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HYDROCOLLOIDS
Food Hydrocolloids 21 (2007) 928935 www.elsevier.com/locate/foodhyd

FOOD

Characteristics of microencapsulated b-carotene formed by spray drying with modied tapioca starch, native tapioca starch and maltodextrin
Jarunee Loksuwan
Department of Food Science and Technology, Faculty of Science and Technology, Thammasat University, Pathumthani 12120, Thailand Received 14 June 2006; accepted 25 October 2006

Abstract Acid-modied tapioca starch, native tapioca starch, and maltodextrin were tested for their ability to serve as wall materials for encapsulating b-carotene. The modied tapioca starch had wider particle size distribution, toward the smaller diameters, as compared to its native starch and maltodextrin. Moisture content and water activity of microcapsules were found to be dependent on type of wall materials. There were differences in total b-carotene and surface b-carotene contents among samples. The total b-carotene was highest for modied tapioca starch while it was lowest for maltodextrin. The surface b-carotene was lowest for modied tapioca starch while it was highest for native tapioca starch. The modied tapioca starch was more effective than its native starch in b-carotene retention. Results obtained suggest that the modied tapioca starch can be considered as potential wall material for encapsulation of b-carotene. r 2006 Elsevier Ltd. All rights reserved.
Keywords: Tapioca starch; Microencapsulation; b-carotene; Spray drying; Steam pressure

1. Introduction Microencapsulation is the technique by which the sensitive ingredients are packed within a coating or wall material. The wall material protects the sensitive ingredient (or core) against adverse reaction, prevents the loss of volatile ingredient, and controls release of the ingredient (Risch, 1993; Shahidi & Han, 1993). In addition, microencapsulation can convert liquids into free-owing powers, which are easy to handle. Microencapsulation has found many applications in food industry. Important applications are to coat colorants, avors, vitamins, and other sensitive food ingredients in order to increase their shelf life (Dziezak, 1988; Shahidi & Han, 1993). Various techniques are employed to microencapsulate food ingredients. Spray-drying is the most often used technique in the food industry (Gibbs, Kermasha, Alli, & Mulligan, 1999; Reineccius, 1988). In this process, the sensitive ingredient was mixed or homogenized in a solution containing wall material to
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form a stable emulsion. The emulsion is then fed into a spray dryer where it is converted to a dried particle. Numerous wall materials or encapsulating agents are available for food application. Gums arabic, hydrolyzed starches, and emulsifying starches are most commonly used as wall materials (Kenyon, 1995; Reineccius, 1988; Shahidi & Han, 1993). Some proteins such as whey proteins (Sheu & Rosenberge, 1995), sodium caseinate (Hogan, McNamee, Riordan, & Sullivan, 2001), and gelatin (Bruschi, Cardoso, Lucchesi, & Gremiao, 2003) are also used as wall materials. Typically, the effective wall materials for spray drying should have functional properties, including good emulsication, lm forming, high solubility, low viscosity at high concentrations and low cost properties (Reineccius, 1988; Trubiani & Lacourse, 1988). Gum arabic, a natural plant exudates polysaccharide of acacia, is a well-known effective wall material for many years and is still the good choice as wall material due to its stable emulsion and good volatile retention. Problems associated with the use of gum arabic in microencapsulation are high cost and limited supply. Emulsifying starches are starches derivatives with lipophilic group, i.e. 1-octenyl succinate. These wall materials have excellent

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emulsication properties (Trubiani & Lacourse, 1988). However, emulsifying starches have some limitations. They exhibit poor avor protection against oxidation and have off avor (Reineccius, 1988). Krishnan, Kshrisagar, and Singhal (2003) studied the efcacy of succinylated waxy maize starch, maltodextrin and gum arabic as wall materials for encapsulation of cardamom oleoresin by spray drying. They reported that succinylated waxy maize starch and maltodextrin had a lower protection to cardamom oleoresin during storage as compared to gum arabic. Maltodextrins are hydrolyzed starches produced by partially hydrolysis of starch with acid or enzymes. Hydrolyzed starches have the advantages of being low cost, bland in avor, and good avor protection against oxidation. Hydrolyzed starches are reported to improve shelf life of orange oil (Anandaraman & Reineccius, 1986) and carrot carotene (Wagner & Warthesen, 1995). These authors also reported that storage stability of core materials increased as hydrolyzed starches DE increased. Problems associate with the use of hydrolyzed starches in microencapsulation are lack of emulsication properties and poor avor retention (Reineccius, 1988). Many researches have used hydrolyzed starches in conjunction with other wall materials or emulsifying agents to improve their emulsifying characteristics. Mixtures of maltodextrins or corn syrup solids with whey proteins were reported as effective wall materials for microencapsulation of ethyl caprylate (Sheu & Rosenberge, 1995). Barbosa, Borsarelli, and Mercadante (2005) reported that maltodextrin with emulsier Tween 80 had the ability to encapsulate a higher amount of bixin than maltodextrin alone. A blend of gum arabic: maltodextrins: modied starch at a 4/6:1/6:1/6 was reported to provide a better protection of cardamom oleoresin than gum arabic (Krishnan, Bhosale, & Singhal, 2005). Preliminary study in our laboratory has shown that the efcacy of acid modied starch for encapsulation required the starch pre-swelling and gelatinization. This can be achieved by autoclaving of the modied starch slurry under steam pressure. This process results in formation of starch paste. The objective of this study was to evaluate the potential of acid modied tapioca starch after treated with heat under steam pressure as wall materials for encapsulation of b-carotene. The microstructure and physicochemical properties of encapsulated powder were investigated. These results were compared to those of its native starch and commercial maltodextrin. 2. Material and methods 2.1. Materials Native tapioca starch was purchased from local market (Thailand). The moisture content was about 8%. Moisture content was determined according to the method described in Section 2.9. Maltodextrin (Star-Dri 240-S, DE 24) was a gift from Burley Jucker Specialties Ltd.

(Bangkok, Thailand). Modied tapioca starch was prepared according to the method described in Section 2.2 in the laboratory of Department of Food Science and Technology of Thammasat University (Pathumthani, Thailand). Trans-b-carotene (powder) was obtained from Sigma Chemical Company (St. Louis, USA). All other chemicals used in this study were of analytical grade. 2.2. Sample preparation Acid modied tapioca starch was prepared from native tapioca starch according to the procedure of Loksuwan (2005) (Thailand Petty Patent No. 2146). Tapioca starch was added to 3 N H2SO4 in a ratio of 1:5 w/v. The mixture was stirred magnetically for 3 h at 60 1C. After hydrolysis the starch slurry was cooled and neutralized with saturated Na2CO3. The acid modied starch was ltered, washed with three volumes of distilled water, followed with 100 ml ethanol (95%). The starch was then dried at 70 1C for overnight. The dried starch was ground using a laboratory blender. Prior to microencapsulation, the modied starch was suspended in distilled water (29% w/w) and heated under steam pressure for 5 min to obtain gelatinized starch paste. Pure transb-carotene was added to the gelatinized starch paste in a ratio of 1:580 w/w, on dry starch basis. The mixture was then homogenized to obtain an aqueous emulsion (feed liquid) and immediately fed to the spray-dryer (Armeld FT 30, Armeld Technical Education Co., Hampsshier, England). The inlet and outlet air temperature were maintained at 17075 and 9575 1C, respectively. Experiments were performed in triplicate. The spray-dried powders were collected, kept in plastic bags wrapped with aluminum foil and stored in desiccators containing silica gel at room temperature. Solution of maltodextrin (29% w/w) and native tapioca starch (20% w/w, due to limit of viscosity) in distilled water were used for comparison study. Pure trans-b-carotene was added to maltodextrin and native tapioca starch solutions in the ratio of 1:580 and 1:400 w/w, on dry basis, respectively. The homogenization and spray drying were performed in the similar manner above. 2.3. Determination of dextrose equivalent (DE) and viscosity DE of modied starch produced by acid hydrolysis was determined using the method of Lane and Eynon (1923). Viscosity (cps) of samples was measured using Brookeld Digital Viscometer (Model DV-II+, Brookeld Engineering Laboratories, Inc., Stoughton, USA). Solutions of modied tapioca starch (29% w/w), native starch (20% w/w), and maltodextrin (29% w/w) in distilled water were prepared. The samples were then placed in a water bath with gently stirred. The viscosity was measured when the temperature of sample reached 80 1C.

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2.4. Particle size distribution The particle size distributions of the spray dried powders were determined using Laboratory test sieve (AS 200 digit, ASTME 11, Retsch, Germany). 2.5. Optical microscope An optical microscope (Polarizing Microscope Axioskop-po, Zeiss) was used to investigate the feed liquids before spray drying and the spray dried powders. The picture was taken at 200 magnication. 2.6. Scanning electron microscopy Scanning electron microscope (SEM) (JEOL JSM-6301F, Jeol Ltd., Tokyo, Japan) was used to study the morphological properties of the spray-dried powders. Powder particles were attached to the SEM stubs of 100 diameter using a twosided adhesive tape. The samples were then sputter coated with gold and examined at 500 , 1000 , and 1500 magnications. An acceleration potential of 5 kV was used during micrograph. 2.7. Analysis of total and surface carotene of spray-dried powder The method of Desobry, Netto, and Labuza (1997) with slight modication was used to analyze the total carotene and surface carotene. Total carotene: Powder (50 mg) was weighed into the 125 ml-ask, dispersed in water (2.5 ml) and extracted with hexane (25 ml). After shaking (500 rpm) for 30 min at room temperature, the hexane fraction was measured at 454 nm with spectrophotometer. Surface carotene: Powder (50 mg) was weighed into the ask and extracted with 25 ml hexane. After shaking at 100 rpm for 15 s, sample was centrifuged at 1000g for 1 min. The supernatant was measured at 454 nm with spectrophotometer. 2.8. Cold water solubility of spray-dried powders The method of Singh and Singh (2003) with slight modication was used to analyze cold water solubility of spray dried powders. One gram of powder was mixed with 100 ml of water using a magnetic stirrer at room temperature for 30 min. A 30-ml aliquot of starch solution was transferred to a 50-ml centrifuge tube and centrifuged (Hettich Zentrifugal Universal 16R, German) at speed 430g for 15 min. A 10-ml aliquot of the supernatant was evaporated on a steam bath and dried in an oven at 110 1C for overnight. 2.9. Determination of moisture content and water activity The moisture content of the samples was measured by hot air oven at 105 1C for 16 h. The water activity

of the samples was measured using an AquaLab (CS2, USA). 2.10. Statistical analysis The data reported in all tables are average of triplicate determinations. Analysis of the data was carried out using ANOVA (SPSS program version 10.0 for Windows). Differences between means were tested using the Duncans multiple range tests at Po0.05. 3. Results and discussion 3.1. Dextrose equivalent (DE) and viscosity DE is a measure of degree of hydrolysis of starch molecule, which related to reducing sugar production. The low DE value means lower amount of reducing sugar produced. The modied starch obtained in this investigation had DE value of 2, indicating that degree of hydrolysis was very low. This means that the acid-modied starch obtained in this investigation contained less amount of low molecular weight sugar than maltodextrin with DE value of 24. In other words, this modied starch contained many amylose molecules with shorter chain length, as the result of acid hydrolysis. Results from the measurement of viscosity showed that at 29% w/w maltodextrin had lower viscosity (13.8 cps) than modied tapioca starch (133.8 cps). At 29% the native starch solution was too viscous to measure its viscosity. Therefore, the viscosity of native starch was measured at 20% w/w, which was found to be 31,880 cps. 3.2. Particle size distribution The particle size distributions of spray-dried powders or microcapsules using Laboratory test sieve are shown in Fig. 1. The weight percent data were plotted against the particle diameter in microns. Modied tapioca starch had wider particle size distribution, toward the smaller diameters, as compared to its native starch and maltodextrin. The most predominant diameters for modied tapioca starch were 75150 m (55.8%), for native starch were 106250 m (69.7%) and for maltodextrin were 106250 m (80.0%). The larger powder particle sizes of maltodextrin can be explained by agglomeration or caking of powder particles, which were observed in this sample. 3.3. Optical microscope Light micrographs of feed liquids and spray-dried powder are showed in Figs. 2 and 3, respectively. Results clearly showed signicant differences among wall materials. The modied tapioca starch showed disintegration of some granules; only a few starch granules still exhibited maltese cross as compared with the native starch. This result indicated that steam pressure treatment caused

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a
Weight (%)

60 50 40 30 20 10 0
< 75 75-106 106-150 150-250 250-300 300-500 500-850 > 850

Particle diameter (u)

b
Weight (%)

60 50 40 30 20 10 0
< 75 75-106 106-150 150-250 250-300 300-500 500-850 > 850

Particle diameter (u)

c
60 50 Weight (%) 40 30 20 10 0
< 75 75-106 106-150 150-250 250-300 300-500 500-850 > 850

Particle diameter (u)

Fig. 1. Particle size distribution of spray-dried powders of b-carotene in (a) modied tapioca starch, (b) native tapioca starch, and (c) maltodextrin.

changes in granular structure of acid modied starch. In the case of maltodextrin, completely disintegration of starch granules was observed. 3.4. SEM of spray-dried powders Spray-dried powders prepared from modied tapioca starch, native tapioca starch, and maltodextrin were observed for granular structure using SEM (Figs. 4 and 5). Results clearly showed signicant differences in size and shape. Microcapsules from modied tapioca starch showed spherical shape with extensive dented surface, while those from native tapioca starch showed rounded shape, smooth surface with no obvious dents. Modied tapioca starch had granules size ranging from o5 to 30 mm, while native tapioca starch had more homogeneous granules ranging in size from 2 to 18 mm. Formation of dented surfaces of spray-dried particles was attributed to the shrinkage of the particles during the

Fig. 2. Light micrographs of in feed liquid. (a) Modied tapioca starch, (b) native tapioca starch and (c) Maltodextrin.

drying process (Rosenberg, Kopelman, & Talmon, 1985, 1990). The extensive dented surfaces of modied tapioca starch was probably attributed to starch granule disrupted resulted in more susceptible to shrinkage during the drying stages. The SEM micrograph of spray-dried maltodextrin showed spherical shapes with smooth and some dented surfaces, and a more heterogeneous size, which mainly

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Fig. 4. SME (500 ) of spray dried powders of b-carotene in (a) modied, tapioca starch, (b) native tapioca starch, and (c) maltodextrin. Fig. 3. Light micrographs of spray dried powders of b-carotene in (a) modied tapioca starch, (b) native tapioca starch and (c) maltodextrin.

consisted of very small granules size o7 mm and few large size of 717 mm. The less dented surface of maltodextrin comparing to modied tapioca starch could be attributed to the difference in sugar composition. Maltodextrin used in this study had DE of 24. Therefore, it consisted of a greater amount of low molecular weight sugar. These low molecular weight sugars may act as a plasticizer preventing shrinkage of the surface during drying. According to

Zhang, Ping, and Xiao (2000) plasticizer is important for the formation of spherical microcapsules with smoothsurface. Bruschi et al. (2003) used gelatin to encapsulate propolis by spray drying and reported that addition of mannitol to gelatin resulted in smooth-surfaced microparticles of propolis. 3.5. Cold water solubility of spray-dried powders Cold water solubility among spray-dried powders showed signicant (Po0.05) differences (Table 1). Modied tapioca

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J. Loksuwan / Food Hydrocolloids 21 (2007) 928935 933 Table 2 Moisture content and water activity of spray dried powders of b-carotene in (A) modied tapioca starch, (B) native tapioca starch, and (C) maltodextrin Type A B C Moisture content (%) 3.1270.39b 6.0070.62c 2.1170.47a Water activity 0.2970.09ab 0.3770.04b 0.2270.02a

Mean of three replicates; means within column followed by different superscripts, are signicantly different at Po0.05 by Duncans test.

starch had higher cold-water solubility than its native starch. Maltodextrin had the highest cold-water solubility, completely soluble. These differences could be attributed to the differences in granular structure. Treatment of tapioca starch with acid resulted in partial depolymerization of starch into smaller molecules resulted in a greater amount of more soluble components. When this starch was heated under steam pressure, the tight organization of starch granules was disrupted, which facilitated the migration of water into the granules and additional leaching out of soluble components. This resulted in an increase in solubility of modied starch. 3.6. Moisture content and water activity of spray-dried powders Moisture contents and water activity of spray-dried powders are shown in Table 2. Moisture contents of spraydried powders varied from 2.116.00% and were differed signicantly (Po0.05). Modied tapioca starch showed lower moisture content than its native starch. Maltodextrin had the lowest moisture content. Similar results were observed for water activity. These differences could be attributed to the structure of granules and viscosity of starch. Native tapioca starch had more rigid or tight crystalline structure and high viscosity (as mentioned earlier), as compared to modied tapioca starch and these could inuence rate of drying. 3.7. Total carotene and surface carotene of spray-dried powders Total carotene and surface carotene contents among the powders are shown in Table 3. There were signicant differences in total carotene and surface carotene contents among the wall materials used. Modied tapioca starch had higher total carotene content (82.18%) than its native starch (68.35%). Maltodextrin showed the lowest total carotene content (46.74%). Surface carotene contents of the dried powders ranged from 19.59% to 104.08%. Modied tapioca starch had the lowest surface carotene while native tapioca starch had the highest surface carotene. These results indicated that, of the wall material studied, modied tapioca starch treated with steam

Fig. 5. SME (1500 ) of spray-dried powders of b-carotene in (a) modied tapioca starch, (b) native tapioca starch, and (c) maltodextrin.

Table 1 Cold-water solubility of spray-dried powders of b-carotene in (A) modied tapioca starch, (B) native tapioca starch, and (C) maltodextrin Type A B C Cold water solubility 90.2572.21b 2.2770.39a 98.4370.28c

Mean of three replicates; means within column followed by different superscripts, are signicantly different at Po0.05 by Duncans test.

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934 J. Loksuwan / Food Hydrocolloids 21 (2007) 928935 Table 3 Total carotene and surface carotene contents of spray dried powders of bcarotene in (A) modied tapioca starch, (B) native tapioca starch, and (C) maltodextrin Type A B C Total carotene (%) 82.1871.47b 68.3573.76c 46.7476.56a Surface carotene (%) 19.5971.40a 104.0873.66c 73.0274.37b

prepared acid modied tapioca starch as compared to its native starch.

Acknowledgments This study was nancially supported by National Research Council of Thailand. The author would like to thank Burley Jucker Specialties Ltd. (Bangkok, Thailand) for providing maltodextrin.

Mean of three replicates; means within column followed by different superscripts, are signicantly different at Po0.05 by Duncans test.

pressure had the highest encapsulation efciency. This was probably due to the composition of modied tapioca starch after steam pressure treatment. The free soluble amylose associated to form a continuous network joint by hydrogen bonds, resulting in a gel structure that entrapped bcarotene in this structure. In addition, amylose is good in lm forming ability; therefore, the presence of high levels of free soluble amylose of modied tapioca starch may have advantages of a rapid crust forming around the b-carotene preventing the loss of b-carotene during drying process. Major lost of volatiles during spray drying was reported to occur at the very early stages of drying process (Reineccius, 1988). Therefore, wall materials, which can form lm rapidly at the surface of drying droplet will exhibit a better avor retention during drying. Rosenberg et al. (1990) reported that increase of soluble solids concentration resulted in decreased the time required for powder crust formation, and consequently, losses of volatiles were reduced. In the case of maltodextrin, the low total carotene content obtained was probably due to the lack of emulsication and low lm-forming capacity resulted in poor b-carotene retention during drying. Maltodextrin used in this study contained molecules, which are too small to impart the emulsifying characteristics. The high-surface carotene content observed for native tapioca starch could be attributed to the high viscosity of the starch. High viscosity caused an increase in time of droplet formation and internal mixing (Rosenberg et al., 1990). And these may allow the carotene to migrate to the surface prior to the formation of dry crust around the particles. 4. Conclusion The results of this study indicate laboratory prepared acid modied tapioca starch after treated with steam pressure has the potential for use as wall material. Acid treatment in combination with steam pressure yields starch with low viscosity at high solid. This starch provided good retension of b-carotene during drying process. The low-surface carotene contents were also observed for this modied tapioca starch which indicates better microencapsulation efciencies. Spray-dried powders from modied tapioca starch showed higher cold-water solubility than its native starch. Changes in surface morphology were observed for microcapsules obtained from laboratory

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