differ-

ence (T-九)[120]. Soottitantawat et al. [116] indicated

the f1avor release rates and oxidation rate of d-limonene

from spray-dried powder could be correlated with the

temperature difference (T一九).In their results， f1avor

release rate constant increased with an increase in T一九

and reached a maximum at roughly (T一九)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-

廿ometryand indicated the system demonstrated differ-

ences in volati1e release as a function of volati1e 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 Hydr百phobicFlavors by Spray Drying 47

Recent advances in understanding the nano-scale

struc加res，and thus packing， of carbohydrate matrices

[123， 124] should lead to better control over diffusion of

small permeants in glassy state. A1so 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 brief1y summarized

in Table 2.

8. Conclusion

The microencapsulation of tropical f1avors by spray

drying is reviewed with the recent1y published papers.

Spray drying is a useful method to encapsulate extracted

f1avors or liquids of the tropical仕uitsin 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 industry. The stability and

release of f1avor 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 m司jorrole in both physical and

chemical stability of the powders. Basic mass-transfer

phenomena of f1avor 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J， Vol. 16， No. 1， p. 53， March. 2015

く>く><>和文要約く〉く>く〉

噴霧乾燥による親水性 または疎水性プレーパーの包括粉末化

スーチンタワットアビナン1，リツタノtータネン2，ネオツールーンペ吉井英文3

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，プレーパーの徐 らのプレーパーの移動，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.プレー

作製する研究が行われている.食品工業において，フ パー粉末の徐放性に関する研究のほとんどは，恒温恒

レーパ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パー

説において，噴霧乾燥によるプレーパーの包括粉末化

と噴霧乾燥粉末からのフレーパー徐放挙動についてま

とめた.疎水的プレーパーは，一般的にオイルにプレー

パーを溶解させたもの またはフレーパーオイルその

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.親水性プレー

パーは，噴霧乾燥粉末内に均一に分散するため包括率

は賦形剤に大きく依存する.これらのそれぞれの粉末

作製における賦形剤，フレーパーのタイプについて，

既往の研究をまとめた.噴霧乾燥粉末は，粉末が凝集

したものや，凸凹のしわが多い粉末，粉末内部が中空

や結晶が析出したものといった様々な形態の粉末があ

る，この粉末の形態は，粉末内機能性物質の安定性や

粉末の流動性に大きく影響する.食品粉末のプレーパー

の保持，徐放特性は，粉末の品質の点から非常に重要

である.プレーパーの徐放に関して多くの研究が行わ

れており，粉末からのプレーパー徐放特性が貯蔵温度

における相対湿度と密接に関係していることが報告さ

れている.乳化プレーパ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)

干761四 0795 香川県木田郡三木町池戸2393

F臨 :087-891-3021， E-mail: foodeng.yoshii@ag.kagawa-u.ac.jp

徐放特性から評価されている.乳化フレーパー粉末や

プレーパー包接シクロデキストリンからのフレーパー

徐放挙動は，次式のアブラミの式で良好に相関できる.

R=exp (一(kのn) (1)

乙乙で，Rは粉末中のプレーパー残留率(ー)， kは徐

放速度定数 (S-1)， tは時間 (S)，nは徐放機構定数(一)

である，このアブラミ式 (Weibull式)は，結晶成長を

相関する速度式で多くの事象を解析するのに用いられ

ている.異なる nの値を用いて，多くのフレーパー徐

放機構に対応しプレーパー徐放挙動を相関できること

から，この式は非常に有用な相関式である.プレーパー

粉末が球で賦形剤中の拡散速度によりプレーパー徐放

速度が決まる場合は，徐放機構定数 nは0.54付近の値

をとる.アブラミ式を用いて噴霧乾燥粉末からのプレー

パー徐放速度定数の湿度依存性(ガラス転移温度依存

性)をみた結果，ガラス転移温度九と徐放環境温度 T

の差 (T一九)に依存していた