Evaluation of type and concentration of wall materials in D-Limonene microencapsulation to determination of optimum condition for flavored rock candy production

Document Type : Research Article


1 Food Science and Technology, Ferdowsi university, International Campus

2 Department of Food Science and Technology, Faculty of Agriculture, Ferdowsi University of Mashhad, Iran

3 Department of Food Processing, Research Institute of Food Science and Technology, Mashhad, Iran


The aim of this study was to produce D-limonene microcapsule with resistant coat (Gum Arabic and maltodextrin) for manufacturing flavored crystal rock candy. Oil-in-water emulsions were prepared at concentrations of 10% and 20% and related characteristics including particle size and emulsion capacity were examined. Microcapsule properties produced by spray drying process such as surface oil content, oil retention, encapsulation efficiency, release rate and morphological characterization by SEM were also evaluated. The results showed that an increase in GA concentration had significant effect on examined factors as the higher ratio of GA/MD led to decrease in z-average diameter. Moreover, the release rate decreased due to increase in wall materials concentration upon 6 weeks at room temperature. Optimal microcapsule by its properties (75/25 of GA/MD by 20% of wall materials), was used to produce flavored rock candy so that, the effect of temperature, pH and the amount of microcapsule on yield and the time for formation of first crystal were investigated. The influence of pH and the amount of microcapsule on yield and also syrup’s temperature and the amount of microcapsule on the time for formation of first crystal were significant (P<0.05). Therefore, to reach the highest yield of rock candy production, 11.80%, and optimum time for the first crystal to be formed, 33.742 min, considering factors were determined as the temperature adjusted on 85 °C, 0.04 gr of microcapsule and pH value of 6.99.


[1] Viclavi, ‌ A. V., Christian, E.W. (2008). Essential of food science, In: Sugars, sweeteners and confections, 3th ed., Springer, pp 331-348.
[2] سازمان ملی استاندارد 1388. نبات – ویژگی و روش‌های آزمون. استاندارد ملی ایران شماره 739.
[3] Gholamhosseinpour, A., Varidi, M. J., Elahi, M., Shahidi, F. (2008). Evaluation of traditional production process of rock candy and optimization of sucrose crystallization (Part2). American-Eurasian J. Agric. & Environ. Sci., 4 (2), 150-155.
[4] Madene, A., Jacquot, M., Scher, J. and Desobry, S. (2006). Flavour encapsulation and controlled release- a review. J. Food Sci. Tech., 41, 1-21.
[5] Juteau, A., Cayot, N., Chabanet, C., Doublier, J. L., Guichard, E. (2004). Flavor release from ­polysaccharide gels: different approaches for the determination of kinetic parameters. Trends Food Sci. Tech., 15, 394-402.
[6] Cho, Y.H., Shin, D.S. and Park, J. (2000). Optimization of emulsification and spray drying processes for the microencapsulation of flavor compounds. Korean J. Food Sci. Tech., 32, 132–139.
[7] Chen, X.G., Lee, C.M. and Park, H.J. (2003). O/W emulsification for the self-aggregation and nanoparticle formation of linoleic acid modified chitosan in the aqueous system. J. Agric. Food. Chem., 51, 3135–3139.
[8] Zhu, F (2017). Encapsulation and delivery of food ingredients using starch based systems, J. Food. Chem., 229, 542-552.
[9] Gharsallaoui, A., G. Roudaut. (2007). Applications of spray-drying in microencapsulation of food ingredients: An overview. J. Food Res., 40, 1107-1121.
[10] Zuidam, N.J., Shimoni, E. (2010). Overview of microencapsulates for use in food products or processes and methods to make them, In Zuidam N.J, Nedovic V.A., (Eds.). Springer-Verlag New York., 3-29.
[11] Jafari, S. M., Assadpoor, E., He, Y., Bhandari, B. (2008). Encapsulation efficiency of food flavors and oils during spray drying. Drying Tech., 26, 816–835.
[12] Renu, R., Fathima, Z. (2015). Microencapsulation of flavors. Int. j. basic appl. biol., 2 (5), 333-338.
[13] نجف نجفی، م. (1389) استفاده از امواج فراصوت در تولید امولسیون و ریزپوشانی ترکیبات موثره روغن هل. پایان نامه دکتری تخصصی، دانشگاه فردوسی مشهد.
 [14] Hogan, S. A., McNamee, B. F., O’Riordan, D. O’Sullivan, M. (2001). Microencapsulating properties of whey protein concentrate. J. Food Sci., 66 (5), 675-680.
[15] Bertolini, A.C., Siani, A.C., Grosso, C. R.F. (2001). Stability of monoterpenes encapsulated in gum Arabic by spray-drying. J. Agric. Food Chem., 49, 780–785.
[16] Beristain, C. I., García, H. S., Vernon-Carter, E. J. (2001). Spray-dried Encapsulation of Cardamom (Elettaria cardamomum) Essential oil with mesquite (Prosopis juli-ora) Gum. Lebensm.-Wiss. u.-Technol., 34, 398-401.
 [17] Krishnan, S., Kshirsagar, A.C. and Singhal, R.S. (2005). The use of gum Arabic and modified starch in the microencapsulation of a food flavoring agent. Carbohydr Polym., 62, 309-315.
[18] Barbosa, M.I.M.J., Borsarelli, C.D. and Mercadante, A.Z. (2005). Light Stability of spray-dried bixin encapsulated with different edible polysaccharide preparations. J. Food Res., 38, 989-994.
[19] Kanakdande, D., Bhosale, R., Singhal, R. S. (2007). Stability of cumin oleoresin microencapsulated in different combination of gum arabic, maltodextrin and modified starch. Carbohydr Polym., 67, 53-541.
[20] Fernandes, R.V., Borges, S.V. (2014). Gumarabic/starch/maltodextrin/inulinas wall materials on the microencapsulation of rosemary essential oil. Carbohydr Polym., 101, 524-532.
[21] صادقیان، ع. (1392) بررسی برهمکنش‌های بین مولکولی بر ویژگی‌های امولسیون و ریزکپسول روغن هل. رساله دکتری، دانشگاه فردوسی مشهد.
[22] Jinapong, N., Suphantharika, M., Jamnong, P. (2008).  Production of instant soymilk powders by ultrafiltration, spray drying and fluidized bed agglomeration.  J. Food Eng., 84, 194–205.
[23]  نجف نجفی، م.؛ کدخدایی، ر. (1390) ریزپوشانی لیمونین به روش خشک کردن انجمادی: تاثیر نوع و غلظت دیواره. نشریه پژوهش‌های علوم و صنایع غذایی ایران. جلد 7. شماره 3. ص 210-217.
[24] قهرمانی فر، امین.؛ محمدی ثانی، علی.؛ نجف نجفی، مسعود.؛ قهرمانی فر، مهدی. (1389). تاثیر ویژگی‌های امولسیون  بر خصوصیات پودرهای حاصل از فرایند ریزپوشانی. مجله علمی پژوهشی علوم و فناوری غذایی. سال 2. شماره 2.
 [25] Vaidya, S., Bhosale, R., & Singhal, R.S. (2006). Microencapsulation of cinnamon oleoresin by spray drying using different wall materials. Dry Tech., 24, 983–992.
 [26] Jafari, S. M., Bhandri, Y. H. E. (2007). Effectiveness of encapsulating biopolymers to produce sub-micron emulsions by high energy emulsification techniques. Food Res Int., 40, 862-873.
[27] حسین زاده، م؛ حداد خداپرست، م. ح.؛ بستان، ا.؛ محبی، م. (1395) ریزپوشانی روغن نعناع (menthaspicata) به روش خشک کردن پاششی. نشریه پژوهش‌های علوم و صنایع غذایی. جلد 12. شماره 4. ص 499-511.
[28] میرعلایی‌مطلق، م.؛ آریان فر، ا.؛ شهیدی نوقابی، ا. م. (1394) ریزپوشانی روغن زنجبیل در عصاره چای سبز با نشاسته‌ی اصلاح شده و مالتودکسترین. ویژه نامه علوم و صنایع غذایی. جلد 13. شماره 1.
[29] Dickinson, E. (2010). Food emulsions and foams: Stabilization by particles. Current Opinion in Colloid & Interface Science., 15, 40-49.
[30] Buff, R. A., Reineccius, G. A., and Oehlert, W. O. (2002). Influence of time-temperature treatment on the emulsifying properties of gum acacia in beverage emulsion. J. Food Eng., 51, 341-345.
[31] Hojjati, M., Razavi, H., Rezaei. K., Gilani, K. (2013). Effect of wall components on characteristics of natural canthaxanthin microencapsulated using spray-drying. Iranian J. Nutrition Sci & Food Tech., 8(3), 46-54.
[32] Muzaffar, K., Kumar, P. (2015). Parameter optimization for spray drying of tamarind pulp using response surface methodology. Powder Tech., 279, 179-184.
[33] Tonon, R. V., Brabet, C., Hubinger, M. D. (2008). Influence of process conditions on the physicochemical properties of acai (Euterpe oleraceae Mart.)  Powder produced by spray drying. J. Food Eng., 88 (3), 411–418.
[34] Papadakis, S. E., Gardeli, C., Tzia, C. (2006). Sprays drying of raisin juice concentrate. Dry Tech., 24, 173-180.
[35] Subramaniam, A., Veazey, R. L., Schober, A., Rada, A., Rong, Y., van Sleeuwen, R. A. T., Golding, R., Zhang, N. (2013). Orange oil stability in spray dry delivery systems, Carbohydr Polym., 97 (2), 352-357.
[36] Soottitantawat, A., Yoshii, H., Furuta, T., Ohgawara, M., & Linko, P. (2003). Microencapsulation by spray drying: Influence of emulsion size on the retention of volatile compounds. J. Food Sci., 68, 2256 – 2262.
 [37] Thijssen, H.A.C., & Rulkens, W.H. (1968). Retention of aromas in drying food liquids. De Lngenieur., 47, 45-56.
[38] Badee, A. Z. M.; Abd El- Kader, Amal E.; Aly, Hanan M. 2012. Microencapsulation of peppermint oil by spray drying. Australian J. Basic&Applied Sci., 6(12), 499-504.
[39] Soottitantawat, A., Bigeard, F., Yoshii, H., Furuta, T., Ohkawara, M. and Linko, P. Influence of emulsion and powder size on the stability of encapsulated d-limonene by spray drying. (2005). Innovative Food Sci & Emerging Tech.,6, 107– 114.
[40] Akhavan Mahdavi. S., Jafari. S.M., Assadpoor, E., Dehnad, D. (2016). Microencapsulation optimization of natural anthocyanins with maltodextrin, gum Arabic and gelatin. Int. J. Biol. Macromol., 8, 379–385.
[41] Chraniot, C., Tzia, C. (2014). Arabic gum Mixtures as encapsulating agents of freeze-dried fennel oleoresin products. Food Bioproc Tech., 7, 1057–1065.
[42] Rubiano, K. D., Cárdenas, J. A., Ciro, V. H. J. (2015). Encapsulation of d-limonene flavors using spray drying: Effect of the addition of emulsifiers. Ingeniería Competitivdad., 17 (2), 77-89.
[43] Gholamhosseinpour, A., Varidi, M. J., Elahi, M., Shahidi, F. (2008). Evaluation of Traditional Production Process of Rock Candy and Optimization of Sucrose Crystallization (Part 1).  American-Eurasian J. Agric. & Environ. Sci., 4 (1), 72-75.
[44] غلامحسین پور، ع.؛ الهی، م.؛ وریدی، م. ج.؛ شهیدی، ف. (1387) بررسی فرایند سنتی تولید نبات و معایب آن. پژوهشهای علوم و صنایع غذایی ایران.  دوره 4،  شماره  1 (نیمه اول) ، ص 23 – 35.