BR102012028472A2 - Tucupi microencapsulated powder and process for obtaining it - Google Patents

Abstract

Tucupi microencapsulated powder and process for obtaining it. The present invention relates to the microencapsulated tucupi powder product and process for obtaining it using the starch hydrolyzate maltodextrin as encapsulating agents. Both the product and the proposed process aim to expand the commercialization of this raw material and increase its commercial life through spray drying or spray drying. The optimized product has less total cyanide and a higher yellow color parameter, and less water activity, which is ideal for the final product. The efficient encapsulation of the product was performed by scanning electron microscopy (mev) thus optimizing the product.

Description

Patent Descriptive Report: "MICROENCAPSULATED POWDER TUCUPI AND PROCESS FOR OBTAINING IT".

FIELD OF THE INVENTION The present invention relates to the microencapsulated tucupi powder product and process for obtaining it using starch hydrolysed encapsulating agents such as malt dextrin. Scanning Electron Microscopy (SEM) was used to validate the optimized product. Both the product and the proposed process aim to expand the commercialization of this raw material and increase its commercial life through spray drying or spray drying.

BACKGROUND OF THE INVENTION Cassava, from the Euphorbiaceae family, is one of the main basic energy foods of the Brazilian population. It is grown in over 80 countries (SILVA, P. A., ASSIS, G.T.

Processing of extruded breakfast cereal enriched with whey protein concentrate. 2006. 70f. Final Paper, Agroindustrial Technology - Food, State University of Pará. 2009). It is estimated that more than 500 million people living in the tropics have cassava as their main source of food (PAÉZ, E. La Investigación Integrada boosts La agroindustia de La yuca in Colombia. Cali-Colombia. CIAT International, v. 13, (1, pp. 4-5, March 1994). Cassava is cultivated in all regions of Brazil, assuming a prominent importance in human and animal food, besides being used as raw material in many industrial products. (MATTOS, P. L. P .; CARDOSO, E. M. R. Cassava Growing for the State of Pará: Economic Importance. Embrapa Cassava and Fruit. Production Systems, ISSN 1678-8796, electronic version. January, 2003).

Cassava roots have an average composition of 68.2% moisture, 30% starch, 2% ash, 1.3% protein, 0.2% lipid and 0.3% fiber (CHISTÉ, RC Study of the physicochemical and microbiological properties in the production of cassava flour from dry and water groups, fine subgroup, type 1. 67f Course Conclusion Paper - Agroindustrial Technology in Food, State University of Pará. ). Cassava roots are therefore essentially energetic, with high carbohydrate levels, mainly polysaccharides. Tucupi is defined as a product or byproduct of cassava root (Manihot esculenta Crantz) and its varieties, predominantly used in Northern Brazilian cuisine, and obtained through an appropriate technological process. This is the partially fermented sauce of the manipueira, which is the milky-looking liquid and light yellow color that drips from the cassava roots (Mcmihot esculenta Crantz), by pressing the grated mass of cassava. It is a byproduct or residue from the industrialization of cassava, which physically is in the form of aqueous suspension and chemically as a miscellany of compounds such as: gum (5 to 7%), glucose and other sugars, proteins, skin cells, denmark and cyanogenic derivatives (hydrocyanic acid, cyanides and aldehydes), various substances and different mineral salts. This sauce rests for one or two days to decant the starch, which is then removed, naturally occurring its fermentation and then boiling (ADEPARÁ - Pará State Agricultural Defense Agency. Tucupi: Identity, quality, packaging and labeling of tucupi Belém - PA, 2008. 12p). The tucupi is a genuinely Amazonian product and can be used as a condiment, sauce or can also be the main raw material of many regional dishes much appreciated by the people of Pará and other regions of Brazil. Among these dishes, we can mention “Tacacá” and “Pato no tucupi”. The technology of tucupi manufacturing is simple, but requires some care in its processing. Selection of the right raw material, hygiene and care throughout the processing are fundamental factors to ensure its quality. Tucupi is a product that has high humidity, greater than 94%, and this factor leads to rapid deterioration of this product in a natural way. This makes the product very perishable, which makes it difficult to transport and store, as well as making the costs of maintaining a good shelf life more expensive. Thus, the production of tucupi powder meets this need, so that the reduction in product moisture directly increases the shelf life of the product, thus expanding the horizons of product transport over long distances. and even exports to other countries (Chisté, Renan Campos, Cohen, Kelly Oliveira and Oliveira, Suzy Sarzi Study of the physical and chemical properties of tucupi. Ciênc. Tecnol. Aliment., Sep 2007, vol.27, no.3 , p.437-440).

For the production of tucupi powder, a possible alternative is dehydration, ie the total or partial removal of water available in a food. The method of dehydration or drying of liquids should be selected based on the physical and chemical properties of the feed. high quality powder is obtained. In the state of the art, dehydration is usually employed by two processes, lyophilization and atomization. The choice of drying technique and additives is also linked to economic factors: freeze drying is more expensive, while spray drying is a good option for drying products with high solids concentration. Freeze drying is a process carried out on its own equipment called freeze drying, its process is done under vacuum, where the water is removed by sublimation, therefore called "cold drying", making it an effective process. However, its disadvantage is its production performed in batches, that is, there is no continuity, which makes the process more susceptible to the proliferation of microorganisms (FURUTA, T.; HAYASHI, H.; OHASHI, T. Some criteria of spray drier design fo food liquid (Drying Technology, v. 12, no 1-2, pp. 151-177 (1994)).

Another state of the art process is atomization. Spray drying, also known as nebulization or spray drying, had its principles established in the mid-16th century, when the first egg drying operation was patented. However, the beginning of its use on an industrial scale dates from the 1920s.

The first large-scale spray drying products were milk and washing powder. Since then, its use has spread throughout the process industry in general, and today is especially applied for drying pharmaceutical and food products. Spray drying is a continuous process where a liquid or paste is transformed into a dry product in the form of a powder, characterized by a relatively short drying time. The process basically consists of atomizing the liquid in a compartment that receives a hot air flow, so that the rapid evaporation of water allows to keep the temperature of the particles low. Thus, this technique allows the drying of heat sensitive products, such as food, biological and pharmaceutical products, without affecting too much their qualities and characteristics (ΤΟΝΟΝ, RV Acai juice spray drying: Influence of process variables, quality and product stability 242f Thesis Doctorate in Food Engineering - Faculty of Food Engineering, State University of Campinas (Campinas, 2009). The composition of tucupi consists approximately of 1.1% starch, which when subjected to hot processes results in a gel-shaped tucupi, also known as starch gelation or retrogradation. In order to prevent starch gelation, the microencapsulation methodology, which consists of entrapping an active agent, small solid particles, liquid droplets or gaseous compounds in a protective shell, thin films or polymeric coatings, is used to be released into a certain condition. The material to be encapsulated is referred to as a “stuffing material”, “active material” or “internal phase”, while the material forming the coating is called “wall material”, “carrier”, “membrane” or “shell”. " In said process, the active agent is tucupi and the protective shell is a starch hydrolyzate.

Starch hydrolysates are α-D-glucose units joined by glycosidic bonds, generally described by their equivalent dextrose, which is the ability to polymerize. The equivalent number of dextroses determines the characteristics of the polysaccharides. According to the state of the art of encapsulating agents, hydrolysates highlighted by the high encapsulating activity of choice may be gum arabic and maltodextrin, when compared to other polysaccharides and proteins, in carbohydrate encapsulation. Maltodextrin is a hydrolyzate widely used in food microencapsulation due to its low cost, the fact that it is less hygroscopic than corn syrups, does not have sweetness and contribute to the body of the food system. The microencapsulation process is widely used by the food industry to decrease the reactivity of a product with the external environment. In drying processes the presence of sugars and / or polymers in the encapsulation system reduces the water content (RIGHETTO, A. M.

Physicochemical characterization and stability of microencapsulated green acerola juice by atomization and lyophilization. Thesis (PhD in Nutrition Science) - Faculty of Food Engineering, State University of Campinas. Campinas, 2003. Available at: <http://bibl Biblioteca.universia.net/fícha.do?id=3901733>. Accessed: August 1, 2009. 176 p.). The drying process is aimed at reducing moisture, so decreasing moisture along with water activity reduces the speed of degradation reactions as well as decreases the amount of water available to serve the metabolism of microorganisms.

Specifically in the case of the production of tucupi powder obtained by spray drying and maltodextrin microencapsulated, atomization proves to be the suitable process for production, since in addition to being a continuous process, the material is subjected to higher temperatures. able to volatilize cyanide, toxic and unwanted substance to the final product. The innovation of the present invention is the production of tucupi powder through spray drying, using maltodextrin as encapsulating agent of the product.

The state of the art discloses the use of drying processes for various products. The process of obtaining dehydrated manipuera, in which its definition was described in patent BR0203896-0, which had as its theme the “Preparation of manipueira powder for use as agricultural input: defensive and fertilizer”, in which the process of freeze drying. This process is made cold, which does not affect the alteration of the properties of the food, however, for tucupi is necessary the extraction of cyanide (CN), responsible for conferring toxicity to it. Cyanide loss occurs through a volatilization process when subjected to hot processes. Spray drying is widely used for product dehydration. Patent application BR0902253-8 deals with the "Process for obtaining Juçara Pulp Powder and / or Concentrate for Use as a Functional Food", wherein the atomization process is used to obtain an Acai Powder Pulp Concentrate. or Juçara. However, when compared to the present proposal, there are changes in the process, and that both the raw material used and the resulting product are different.

SUMMARY OF THE INVENTION The invention relates to a product, tucupi powder, obtained by spray drying and microencapsulated as a starch hydrolyzate, maltodextrin, and its production process. Scanning Electron Microscopy (SEM) was used to validate the production process. The benefits of using the invention are varied, highlighting the possibility of making the product easier to transport and store and especially increasing its shelf life.

In one aspect, the present invention provides a method for obtaining the tucupi powder product, characterized in that it involves the steps of: 1) obtaining the tucupi; 2) use of an encapsulating agent; 3) homogenization and 4) drying, which results in obtaining the microencapsulated tucupi. Consequently, the product may be packaged for storage and marketing purposes.

In another aspect, the present invention is the product the microencapsulated tucupi powder.

The foregoing and additional aspects of the present invention and the manner of obtaining them will become apparent, and the invention will be better understood by reference in the "Detailed Description of the Invention".

BRIEF DESCRIPTION OF THE FIGURES

Figure 1. Flowchart of microencapsulated tucupi processing.

Figure 2 (Annex 1). Response surface for the total cyanide parameter (mg / kg).

Figure 3 (Annex 2). Response surface and contour for the color parameter L *.

Figure 4 (Annex 3). Response surface and contour for parameter a *.

Figure 5 (Annex 4). Response surface and contour for parameter b *.

Figure 6 (Annex 5). Response surface and contour for the Aw parameter.

Annex 6. Experiments 1 (III), 2 (V) and 3 (I), respectively.

Annex 7. Experiments 4 (II), 5 (XI) and 6 (X), respectively.

Annex 8. Experiments 7 (VIII), 8 (IX) and 9 (IV), respectively.

Annex 9. Experiments 10 (VI) and 11 (VII), respectively.

Figure 7. Images of powders resulting from tucupi drying with 10% total solids produced under different inlet air temperatures. (I) 150 ° C, at 20 pm scale; (II) 190 ° C, at a scale of 20 pm.

Figure 8. Images of powders resulting from tucupi drying, with 7.5% total solids, produced under different inlet air temperatures. (I) 170 ° C, at 20 pm scale; (II) 200 ° C, at 20 pm scale.

Figure 9.1 image of experiment V resulting from tucupi drying at 5% total solids at 190 ° C inlet air temperature, in a 20 pm scale.

Figure 10. Image of experiment I resulting from tucupi drying at 10% total solids at 150 ° C inlet air temperature at a scale of 20 pm.

Figure 11. Images of tucupi drying powders at 170 ° inlet air temperature produced under different total solids concentrations. (I) Experiment IX - 11% total solids, 20 pm scale; (II) Central Experiment - 7.5% of total solids, in 20 m scale; (III) Experiment VIII - 4% total solids, 20 pm scale.

Figure 12. Images of powders resulting from tucupi drying at 190 ° inlet air temperature produced under different concentrations of total solids. (I) Experiment II - 10% total solids, 20 pm scale; (II) Experiment V - 5% total solids, 700 pm scale.

DETAILED DESCRIPTION OF THE INVENTION The present invention is for the purpose of obtaining powdered tucupi obtained by spray drying and carbohydrate microencapsulated, preferably maltodextrin, as well as its maximized production process.

In the following description, a number of terms are used extensively. The following definitions are provided to facilitate understanding of the invention. The term “harvest” should be understood as the harvest of cassava roots that should be between 16 and 20 months, preferably between April and August, when they have the maximum yield. Processing should take place immediately after harvest or within 36 hours to avoid loss. During the harvesting process, mechanical damage to the roots should be avoided. The term “Washing” should be understood as the process of eliminating excess soil adhering to the shell and avoiding the presence of impurities that impair the quality of the final product. The term “Peeling” should be understood as the process that eliminates the fibers present in the husks, the tannins that darken the flour and the part of hydrocyanic acid. The peeling may be manual or mechanical, for example using a cylindrical or screw-shaped peeler. However, the need for washing after the peeling process is highlighted. The term “grinding” should be understood as the process responsible for breaking down root cells, releasing starch granules and allowing flour homogenization. Preferably, the milling should be carried out in a cylinder provided with a central axis with saws. The term "pressing" should be understood as the process that aims to reduce the moisture present in the crushed mass in order to prevent the emergence of undesirable fermentations, save time and fuel in roasting, enabling roasting without excessive lump formation. Pressing should occur shortly after grinding. The term “Decantation” should be understood as the process of collecting the liquid extracted from the manipueira pressing, and its subsequent rest time for one or two days for starch sedimentation. The term “manipueira fermentation” should be understood as the natural fermentation during one or two days, which occurs during the decantation period. The term "addition of seasonings" shall be understood as a group of seasonings, such as salt, garlic, pepper, parsley and coriander, to be added during tucupi boiling over a period of approximately fifteen minutes at temperatures above about 90 ° C. . The term "Storage" should be understood as the process in which tucupi, after boiling and still hot, is packaged at room temperature, preferably 24 ° C to 28 ° C in polyethylene containers, among other materials, suitable for food storage. . The term “spray drying”, as well as its synonyms: nebulization and spray drying, should be understood as the continuous process, where a liquid or paste is transformed into a dry product, in the form of a powder, characterized for a while. relatively short drying time. More specifically, the process should be understood as a process in which liquid atomization occurs in a compartment that receives a hot air flow, so that rapid evaporation of water allows the temperature of the particles to be kept low, allowing the drying of sensitive products. heat without affecting too much its quality, being carried out in four stages: the atomization of the liquid material, the liquid-air contact, the drying of the sprayed liquid and the separation of the dried product with the hot air. The term “Microencapsulation” should be understood as a technique that entails trapping an active agent, such as: small solid particles, liquid droplets or gaseous compounds, in a protective shell, such as: thin films or polymeric coatings, to be released on a given condition. The active agent may also be called a filler material, active material or internal phase, while the shell material may also be called a wall, carrier, membrane or shell material.

It is further understood that said process is used for the purpose of reducing the reactivity of the product with the external environment, reducing the evaporation or the transfer rate of the material to the environment, obtaining the atomized product a more uniform and solid form. Easy mixing. The term "Wall Material" should be understood as the material that will be used to coat the Stuffing Material with the function of providing protection from light, moisture and contact with other substances during storage, preventing loss of encapsulated volatile compounds, obtaining an easy-to-handle end product that can be incorporated into dry foods. Examples of wall materials are Carbohydrates such as: Starch, maltodextrins, corn syrup, dextran, sucrose, cyclodextrin, carboxymethylcellulose, methyl and ethyl cellulose, acetyl cellulose and nitrocellulose; Celluloses: Gums, arabic gum, agar, sodium alginate and carrageenan; Lipids, such as: Wax, paraffin, trystearine, stearic acid, mono- and diglycerides, greases and oils; and Proteins such as Gluten, Casein, Gelatin, Albumin, Hemoglobin and Peptides. The term "Maltodextrins" is to be understood as starch hydrolysates consisting of αD-glucose units joined primarily by glycosidic bonds and having a general formula equal to [(C6H105) nH20] where the equivalent number of dextrose (ED) is less than 20 (DE <20) (KENNEDY, JF; KNILL, CJ; TAYLOR, DW Maltodextrins.

In: KEARSLEY, M.W .; DZIEDZIC, S.Z. Handbook of Starch Hydrolysis Products and their Derivatives. London, Blackie Academic & Professional, 1995, p.65-82). The term “Parameters for tucupi atomization” should be understood as the set of parameters considered most important for the process of tucupi atomization, which is formed by the parameters: inlet air temperature, outlet air temperature and percentage of soluble solids. The term “Inlet air temperature” should be understood as the temperature of the air entering the atomizing equipment and is related to the drying process and possible product degradation. It is desirable that the inlet temperature be as high as possible to promote rapid formation of the semipermeable membrane on the surface of the droplet, provided that no vapor bubbles are formed, which temperature is preferably from 140 ° C to 210 ° C, preferably 170 ° C. ° C. The term “Outlet air temperature” should be understood as the temperature of the air leaving the atomizing equipment and related to the final moisture of the product. It is desirable that the outlet temperature does not change the aroma of the product, preferably at temperatures of 80 ° C to 90 ° C. The term “percentage of soluble solids” should be understood as the ratio between solution before and after drying given as a percentage. This parameter is related to the proper functioning of the equipment. Since the high amount of soluble solids can cause the atomizer cylinder openings to clog, interrupting the process, but otherwise the solution may not dry out as the particles will still be larger and the hot air may not be enough to completely dry the product, resulting in a product with higher than ideal moisture. Preferably the percentage range of total solids of the present invention ranges from 4% to 11%, preferably 7.5%. The term “Characterization of powdered food” should be understood as the process that is used to determine the microstructure of tucupi microparticles, using the Scanning Electron Microscopy (SEM) technique, thus determining its properties. The term “Scanning Electron Microscopy - SEM” should be understood as the technique in which an electron beam is generated from heating a tungsten filament and focused through electromagnetic lenses towards a particular sample thus forming a image with high resolution power that can finally be captured, being used to analyze the microstructure of the tucupi powder product, evaluating the physical characteristics of the product. Tucupi can be obtained in several ways. Preferably, by the following steps: 1) Cassava harvesting; 2) washing; 3) Peeling; 4) crushing; 5) pressing; 6) Starch decantation and fermentation; 7) Optionally, addition of condiments; and 8) Boil. Subsequently, the product may be packed for storage.

Cassava roots can be harvested from 16 to 20 months, from April to August, when they have the maximum yield. The process should take place immediately after harvest or within a maximum of 36 hours to avoid loss, darkening, which would result in a lower quality product, as soon after the fermentation process begins the roots. Friction and mechanical damage to the roots should be avoided, which would cause fermentation to begin, resulting in a lower quality product.

The roots should be washed to remove soil adhering to their bark and to avoid the presence of impurities that impair the quality of the final product. Peeling eliminates the fibers present in the husks, the flour-darkening tannins, and the portion of hydrocyanic acid that is most concentrated in the husks. The peeling can be manual, made with sharp knives or scraper, or mechanical, using the cylindrical peeler or screw form.

After manual stripping, the roots should be washed again to remove any impurities adhered to them during the process.

In the mechanical debarker, washing and debarking are carried out at the same time by rubbing the roots with each other and with the walls of the equipment, with continuous flow of water. Proper washing and peeling results in higher quality products. Grinding is done so that the root cells are broken, releasing the starch granules and allowing flour homogenization. Milling is usually done in a cylinder with a central shaft with saw blades. Cylinder saws should not have bent, missing, worn or rusty teeth as this interferes with the final product. Pressing should take place immediately after grinding to prevent flour fermentation and browning. It is made in tipitis, hand screw presses or hydraulic presses and aims to reduce, as little as possible, the moisture present in the crushed mass, in order to prevent the emergence of undesirable fermentations, save time and fuel in roasting, enabling a seamless roasting. excessive lump formation. The water resulting from pressing grated cassava is called “manipueira”, it is very toxic and polluting.

After collecting the manipueira, it is resting for one or two days to decant the starch that is later removed, naturally occurring its fermentation. Condiments are added during the boiling of tucupi, which takes about fifteen minutes at temperatures above 90 ° C to decrease the concentration of cyanide present in the product. After boiling, tucupi is normally packaged, still warm, in PET or similar bottles and stored at room temperature (about 28 ° C).

Thus, the present invention is characterized by a method of obtaining the microencapsulated tucupi powder, characterized by the steps of: 1) obtaining the tucupi; 2) use of an encapsulating agent as a wall material; 3) homogenization; 4) drying, which results in obtaining the microencapsulated tucupi; and optionally 5) wrapping and storage. The invention is further characterized by the pencro-encapsulated tucupi.

The following illustrative examples will serve to further describe the present invention. However, the data and procedures illustrated merely refer to some embodiments of the present invention and should not be construed as limiting the scope thereof.

Example 1 - Tucupi Sample A tucupi sample was collected, still in the conventional manufacturing process, with the boiling step remaining, from a manufacturer of the 25 de Setembro Fair in the municipality of Belém, Pará state, Brazil. heat treated for 15 minutes at 100 ° C. The sample was then stored in 2 liter polyethylene (PET) plastic bottles, still hot. The material was transported to Embrapa Eastern Amazon Agro - Industry Laboratory, Belém - PA, and frozen at - 20 ° C until analysis and preparation for atomization.

Example 2 - Wall Material Maltodextrin - DE 1910, supplied by the company Com Products Brasil - Ingredientes Industriais Ltda. to the specifications described in Table 1.

Example 3 - Allomization A NIRO ATOMIZER Spray-dryer, model AS0340 with evaporation capacity between 80Kg and 85Kg of water / h was used to prepare the material.

Example 4 - Physicochemical analysis of liquid tucupi pH determination

Obtained directly with the aid of pH meter according to AO AC method 42.1.04 (1984) at 25 ° C (A. O. A.C. 1984. Officials methods of Analysis. Association of official Analytical chemists. Washington. D.C., USA).

Determination of moisture Obtained by prior evaporation of the sample in a water bath, followed by oven drying at 105 ° C according to AOAC Method 31.1.02 (AOAC 1984. Officials methods of Analysis. Analytical chemists, Washington, DC, USA).

Determination of ash content Obtained by prior evaporation of the sample in a water bath followed by incineration in a muffle furnace at 560 ° C according to AOAC method 31.1.04 (1984). (A.O. A.C. 1984.

Officials methods of Analysis. Assoiciation of official Analytical chemists. Washington. D.C., USA) Determination of total titratable acidity Determined by titration with sodium hydroxide according to AOAC Method 945.15 (1984). (AOAC 1984. Officials methods of Analysis. Assoiciation of official Analytical chemists. Washington. DC, USA) Determination of protein content Determined by the micro Kjeldahl technique, based on hydrolysis and subsequent distillation of the sample with conversion factor of 6.25 to according to AOAC Method 31.1.08 (1984). (A.O. A.C. 1984. Officials methods of Analysis. Association of official Analytical chemists.

Washington. D.C., USA) Determination of soluble solids content Determined according to AOAC Method 37.1.15 (1984). (A.O. A.C. 1984. Officials methods of Analysis. Assoiciation of official Analytical chemists. Washington. D.C., USA) Determination of total solids Determined by moisture subtraction (%) in 100% of the sample.

Brix / Acidity Ratio Obtained by dividing the total soluble solids content (° Brix) by the total titratable acidity value (%).

Total cyanide quantification Determined by the enzymatic method (lyenase enzyme extracted from cassava roots), the methodology being described by Cooke (COOKE, RD "An enzymes assay for the Cyanide content of Cassava - Manihot Esculenta Crantz". J. Sci. Food Agri ., 29, 345-352, 1978) and subsequently adapted by Essers (ESSERS, AJA; BOSVELD, Margaret; GREFT, Remco M. van der; VORAGEN, Alfons GJ Assay for the cyanogens content in cassava Products. Preliminary Version, December 9f Department of Food Science, Wageningen.

Agricultural University, Netherlands, 1993) in which cyanide (CN) is oxidized to cyanogen halide claramine T or N-chlorosuccinimide. This compound reacts with isonicotinic acid to produce a dialdehyde that couples with amines or compounds with the methylene group as dimethylbarbituric acid to form a colored complex and further read on a spectrophotometer at 605 nm.

Determination of total and reducing sugars Determined by the Lane-Eynon technique (IAL - ADOLFO LUTZ INSTITUTE. Analytical Standards of Instituto dolfo Lutz .v. 1: Chemical and Physical Methods for Food Analysis. 4th ed. São Paulo: IMESP, 2004) .

Determination of the amount of total starch by acid hydrolysis According to CEREDA (CEREDA, P. P .; DAIUTO, E. R .; VILPOUX, O.

Methodology of starch determination in acid microwave digestion. ABAM - BRAZILIAN ASSOCIATION OF CASSAVA STARCH PRODUCERS. YEAR II - N ° 8 - September - December / 2004). After that, the volume is completed in a 250 mL volumetric flask and titered by Lane-Eynon sugars (IAL, 2004).

Determination of Total Carotenoids It was performed according to the methodology described by GODOY and RODRIGUEZAMAYA (GODOY, Η. T .; RODR1GUEZ-AMAYA, DB. Carotenoid composition in nectarine - Brazilian Persian Prunus. Rev. Inst. Adolfo Lutz, 57: 73-79, 1998 ).

Absolute Density The absolute density (D) of the samples was determined at 25 ° C on an AccuPyc 1330 Automatic Gas Pycnometer (Helium Gas, Norcross, USA).

The results of the physicochemical characterization can be seen in Table 2.

Table 2 - Physical and chemical characterization of tucupi (liquid). There is no legislation for tucupi and the published literature is inexpressive, so the results were compared to the author Chisté (Chisté, Renan Campos, Cohen, Kelly Oliveira and Oliveira, Suzy Sarzi. Study of the physicochemical properties of tucupi. Ciênc.

Tech Aliment., Sep 2007, vol.27, no.3, p.437-440) who analyzed several tucupi samples randomly chosen at free markets in the Belém-PA market.

The results are satisfactory when compared to the values found by Chisté (Chisté, Renan Campos, Cohen, Kelly de Oliveira and Oliveira, Suzy Sarzi. Study of the physicochemical properties of tucupi. Ciênc. Tecnol. Aliment., Sep 2007, vol.27 , no.3, p.437-440). However, for protein and total cyanide results, highlighted in bold, the values are not within the range found by the author. According to Chisté (CHISTÉ, R. C .; COHEN, K. O .; OLIVEIRA, S. S. Study of the physicochemical properties of tucupi.

Available at: <http: //www.scielò.br/scielo.php? Pid = S0101- 20612007000300002 & script = sci_arttext & tlng = g>. Accessed: August 01, 2009), there are significant variations between the physicochemical characteristics of the samples under study, proving the lack of product standardization. In fact, the tucupi manufacturing process varies from producer to producer, as does the variety of cassava used in the manipueira extraction process. This also explains the protein value of the raw material that is not within the range found by Chisté (CHISTÉ, RC; COHEN, KO; OLIVEIRA, SS. Study of the physicochemical properties of tucupi. Available at: <http: // www. scielo.br/scielo.t>hp?pid=S0101- 20612007000300002 & script = sci_arttext & tlng = g>.

Accessed: August 01, 2009).

We also found the ° Brix / acidity ratio of 0.82, total and reducing sugars, with 1.06% and 1.03%, respectively and soluble solids, the value found was 3.75 ° Brix.

For the starch content, a value of 1.1% was obtained. Total carotenoids had a value of 24.55 pg / 100g. Lipids had a value of 0.4%.

Example 5 - Experimental Design In order to establish the best process conditions, a central rotational composite design (DCCR) was performed in which the influence of the factors inlet air temperature and tucupi total solids concentration were studied. The values established were based on the stipulated factors. by Taxi (TAXI, C. AD. AD Microencapsulated Camu-Camu (Myrciaria dubia) juice obtained by spray drying. Thesis (Doctorate in Food Technology) - School of Food Engineering, State University of Campinas. Campinas, 2001 .). The processing aimed to optimize the drying conditions of tucupi to obtain lower total cyanide content, color parameter index b * (associated with the blue-yellow dimension) with a tendency to yellow scale and lower water activity (Aw).

Thus, each factor was studied at 5 different levels (KHURI A.J.; CORNELL F.A. Response surfaces: design and analysis. New York: Mercei Dekker. 510p, 1996) as shown in Table 2.

Table 3 - Definitions of the levels of the two variables studied in the atomization process of the maltodextrin microencapsulated tucupi. Planning requires the execution of a minimum number of experiments. In the optimization of the microencapsulated tucupi atomization process, 11 tests were performed (Table 4), being 4 factorials (combination between ± 1 levels), three central (two variables at level 0) and four axial (one variable at level ± ae two at level 0) generating a quadratic model, where the value of the dependent variables (hydrocyanic acid content, L, a *, b and Aw) is a function of the independent variables (inlet air temperature and tucupi soluble solids concentration), Table 4 - Experimental Design 22 coded matrix for "optimizing the microencapsulated tucupi atomization process.

Table 5 shows the values of total cyanide content, color parameters (L, a *, b *) and water activity (Aw) obtained experimentally from the physicochemical analyzes of the microencapsulated tucupi, following the worksheet. experimental planning.

Table 5 - Total cyanide responses, color parameters (L *, a *, b *) and Water Activity (Aw).

Example 6 - Processing for obtaining the microencapsulated tucupi Figure I illustrates the flowchart of the processing steps for obtaining the microencapsulated tucupi dry extract.

Following the above flow, maltodextrin was added to the tucupi and it was homogenized to enter the drying process. The tucupi atomization system in the drying chamber was made with a 1mm nozzle tip and 4Kgf / cm2 air pressure (this air pressure provides nozzle rotations from 30,000 rpm to 32,500 rpm). The microencapsulated tucupi samples were placed in glass jars, covered with aluminum foil in order to avoid contact of the material with light.

After packaging, the material was stored in a desiccator to avoid moisture retention of the product.

The results of cyanide content (mg / kg), water activity and color parameter b * were analyzed by the response surface methodology using the STATISTICA 5.0 program. Example 7 - Determination of the cyanide Determined by the enzymatic method (enzyme denosis extracted from cassava roots), the methodology being described by Cooke (COOKE, RD “An Enzyme Assay for the Cyanide Content of Cassava (Manihot Esculenta Crantz).” J. Sci. Food Agri., 29, 345-352, 1978 ) and subsequently adapted by Essers et al. (ESSERS, A. J. A.; BOSVELD, Margaret; GRIFT, Remco M. van der; VORAGEN, Alfons G. J. Assay for cyanogens content in cassava products. (Preliminary) Version, December, 1993). 9f. Department of Food Science, Wageningen. Agricultural University, Netherlands, 1993), in which cyanide (CN-) is oxidized to cyanogen halide claramine T or N-chlorosuccinimide. This compound reacts with isonicotinic acid to produce a dialdehyde that couples with amines or compounds with the methylene group as dimethylbarbituric acid to form a colored complex and further read on a spectrophotometer at 605 nm.

Total Cyanide The result of the statistical analysis, applied to the experimental data of total cyanide loss (mg / kg) present in microencapsulated tucupi is presented in Tables 6 and 7. These values were determined by residual SS and pure error. The effects of factors in bold are significant at the 95% confidence level (p <0.05).

Table 6 - Estimated effect, residual error, t-coefficient and statistical significance at each factor in the coded model for microencapsulated tucupi for cyanide. (L): Linear, (Q): Quadratic Table 7 - Estimated effect, pure error, t-coefficient, and statistical significance at each factor in the coded model for microencapsulated tucupi for cyanide. (L): Linear, (Q): Quadratic The estimated effect indicates how much each factor influences the responses analyzed, in this case, the total cyanide loss. The higher its value, the greater its influence, and a positive effect indicates that by going from a minimum to a maximum of the variable, the response increases. On the other hand, a negative effect indicates the opposite, that is, from a minimum value to a maximum value, the response decreases (BOX, GEP; WETZ, J. Criteria for judging adequacy of estimation by an approximate response function. University of Wisconsin Technical Report, no. 9, 1973).

The linear temperature parameter has a negative effect on the response, so an increase in temperature leads to a decrease in cyanide content. Quadratic temperature,% Total Solids (linear and quadratic) and the interaction of maltodextrin with temperature were not significant, showing that any change in their values does not interfere with the total cyanide content.

As described in the scientific literature, this author mentions that when tucupi is subjected to high temperatures, there is a more intense hydrolysis of cyanic compounds and consequent cyanide volatilization to the environment (Chisté 2007).

Also according to literature reports, t value indicates how large the variable is in relation to its deviation. Thus, the higher the t value, the greater the probability that the variable will be statistically significant (Box and Wetz (1973). The value of the p coefficient is at the level of significance of the independent variable on the response under study. confidence the value of 95%.

Thus, it can be stated that for p values below 5%, the variable is considered statistically significant. Otherwise, it is not considered significant (Box and Wetz (1973).

As can be seen in Tables 6 and 7 the significant factors were the same for pure error as for residual SS. The significant factor, highlighted in bold at 95% confidence, considering pure error, is linear temperature. For residual SS, the linear temperature is significant at 93% and it is therefore not justified to remove them from the model.

After eliminating the parameters with no significant effects, the analysis of variance (ANOVA) revealed the significance of regression and lack of adjustment with 95% confidence (p <0.05) using the F test for studied planning, according to Table 8.

Table 8 - Analysis of variance (ANOVA) of the model adjusted for the total cyanide content in the microencapsulated tucupi. SQ: Quadratic sum, GL: Degree of freedom, MQ: Quadratic average.

A regression, although significant from the point of view of the F test, may not be useful for making predictions because it covers a small range of factors studied. (BARROS NETO, B .; SCARMINIO, I.S .; BRUNS, R.E. How to do research and development experiments in science and industry. Campinas: UNICAMP Editor, 2001). For a regression to be not only statistically significant but also useful for predictive purposes, the F value calculated for the regression must be at least four to five times greater than the tabulated F value. On the other hand, the F of lack of adjustment in relation to pure error, on the contrary, should present the lowest possible value, since a high F indicates that there is a great lack of adjustment of the data to the obtained model (Box and Wetz 1973).

Analyzing the values obtained in Table 8, it is observed that the model presented significant but not predictive regression (Box and Wetz 1973), because the lack of adjustment was not significant, F calculated lower than the tabulated F. For this reason, the proposed model serves only as a trend graph for future work. The coefficient of determination (R2) obtained was 0.42, indicating that the model explained 42% of the variation of the experimental data. The coded model proposed to represent total cyanide loss in microencapsulated tucupi is the following equation: Cyanide (mg / kg sample) = 7.66-1.66T

Where: T = Temperature (° C).

For a better visualization of the model fit, the cyanide content values predicted by the model were calculated and compared with the experimental values, obtaining the relative deviations between them, as shown in Table 9.

Table 9 - Experimental values and predicted values by the coded model for the Total Cyanide (CT) content response in microencapsulated tucupi.

According to Table 9, it is found that standard deviations ranged from (0.0963 to 1.4365). Tests 1, 3, 5 and 10 are those with high deviations, which justifies a possible lack of adjustment. As total cyanide values are important for the study, it would be ideal to perform new experiments by shifting the intervals of this variable so that the highest CT values would no longer be at the extremes of the surface (Experiments 1 and 3).

However, the temperatures used in the tests that presented the largest deviations are already considered high for this type of biological material, so it is not convenient to increase them even more. Experiments 5 and 10 were found at the central point of the surface, the ideal would be to repeat the cyanide quantification, but the same was not done due to the absence of reagents for this analysis. Figure 2 (Annex 1) shows the response surface and contour generated by the proposed model. The surface shows that with increasing temperature there is a loss of total cyanide content and is independent of% Total Solids.

Example 8 - Color Parameters The instrumental color was determined by tristimulus colorimetry using a MINOLTA model CR 400 colorimeter. L *, a * and b * values were determined following parameters D65 (daylight) and 10 ° (observer angle), using CIE Lab patterns, where the L * coordinate corresponds to the luminosity, and a * and b * refer to the green (-) / red (+) and blue (-) / yellow (+) coordinates. ) respectively.

Parameter L * (Luminosity) The result of the statistical analysis, applied to the experimental data of the luminance variation in the microencapsulated tucupi as a function of temperature and total solids concentration, is presented in Tables 10 and 11. These values were determined through the residual SS. and pure error. The effects of factors in bold are significant at the 95% confidence level (p <0.05).

Table 10 - Estimated effect, residual error, t coefficient and statistical significance at each factor in the color coded microencapsulated tucupi model, parameter L *. (L): Linear, (Q): Quadratic.

Table 11 - Estimated effect, pure error, t coefficient and statistical significance, for each factor in the color coded microencapsulated tucupi model, parameter L *. (L): Linear, (Q): Quadratic It can be seen from tables 10 and 11 that the significant factors are the same for residual error and pure error. It is also verified that the parameters Quadratic Total Solids have negative effect meaning that the curvature of the graph should be down in relation to the response. The temperature (linear and quadratic) regarding the interaction of maltodextrin with temperature were not significant, showing that any change in its values does not affect the color parameter L *.

After eliminating the parameters with no significant effects, the analysis of variance (ANOVA) revealed the significance of regression and lack of adjustment with 95% confidence (p <0.05) using the F test for studied planning, according to Table 12.

Table 12 - ANOVA for the color parameter L * (brightness). SQ: Quadratic sum, GL: Degree of freedom, MQ: Quadratic average.

Table 12 shows that the adjusted model is significant and predictive, since the calculated regression F is 9.70 times higher than the tabulated F; the calculated F of misadjustment is much smaller than the tabulated F, meaning that there was no major misadjustment of the data. The coded model proposed to represent the maltodextrin-related color variation L (linear and quadratic) is the following equation. L = 82.04 + 8.77ST-5.33ST2 Where: T: Temperature (° C); and ST:% Total Solids (%). The coefficient of determination (R2) was 0.87, indicating that the model explained 87% of the observed data variation. Figure 3 (Annex 2) shows the response surface and level curve, generated by the proposed model, considering the average points of maltodextrin and temperature. This surface confirms the analysis of the effects performed previously and allows to visualize the variation of the response for each studied parameter.

The brightness, ranging from white to black, is found to be independent of temperature.

For total solids there is a higher brightness from 7.5% of total solids up to 10%.

Parameter a * (green to red) The result of the statistical analysis, applied to the experimental data of the variation of parameter a * in the microencapsulated tucupi as a function of temperature and total solids concentration, is presented in Tables 13 and 14. These values were determined. through residual SS and pure error. The effects of factors in bold are significant at the 95% confidence level (p <0.05).

Table 13 - Estimated effect, residual error, t-coefficient and statistical significance at each factor in the coded model for microencapsulated tucupi for color, parameter a *. (L): Linear, (Q): Quadratic.

Table 14 - Estimated effect, pure error, t-coefficient and statistical significance, for each factor in the color coded microencapsulated tucupi model, parameter a *. (L): Linear, (Q): Quadratic.

As can be seen in Tables 13 and 14 the significant factors were the same for pure error as for residual SS. The significant factor highlighted in bold at 95% confidence, considering pure error, is% Linear Total Solids and quadratic maltodextrin and the interaction between% Total Solids x temperature. For residual SS,% Linear and quadratic Total Solids have values above 95% confidence, the interaction between% Total Solids x temperature is significant at 91% and it is therefore not justified to remove it from the model.

It is also verified that the parameters,% Quadratic Total Solids and the interaction% Total Solids x temperature, have positive effect in relation to the response, that is, an increase of these parameters causes an increase of the parameter a *. A% Linear Total Solids has a negative effect, so the lower the added maltodextrin concentration, the a * parameter increases. The temperature, linear and quadratic, was not significant, showing that any change in their values does not affect the color parameter a *. t After the elimination of parameters with no significant effects, the analysis of variance (ANOVA) revealed the significance of regression and lack of adjustment with 95% confidence (p <0.05) using the F test for the studied planning, according to Table 15.

Table 15 - ANOVA for color parameter a *. SQ: Quadratic sum, GL: Degree of freedom, MQ: Quadratic average.

Table 15 shows that the adjusted model is significant and predictive, since the calculated regression F is 8.28 times higher than the tabulated F; the calculated F of misadjustment is much smaller than the tabulated F, meaning that there was no major misadjustment of the data. R2 of 0.93 indicates good model reproducibility. The coded model proposed to represent the variation of a * parameter related to% Total Solids (linear and quadratic) and the% Total Solids x temperature interaction is in the following equation. a * = 0.52-3.18M + 1.88 (ST) 2 + 0.99T (ST) Where: T: Temperature (° C); and ST:% Total Solids (%). Analysis of variance showed that the model adjusted for the a * parameter was significant with 95% confidence. The coefficient of determination (R2) was 0.93, indicating that the model explained 93% of the observed data variation. Figure 4 (Annex 3) presents the response surface and level curve, generated by the proposed model, considering the mean points of maltodextrin and temperature. This surface confirms the analysis of the effects performed previously and allows to visualize the variation of the response for each studied parameter.

It can be seen from the graph in Figure 4 (Annex 3) that the parameter a *, which varies from lowest (green) to highest (red) intensity, the intensity of a * optimal is the region with the highest% total solids, between 9, 5% and 11%, and lower temperature, ranging from 140 ° C and 145 ° C, from this value the temperature will lose importance in this parameter. The low maltodextrin content and low temperatures show that the material did not have an efficient encapsulation, so the starch present in the material may have undergone a gelling process. In the experiment, it was observed that at the end the product looked like a caramel, concluding that the product gelled, this gel with high humidity together with the incidence of temperature caused the caramelization of the final product.

Parameter b * (blue to yellow) The result of the statistical analysis, applied to experimental data of the variation of parameter b * in the microencapsulated tucupi as a function of temperature and total solids concentration, is presented in Tables 16 and 17. through residual SS and pure error. The effects of factors in bold are significant at the 95% confidence level (p <0.05).

Table 16 - Estimated effect, residual error, t-coefficient and statistical significance, for each factor in the coded model for microencapsulated tucupi for color, parameter b *. (L): Linear, (Q): Quadratic.

Table 17 - Estimated effect, pure error, t-coefficient and statistical significance at each factor in the color coded microencapsulated tucupi model, parameter b *. (L): Linear, (Q): Quadratic.

As can be seen in Tables 16 and 17 the significant factors were the same for pure error as for residual SS. The significant 95% confidence factor, considering pure error and residual SS, are% Linear Total Solids, Quadratic Total Solids%, highlighted in bold.

It is also verified that the parameter,% Quadratic Total Solids has a negative effect on the response, that is, there is a maximum value located at the top of the studied surface. The temperature (linear and quadratic) and the interaction% Total Solids x temperature were not significant, demonstrating that any change between the studied values does not interfere with parameter b *.

After eliminating the parameters with no significant effects, the analysis of variance (ANOVA) revealed the significance of regression and lack of adjustment with 95% confidence (p <0.05) using the F test for studied planning, according to Table 18.

Table 18 - ANOVA for color parameter b *. SQ: Quadratic sum, GL: Degree of freedom, MQ: Quadratic average.

Table 18 shows that the adjusted model is significant and predictive, since the calculated regression F is 4.25 times higher than the tabulated F; the calculated F of misadjustment is much smaller than the tabulated F, meaning that there was no major misadjustment of the data. The coded model proposed to represent the b * parameter variation related to the% total solids (linear and quadratic) is represented in the following equation. b * = 31.9 + 6.52ST - 8.46ST2 Where: ST:% Total Solids (%). Analysis of variance showed that the model adjusted for the b * parameter was significant with 95% confidence. The coefficient of determination (R2) was 0.89, indicating that the model explained 89% of the observed data variation. Figure 5 (Annex 4) shows the response surface and contour curve generated by the proposed model, considering the maltodextrin and temperature midpoints. This surface confirms the analysis of the effects performed previously and allows to visualize the variation of the response for each studied parameter.

Figure 5 (Annex 4) shows that the region where parameter b * had its highest intensity is in the central region, where the amount of total solids is 7.5% of the graph. In the related scientific literature, the work with optimized acai (Tonon 2009) found that powders produced with higher maltodextrin concentrations had lower intensity in b *, which was predictable, since the increase in maltodextrin content causes a “dilution”. pigmentation of the product, but for encapsulated tucupi this statement has limitations, because the carrier at high temperatures undergoes caramelization and at low concentrations of maltodextrin, the process demonstrates inefficient encapsulation, causing the gelation process and then caramelization. The intensity of the color parameter b * tending to yellow is important for the product, as the yellow color is a sensory factor for the encapsulated tucupi and is related to the amount of pigments kept in the product. The greater the amount of carotenoid pigments, the higher the quality of the product in terms of sensory and nutritional terms.

Example 9 - Water Activity (Aw) Obtained by direct reading at 20 ° C on the Aqualab model CX-2Aw water activity meter. The result of the statistical analysis, applied to the experimental data of the variation of the Aw parameter in the microencapsulated tucupi as a function of temperature and total solids concentration, is presented in Tables 19 and 20. These values were determined by residual SS and pure error. The effects of factors in bold are significant at the 95% confidence level (p <0.05).

Table 19 - Estimated effect, residual error, t-coefficient and statistical significance for each factor in the color coded model for microencapsulated tucupi, Aw * parameter. (L): Linear, (Q): Quadratic.

Table 20 - Estimated effect, pure error, t-coefficient and statistical significance, for each factor in the coded model for microencapsulated tucupi for color, Aw * parameter. (L): Linear, (Q): Quadratic.

As can be seen in Tables 19 and 20, the significant factors for Pure Error are quadratic temperature,% Linear and quadratic Total Solids, highlighted in bold.

In addition to the factors found for pure error, SS Residual also presented significant results for linear temperature.

It is verified that the region of curvature will be where will be the region of least water activity. Linear temperature and% Solids x temperature interaction were not significant.

After eliminating the parameters with no significant effects, the analysis of variance (ANOVA) revealed the significance of regression and lack of adjustment with 95% confidence (p <0.05) using the F test for studied planning, according to Table 21.

Table 21 - ANOVA for Aw * color parameter. SQ: Quadratic sum, GL: Degree of freedom, MQ: Quadratic average.

Table 21 shows that the adjusted model is significant and predictive, since the calculated regression F is 10 times higher than the tabulated F; the calculated F of misadjustment is much smaller than the tabulated F, meaning that there was no major misadjustment of the data. The coded model proposed to represent the variation of Aw parameter related to linear temperature and% Linear and quadratic Total Solids is in the following equation.

Aw = 0.23 + 0.10T2 - 0.04ST + 0.04ST2 Where: T: Temperature (° C); and ST:% Total Solids (%). Analysis of variance showed that the model adjusted for the Aw parameter was significant with 95% confidence. The coefficient of determination (R2) was 0.89, indicating that the model explained 89% of the observed data variation. Figure 6 (Annex 5) presents the response surface and level curve, generated by the proposed model, considering the mean points of% Total Solids and temperature. This surface confirms the analysis of the effects performed previously and allows to visualize the variation of the response for each studied parameter.

Both total solids concentration and temperature were determinant in Aw.

According to Taxi (2001) who worked with camu-camu powder, there is an optimal concentration of total solids in which the retention of compounds is higher, because when working with concentrations above the optimum, there may be a decrease in encapsulant solubility and, therefore, its film-forming ability on the filling material would be diminished and thus the retention of the compounds would be reduced. The air inlet temperature of the drying air is fundamental for the decrease of water present in the product, its relation with the concentration of encapsulants is fundamental to be able to reach the desired point, because very high temperatures can cause the caramelization process of the carrier agent.

By crossing the regions with the lowest water activity and the highest value of the color parameter b * it was found that the central point is the optimal point region. Its total solids percentage is 7.5% and the temperature is 170 ° C.

Example 10 - Particle Analysis Annexes 7, 8, 9 and 10 present photos of the experiments of the present invention.

Morphology For SEM analysis, two samples taken from the design (one from minimum point F1 and one from maximum point F8) were dehydrated in an oven with forced air circulation at 105 ° C, and were adhered to stubs through of double-sided and gold-plated carbon layer tape approximately 20nm thick for 150 seconds at 25 mA current. Electron micrographs were obtained using a Leo Model 1450 VP Scanning Electron Microscope at an electron acceleration (EHT) of 15 KV, working distance (WD) ranging from 11-20 mm and using a secondary electron detector (SEI). The micrometer scales were projected under the same optical conditions. The objective was to verify the efficiency of the process, that is, due to the microencapsulation of maltodextrin in the tucupi solids according to the variations determined in the planning. Morphology analysis was performed for particles produced with different maltodextrin concentrations and under different drying air inlet temperatures.

The images presented in Figure 7 correspond to the particles produced with 10% total solids concentration and pressure of 4 kg / cm2, using different drying air inlet temperatures.

The images shown in Figure 8 correspond to the particles produced with 7.5% concentration of total solids and pressure of 4 kg / cm2, using different drying air inlet temperatures. The image shown in Figure 9 corresponds to the initial particles, with a concentration of 5% total solids and a pressure of 4 kg / cm2, using different drying air inlet temperatures.

According to micrographs 1, 2 and 3 the particles presented spherical shape, which is characteristic of powders produced by the spray drying process. The particle surfaces were predominantly rough, although some had a completely smooth surface, and it was observed that the higher the temperature, the particles are less rough.

Similar results were obtained by Righetto (RIGHETTO, AM Physicochemical characterization and stability of microencapsulated green acerola juice by atomization and lyophilization. Thesis (Doctorate in Nutrition Science) - Faculty of Food Engineering, Campinas State University. Campinas, 2003 Available at: <http://bibl Biblioteca.universia.net/ficha.do?id=3901733> Accessed: August 1, 2009. 176 pr), for merooencapsulated acerola juice with 20DE maltodextrin and gum, as also with Tonon (ΤΟΝΟΝ, RV Acai juice spray drying: Influence of process variables, product quality and stability. 242f. Thesis (PhD in Food Engineering) - School of Food Engineering, State University of Campinas. Campinas , 2009), for aeroi encapsulated acai juice with maltodextrin IODE, 20DE and 3 ODE. The literature reports similar results (Alamilla-Beltrán et al. (ALAMILLA-BELTRÁN, L., CHANONA-PÉREZ, JJ; JIMÉNEZ-APARICIO, AR; GUTIÉRREZ-LÓPEZ, GF Description of morphological changes of particles and spray drying. Journal of Food Engineering, v.67, n.1-2, pp. 179-184, 2005), in studies studying the morphological alterations of maltodextrin particles produced under different drying temperatures, in spray dryer. Differences in the morphology of the powders obtained under the different drying conditions may be due to differences in the drying rate, higher temperatures correspond to higher drying rates, and the physical characteristics of the shell, which may be more “flexible” in the case of the particles produced. at lower or medium temperatures, or more rigid, for particles produced at higher temperatures Experiment III, with 5% total solids and 150 ° C r and experiment XI, with 7.5% total solids and 140 ° C inlet air temperature, were not read because the image is generated by the interaction of the electron beam and matter. Then, samples that contain moisture when interacting with the electron beam will generate vapors, and these will generate oxidation of fundamental components such as the filament, which makes the electron beam emitted, and the column containing the electromagnetic lenses that make the electron beam. electron capture that forms the image.

On the other hand, before being placed in the apparatus, the sample has to be covered with a thin layer of gold, and liquid, frozen samples, such as sample III and XI, and with a high degree of humidity, this cover does not keep on the surface and decant in the sample.

In a study carried out in 2006 (NIJDAM, JJ; LANGRISH, TAJ The effect of surface composition on the functional properties of milk powders. Journal of Food Engineering, v.77, n.4, p.919-925, 2006) was also observed. the formation of stiffer particles when used at higher temperatures in the production of spray dryer milk powder particles. According to the authors of the paper, when the temperature is sufficiently high, the moisture evaporates quickly and the shell becomes dry and hard, so that the particles do not wilt when the vapor formed inside the vacuole condenses at the moment when they evaporate. move to the cooler regions of the dryer. However, when the drying temperature is lower, the shell remains moist and flexible longer, so that the particles may become wilted and wrinkled when cooled.

The depressions that appear on surfaces are formed due to particle contraction during drying and cooling (Thies, 2001). In addition, the extent of depressions observed in spray drying particles is a function of the nature of the carrier agent used and is significant in those with polysaccharide coverage. Hollow particle formation is also a common feature in particles produced by spray drying. The formation of this void within the particle is related to its expansion during the final stages of the drying process (RE, M.I.

Microencapsulation by spray drying. Diying Technology, v.16, no. 6, p.1195-1236, 1998). This type of structure was also observed in other works by different authors (NOGUEIRA, RI Process of obtaining chicory inulin (Cichorium intybus) powder. 151f. Thesis (Doctorate in Agricultural Engineering) - Faculty of Agricultural Engineering, State University of Campinas, Campinas, 2002; LEITE, JTC; PARK, KJ; RAMALHO, JRP Analysis of inulin powder microstructure by scanning electron microscopy In: XVIII Brazilian Congress of Food Science and Technology (CBCTA 2002), 2002, Porto Alegre , Brazil, Anais, CD-Rom), studying spray drying of suspensions composed of inulin and modified and hydrolysed starches, used as carrier agents. The appearance of the hollow particles is due to the formation of a vacuole, a vapor bubble within the particles, just after the development of the "shell" on their surface.

This shell swells when the particle temperature exceeds the local boiling temperature and the vapor pressure within this vacuole exceeds the local ambient pressure (NIJDAM, JJ; LANGRISH, TAJ). Food Engineering, v.77, no. 4, p.919-925, 2006).

Two experiments were performed with temperature of 150 ° C, the image presented in Figure 10 corresponds to the initial particles of experiment I, with pressure of 4 kg / cm2 and 10% of total solids. The image shown in Figure 11 corresponds to the initial particles, with a temperature of 170 ° C of total solids and a pressure of 4 kg / cm2, using different maltodextrin concentrations.

According to Figure 11, the particles were close to each other, which is characteristic of powders produced with encapsulants, generally polysaccharides. Particles were predominantly agglomerated, small particles occurring on the surface of larger particles, although some scattered granules can be found. In addition, it was observed that the lower the concentration they are the more crowded. Cluster formation is an especially important fact because it confers greater protection to the stuffing (COLOMBO, VE; GERBER, F. Structures and properties of stabilized vitamin and carotenoid dry powders. Food Structure, v. 10, pp. 161-170, 1991 ). The image shown in Figure 12 corresponds to the initial particles, with 190 ° C total solids temperature and pressure of 4 kg / cm2, using different maltodextrin concentrations.

In Figure 12, Experiment II presents with good parts of the agglomerated particles, while Experiment V is presented as a caravel, because its encapsulation was not efficient. In all observations, regardless of the material concentration and drying inlet air temperature, the variation in particle size was clear.

Particle Size Arrangement Particle size was obtained by directly measuring the diameter of the spherical structures provided by the microscope with a caliper and using the scale of the figures.

Measurements of the smaller and larger spheres were taken in order to know the diameter range of the spheres produced in relation to the different conditions of the spray drying process, according to the method described by Nogueira (NOGUEIRA, RI). Chicory (Cichorium intybus) Powder 15lf Thesis (Doctorate in Agricultural Engineering) - Faculty of Agricultural Engineering, State University of Campinas, Campinas, 2002).

Due to the large difference in morphology observed in micrographs, and to have a concentration parameter were determined the smallest and largest particle diameter characterizing the maximum range of variation. This can be observed in Table 22.

Table 22 - Maximum and minimum particle diameter values of tucupi extract powder for each Spray diyer test condition.

Samples III and XI were not analyzed, as they were not analyzed by SEM, sample V was caravel-shaped, which prevented the measurement of its diameter. As for the samples that were performed this analysis, it can be observed that there was a large size variation in all samples, which presented capsules with diameters ranging from 3.5 pm to 45pm. These values are within the particle size range reported by NONHEBEL and MOSS (1971). Sample IV produced smaller particles in the order of 3.5 pm to 33.5 pm.

Example 11 - Hygroscopic Properties Water Solubility Index (ISA) The water solubility index was determined according to the method described by ANDERSON (ANDERSON, R.A.; CONWAY, H.F .; PFEDFER, V.F .; GRIFFIN JR. E. L.

Gelatinization of corn grits by roll-and extrusion-cooking. Cereal Science Today. Minneapolis, v. 14, no. l, p. 4-12,1969). Water Absorption Index (IAA) The water absorption index was determined according to the method described by SILVA & SUGITA (2007).

The results of the analyzes for hygroscopic properties are shown in Table 23.

Table 23 - Hygroscopic properties of microencapsulated tucupi (powder) on wet basis. * Solubility of water; ** water absorption index; ***Water activity. Water Solubility Index (ISA) Table 23 shows that the ISA found for tucupi powder ranged from 4.00 ± 0.67% to 56.87 ± 0.75%. Maia et al. (1999) reported ISA values ranging from 24.00% to 34.45% for dehydrated rice and soy porridges. It is noticeable that the ISA is very influenced by the parameters, due to the large variation found in the experiments, Water Absorption Index (IAA) In Table 23 it is possible to observe that the IAA found for tucupi powder ranged from 0.60 ± 0, 10% and 8.53 ± 0.11%. The values reported in the literature for cornmeal and corn bran are respectively 3.3% and 7.1% (Ferreira 2006). Thermal processes, such as the atomization process, increase IAA values due to gelatinization of starch granules and protein denaturation (Alvim et al. 2002). Gelatinized granules absorb more water than granules in their native state and proteins, due to conformational and structural changes, have their hydrophilic / hydrophobic balance altered.

Example 12 - Physicochemical Analysis of pH Optimized Microencapsulated Tucupi

Obtained directly with the aid of pH meter according to AOAC Method 42.1.04 (1984) at 25 ° C. Total Titratable Acidity Determined by titration with sodium hydroxide according to AOAC Method 945.15 (1984). Moisture Obtained by prior evaporation of the sample in a water bath, followed by drying in an oven at 105 ° C according to AOAC Method 31.1.02 (1984) .Grey Obtained by prior evaporation of the sample in a water bath, followed by furnace incineration plants at 560 ° C according to AO AC method 31.1.04 (1984).

Proteins Determined by the micro Kjeldahl technique, based on hydrolysis and subsequent distillation of the 6.25 conversion factor sample according to AO AC Method 31.1.08 (1984) .Total Sugars and Reducers Determined by the Lane-Eynon technique ( IAL - ADOLFO LUTZ INSTITUTE Analytical Standards of Instituto dolfo Lutz .vl: Chemical and Physical Methods for Food Analysis 4th ed São Paulo: IMESP, 2004.) Starch According to CEREDA et. al. (CEREDA, P. P .; DAIUTO, E. R .; VILPOUX, O.

Methodology of starch determination in acid microwave digestion. ABAM - BRAZILIAN ASSOCIATION OF CASSAVA STARCH PRODUCERS. YEAR II - N ° 8 - September - December / 2004). Thereafter, the volume is completed in a 250 ml volumetric flask and the titration of sugars is performed by Lane-Eynon (IAL - ADOLFO LUTZ Institute. Analytical Standards of the Instituto dolfo Lutz .vl: Chemical and physical methods for food analysis. 4th edition São Paulo: IMESP, 2004.) Carotenoids It was performed according to the methodology described by GODOY and RODRIGUEZAMAYA (GODOY, T. T .; RODRIGUEZ-AMAYA, DB. Adolf Lutz, 57: 73-79, 1998.).

Bulk density Determined according to the methodology described by Tonon (ΤΟΝΟΝ, RV Acai juice spray drying: Influence of process variables, product quality and stability. 242f. Thesis (Doctorate in Food Engineering) - School of Food Engineering, State University of Campinas (Campinas, 2009). The density was calculated according to the following equation: d = m / V

Where: m: mass (g); and V: volume (mL).

Absolute Density Absolute density (D) of samples was determined at 25 ° C on an AccuPyc 1330 Automatic Gas Pycnometer Helium Gas Pycnometer (Micromeritics, Norcross, USA). Intragranular Porosity Intragranular Porosity (E) of powders was determined according to with the following Equation: E = 1 - (d / D) Where: d is the apparent density (g / mL); and D is the bulk density (g / mL) of the sample.

The results of the physicochemical characterization can be seen in Table 24.

Table 24 - Physicochemical characterization of tucupi. * Author's data; ** ml NaOH x 100'1; *** Calculated as a function of β-Carotene; **** Values obtained after reconstitution.

Table 24 shows that there was an increase in tucupi pH, from 3.71 to 3.88. Righetto (RIGHETTO, AM) Physicochemical characterization and stability of microencapsulated green acerola juice by atomization and lyophilization Thesis (PhD in Nutrition Science) - Faculty of Food Engineering , State University of Campinas, Campinas, 2003.

Available at: <http://bibl Biblioteca.universia.net/ficha.do?id=3901733>. Accessed: August 1, 2009. 176 p.) Found for microencapsulated (liquid) acerola juice pH 4.7. As a result, the total titratable acidity decreased from 6.19% to 4.67%.

There was a significant increase in the content of total and reducing sugars due to the addition of maltodextrin to tucupi. As expected, the humidity decreased significantly due to the atomization process (from 95.75% to 6.41%). There has been a considerable increase in ash content, along with an increase in protein content, both due to decreased tucupi moisture content.

There was a decrease in the amount of total carotenoids in the powder in relation to the liquid (from 24.55pg / 100g to 13.18pg / 100g), because carotenoids are thermosensitive, which causes this loss. Moreover, tucupi cannot be considered a product with significant carotenoid value, other work in the area (OLIVEIRA, Μ. A. Evaluation of the influence of drying adjuvants on the properties of atomized cashew juice. Dissertation submitted to Course Coordination Graduate in Food Technology, Federal University of Ceará, as a partial requirement to obtain a Master's degree in Food Technology (Fortaleza, CE. 2008) reports the value found in atomized cashew juice values of 330pg / 100g for total carotenoids.

With respect to starch, the increase may be related to the atomization process which provides the concentration. There are no references to the starch present in tucupi.

According to Chisté (CHISTÉ, RC Study of the physicochemical and microbiological properties in the production of cassava flour from the dry and water groups, fine subgroup, type 1. 67f. Final Paper - Agroindustrial Technology in Food, State University Belém, 2006) for cassava flour starch contents ranging from 73.59 ± 0.28% to 77.21 ± 0.31%. The difference between these quantities is because flour is the main product of cassava, while tucupi is a byproduct of cassava. The difference between the amount of starch and the amount of total sugars was also observed by Caniato (Caniato et. Al. 2004) in green corn cultivars.

Also according to Table 24, it is possible to observe that the absolute density varies from liquid tucupi to powder. This is due to the addition of maltodextrin in the product.

According to Tonon (ΤΟΝΟΝ, RV Acai juice spray drying: Influence of process variables, product quality and stability. 242f. Thesis (PhD in Food Engineering) - School of Food Engineering, State University of Campinas. Campinas, 2009.), porosity is an important property in the case of microcapsules where encapsulated material is susceptible to oxidation reactions. The larger number of voids implies the presence of a higher amount of oxygen, which can cause faster degradation of the protected compound. For this author, the porosity results were between 68.33% and 75.49% for acai juice powder, while for the microencapsulated tucupi the result was 15.46%, demonstrating that the result was satisfactory. . The lipid content found is very low. There are no data on tucupi lipid content in the literature. In cassava flour, the lipid content ranges from 0.11% to 0.31%. (CHISTÉ, RC Study of physicochemical and microbiological properties in the production of cassava flour from dry and water groups, fine subgroup, type 1. 67f. Course Conclusion Paper - Agroindustrial Technology in Food, State University of Pará Belém, 2006) According to Taco (2006), raw cassava has 0.3% lipids.

Process yield This was obtained by dividing the weight of the encapsulated tucupi by the weight of the raw material multiplied by 100 to express the percent yield as shown in the following equation. R (%) = (pte / pmp) x 100 Where: pte is the weight of encapsulated tucupi (g); and pmp is the weight of the raw material (g). The yield of the microencapsulated tucupi atomization process was 57.64%.

According to Tonon (ΤΟΝΟΝ, RV Acai juice spray drying: Influence of process variables, product quality and stability. 242f. Thesis (PhD in Food Engineering) - School of Food Engineering, State University of Campinas. Campinas, 2009), the product yield is directly linked to the temperature and amount of the added carrier agent (maltodextrin). The temperature has a positive effect on the results, its increase causes an increase in yield. Regarding the carrier agent, the higher its concentration, the lower the process yield, which may be related to an increase in viscosity. According to CAI and CORKE (CAI, Y.Z .; CORKE, H.

Production and properties of spray-dried Amaranthus betacyanin pigments. Journal of Food Science. V.65, no. 6, p. 1248-1252, 2000), maltodextrin may have caused the largest amount of solids to stick to the wall of the atomization chamber.

Color analysis A value of ΔΕ * was found for the color analysis of 36.32. This variation was responsible for a variation in the final color of the product, so that there was a loss in yellow coloration in the final product, making it less attractive. This decrease in yellow color was mainly caused by the increase in maltodextrin concentration, due to its white color, and loss of total carotenoids in the final product, due to the heating occurred in the atomization process.

Example 13 - Ideal conditions of the product The results obtained in the physical and chemical analyzes showed that the tucupi sample presented an average humidity of 95.75, ashes 0.8, the total titratable acidity content was 4.59. For protein content was found, on average, 0.89, pH was on average, 3.71, being considered a product of high acidity. For the ° Brix / acidity ratio, a value of 0.82 was found.

By optimizing the atomization process, it was determined that the ideal sample was in the central region of the defined through experimental design. The temperature was set at 170 ° C and 7.5% total solids. According to the optimized sample particles presented spherical shape, which is characteristic of powders produced by the spray drying process. The particle surfaces were predominantly rough, although some had a completely smooth surface, and it was observed that the higher the temperature, the particles are less rough.

There is a decrease in total titratable acidity from 6.19% to 4.67%, a significant increase in the content of total and reducing sugars due to the addition of maltodextrin to tucupi.

There is a considerable increase in ash content, along with an increase in protein content, both resulting from decreased tucupi moisture content.

There is a slight decrease in the amount of total carotenoids in the powder relative to the liquid (from 24.55gg / 100g to 13.18gg / 100g). Regarding starch, the increase may be related to the addition of maltodextrin to tucupi, and also to the atomization process, which provides its concentration.

Claims (9)

1 - Production process of tucupi powder, characterized in that it comprises the following steps: 1) obtaining the tucupi; 2) use of an encapsulating agent; 3) homogenization; and 4) drying, which results in obtaining microencapsulated tucupi. Process of tucupi powder according to Claim 1, characterized in that the encapsulating agent is a carbohydrate, preferably maltodextrin. Process for producing tucupi powder according to claim 1, characterized in that the drying takes place by atomization. Tucupi powder production process according to Claim 3, characterized in that the drying is by spray drying. Production process of tucupi powder according to claim 4, characterized in that drying uses the percentage range of total solids ranging from 4% to 11%. Tucupi powder production process according to Claim 5, characterized in that the percentage of total solids of 7.5% is preferably used. Process for the production of tucupi powder according to claim 4, characterized in that the drying utilizes the inlet air temperature ranging from 140 ° to 200 ° C. Process for producing tucupi powder according to claim 7, characterized in that it preferably uses a temperature of 170 ° C. 9 - Microencapsulated tucupi powder product.