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    Food Hydrocolloids 33 (2013) 199e206

    Contents lists available

    Food Hydrocolloids

    journal homepage: www.elsevier .com/locate/ foodhyd

    Inulin potential for encapsulation and controlled delivery of Oreganoessential oil

    Sara Beiro-da-Costa a,b,c,*, Cludia Duarte a, Ana I. Bourbon b, Ana C. Pinheiro b,M. Isabel N. Janurio a, Antnio A. Vicente b, M. Lusa Beiro-da-Costa a, Ivonne Delgadillo c

    aCEER e Biosystems Engineering, Instituto Superior de Agronomia, Technical University of Lisbon, Tapada da Ajuda, 1349-017 Lisboa, Portugalb IBB e Institute for Biotechnology and Bioengineering, Centre of Biological Engineering, University of Minho, Campus de Gualtar, 4710-057 Braga, PortugalcChemistry Department e Research Unit QOPNA e University of Aveiro, Campo de Santiago, 3810-193 Aveiro, Portugal

    a r t i c l e i n f o

    Article history:Received 14 January 2013Accepted 18 March 2013

    Keywords:InulinEncapsulationCapsules morphologyCapsules structureOregano essential oilReleasing ability

    * Corresponding author. CEER e Biosystems EnginAgronomia, Technical University of Lisbon, TapadaPortugal. Tel.: 351 3653246.

    E-mail address: (S. Beiro-da

    0268-005X/$ e see front matter 2013 Elsevier Ltd.

    a b s t r a c t

    The ability of inulin, a prebiotic material, as encapsulation matrix was explored. Microcapsules of Raf-tiline were produced by spray drying inulin solutions at different solids content (5, 15 and 25%) at 120,155 and 190 C, according to a Central Composite Rotatable design. Produced capsules were analysed formorphology and size by SEM and physiochemical characterized by DSC, IR and RAMAN. Oreganoessential oil was incorporated in the inulin solutions at 15% solids basis and the emulsions dried at thesame conditions. The above mentioned methodologies were applied to evaluate the encapsulation abilityand the changes induced by the presence of the EO in capsules morphology and structure. Furthermorethe kinetics and amount of release was assessed by a spectrophotometric method. Results showed that itwas possible to produce regular spherical inulin microcapsules (3e4.5 mm) for all the tested experi-mental conditions. According to IR and Raman results mainly drying temperature affected the structureof the capsules, three groups being clearly formed. These groups could be related to the morphology ofinulin crystals. The EO was successfully encapsulated in the system as demonstrated by IR and Ramananalysis. The differences found in the EO releasing amount, make clear that different degrees of corematerial retention is achieved, what should be related to structural changes in the matrix wall, denotingin some processing conditions interactions phenomena among inulin and EO. Those different releasingprofiles patterns may be quite useful in finding different potential uses for the encapsulates.

    2013 Elsevier Ltd. All rights reserved.

    1. Introduction

    Inulin belongs to the group of fructans that naturally occurs asplant storage carbohydrate in many members of the Asteraceaefamily. It is a polymer of b(2/1)-linked D-fructose units, consti-tuting chains of different lengths each of them with a terminalglucose unit. As summarized by Barclay, Ginic-Markovic, Cooper,and Petrovsky (2010), in this structure only one atom of the poly-mer backbone is attached to the fructose ring making inulin un-usually flexible for a polysaccharide conferring its ability to assumea range of different structures.

    Among the natural sources of inulin, industrial chicory(Cichorium intybus L., var. sativum) is one of the most important,due to its high content of inulin and the presence of a considerable

    eering, Instituto Superior deda Ajuda, 1349-017 Lisboa,


    All rights reserved.

    fraction of inulin compounds with a high degree of polymerisation(Janurio, 1999; Orafti, 1996; Van Loo, Coussement, De Leenheer,Hoebregs, & Smits, 1995). Inulin and fructooligosaccharides areactually important natural ingredients used in food industry by itsvery interesting and diversified technological and functionalproperties. These compounds behave as prebiotics what meansthey are non-digestible by the human organism only beingdegraded by certain colon bacteria (probiotics) like bifidobacteria(Gibson & Kolida, 2007; Roberfoid, 2007). This selective stimula-tion of those gut bacteria provides several benefits to the hosthealth (Kaur & Gupta, 2002; Roberfroid, 2000). Additionally, toinulin are attributed important biological effects such as anti-cancer (Korbelik & Cooper, 2007) and immunomodulatory prop-erties (Silva, Cooper & Petrovsy, 2004). Besides the uses in the foodindustry it has also important applications in pharmaceutical, asexcipient, stabilizer and slow release drug delivery medium(Barclay et al., 2010).

    Microencapsulation is a technology that allows sensitive in-gredients to be physically entrapped in a homogeneous or

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  • Table 1Experimental design. Coded and decoded values of independent variables.

    Inulin (%) Temperature (C) Inulin (%) Temperature (C)

    1 1 5 1201 1 5 1901 1 25 1201 1 25 1901 0 5 1551 0 25 1550 1 15 1200 1 15 1900 0 15 1550 0 15 155

    S. Beiro-da-Costa et al. / Food Hydrocolloids 33 (2013) 199e206200

    heterogeneous matrix aiming at their protection. The encapsula-tion can be achieved by several processes such as spray-drying,spray-cooling, spray-chilling, freeze-drying, coacervation, etc..(Gouin, 2004). However, mainly due to the low cost and availableequipment sprayedrying is the most commonly applied technol-ogy (De Vos, Faas, Spasojevic, & Sikkema, 2009; Gharsallaoui,Roudaut, Chambin, Voilley, & Saurel, 2007; Lopez-Rubio, Gavara,& Lagaron, 2006).

    Spray-drying is a unit operation by which a liquid product isatomized in a hot gas current to instantaneously obtain a powder.The initial feed material can be a solution, an emulsion or a sus-pension and the final product obtained, depending also on oper-ating conditions, can be a powder with particles ranging from 10 to50 mm (Gharsallaoui et al., 2007).

    Among others, the most common polymers used for food in-gredients encapsulation include gelatine (Chiu et al., 2007; Shu, Yu,Zhao, & Liu, 2006), arabic gum (Brckner, Bade, & Kunz, 2007;Kanakdande, Bhosale, & Singhal, 2007), modified starches(Brckner et al., 2007; Kanakdande et al., 2007) and whey protein(Brckner et al., 2007).

    Oregano is an aromatic plant quite widespread in Mediterra-nean countries, used as food ingredient due to the pleasant flavour.Besides, the antioxidant (Fasseas, Mountzouris, Tarantilis, Polissiou,& Zervas, 2008; Kulisic, Radonic, Katalinic, & Milos, 2004) andantimicrobial (Govaris, Solomakos, Pexara, & Chatzopoulou, 2009;Seydim & Sarikus, 2006) properties of Oregano essential oil (EO)makes this natural component also a good option as food preser-vative (Goulas & Kontominas, 2007) and health promoter. Carvacroland thymol are the two main phenols that constitute oregano EOand primarily responsible for its antioxidant activity (Kulisic et al.,2004). However, EO composition can be changed as result ofoxidation, chemical interactions or volatilization. To limit aromadegradation/loss during processing and storage and to control thedelivery of the compound at the desired time and site encapsula-tion of volatile ingredients are beneficial prior to use in foods orbeverages (De Vos et al., 2009; Madene, Jacquot, Scher, & Desobry,2006).

    Moreover and related to the prebiotic action it should also benoted the accrued interest of the potential use of inulin as wallmaterial for encapsulation/protection of bioactive compoundssusceptible to changes/degradation along the human digestivetract, since its release takes place only in the intestine, where theywill be absorbed. Due to these functional properties, in addition totheir technological properties and its low price (De Vos et al., 2009)drew the attention of inulin by the food industry. However till nowin the food field, the use of inulin as wall material is almost un-exploited. Sanz, Tapia, Chvez, & Robert (2009) report the ability ofinulin for microencapsulation of bioactive compounds from cactuspear fruit.

    To assess the ability of a microcapsule to act as an active agentcarrier, diffusion of the selected compounds should be analysed.The rate of diffusion of a compound through the polymer wall of amicrocapsule strongly depends on the preparation method of themicrocapsules and on the permeability of the polymer membrane(Hansan et al., 2007).

    The objective of the present work is to evaluate the potentialof inulin as wall material for encapsulation and controlled releaseof Oregano essential oil. In order to understand both the charac-teristics of the wall capsules and the way the essential oil isthereat retained the use of several accessing methodologies areneeded. In this scope morphological, physical and chemicalproperties of spray-dried materials accessed by scanning electronmicroscopy (SEM), differential scanning calorimetry (DSC), ATR-MID infrared spectroscopy and RAMAN were used as analyticaltools.

    2. Mat