Encapsulation compositions and process for preparing the same

Drug – bio-affecting and body treating compositions – Preparations characterized by special physical form – Biocides; animal or insect repellents or attractants

Reexamination Certificate

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C424S400000, C424S405000, C424S406000, C424S439000, C424S440000, C424S441000, C424S442000, C424S484000, C424S485000, C514S774000, C514S777000, C514S778000, C514S779000, C514S780000, C514S781000, C514S782000

Reexamination Certificate

active

06790453

ABSTRACT:

BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to encapsulation compositions in which an encapsulate is encapsulated in a glassy matrix. More particularly, the present invention relates to flavor encapsulation compositions in which a flavoring agent is encapsulated in a glassy matrix. The present invention further relates to processes for preparing such compositions.
2. Discussion of the Background
The encapsulation of encapsulates is an area of active research. In particular, the encapsulation of encapsulates such as medications, pesticides (including insecticides, nematocides, herbicides, fungicides, microbicides etc.) preservatives, vitamins and flavoring agents is desired for a number of reasons. In the case of medications and pesticides, encapsulation may be desired to achieve the controlled release of the medication or pesticide. In the case of vitamins, encapsulation may be carried out to protect the vitamin from air-oxidation and, thus, to extend shelf life of the vitamin. In the case of the flavoring agent, the encapsulation may be carried out to place the flavoring in an easily metered form which will release the agent at a controllable event, such as the addition of water.
It is generally known to skilled practitioners in the field of flavor encapsulation that the current practical commercial processes leading to stable, dry flavors are limited to spray drying and extrusion fixation. The former process requires emulsification or solubilization of the flavor in an aqueous carrier containing the encapsulation solids, followed by rapid drying in a high temperature, high velocity gas stream and collection as a low density bulk solid.
While spray drying accounts for the majority of commercially encapsulated flavor materials, several limitations of the process are evident. Low molecular weight components of complex or natural flavor mixtures generally exhibit high vapor pressures and are usually lost or disproportionate during the process. The resultant flavor-carriers are porous and difficult to handle. In addition, deleterious chemical reactions such as oxidation can result on surfaces exposed during and after drying. The final product, a dry, free flowing powder, will release the encapsulant rapidly upon hydration whether rapid release is desired or not.
U.S. Pat. No. 3,971,852 discloses the use modified starch, gums and other food polymers with low molecular weight polyhydroxy compounds with spray drying to yield a glassy matrix with encapsulated oil at a maximum of 70-80% by volume. The system forms a shell surrounding the oil flavoring but is limited to lipophilic flavoring agents.
U.S. Pat. No. 4,532,145, discloses a process for preparing compositions in which a volatile flavorant is fixed by spray drying from a carrier solution made up of 10-30% of a low molecular weight component such as a sugar or edible food acid with the balance of the solids being a maltodextrin carbohydrate in the amount of 70-90%.
U.S. Pat. No. 5,124,162 discloses a carrier mixture composed of mono- and disaccharides (22-45%), maltodextrins (25-50%), and a high molecular weight carbohydrate such as chemically modified starch, gum arabic or gum acacia (10-35%) to which flavoring agents are added and the subsequent solution spray dried to yield a free flowing powder with a bulk density of 0.50 g/cc.
U.S. Pat. No. 5,601,760 discloses a carrier mixture utilizing whey protein isolates to encapsulate lipid flavor systems. The protein constitutes 35 to 100% of the encapsulating matrix with the remainder consisting of sugars. Other disclosed proteins include whey protein concentrates, &bgr;-lactoglobulin and &agr;-lactoalbumin.
Several technical issues unmet by these approaches are evident. First thermally sensitive flavors undergo undesirable reactions including oxidations, rearrangements and hydrolyses. Secondly, volatile components are lost or disproportionate during atomization and evaporation in the dryer.
A second process route, that of melt encapsulation has been utilized to advantage with lipid-based flavors. In this technology, a melt is prepared by boiling off sufficient water from a high solids carbohydrate syrup, adding flavoring oils with emulsifier, agitating under pressure to emulsify the oil in the melt and injecting the mixture into a chilling, dehydrating solvent bath to obtain fine rod-like filaments. After solvent removal, the matrix is reduced in size and, in some cases, coated with an anti-caking agent before being packed. See, e.g., U.S. Pat. Nos. 2,809,895; 3,041,018; 2,856,291; 2,857,821; and 3,704,137. Subsequent improvements in the art are disclosed in U.S. Pat. No. 3,314,803, for the encapsulation of volatiles such as acetaldehyde, and in U.S. Pat. No. 4,707,367, which discloses encapsulation of up to 35% by weight flavor oil in the glassy matrix.
U.S. Pat. No. 4,689,235 discloses the use of modified starch-maltodextrin carriers in the range of 5 parts modified starch:95 parts maltodextrin to 95 parts modified starch:5 parts maltodextrin. The carrier is dissolved to form a syrup, the water is cooked off, flavor is added and emulsified, and the melt is injected into a solvent bath.
An alternative route to encapsulating flavors is disclosed in U.S. Pat. No. 4,230,687. In this approach, high molecular weight carriers such as proteins, starches and gums are plasticized by addition of significant amounts of water in the presence of the encapsulate and subjected to a high shear dispersing process. The rubbery or plastic matrix with encapsulate is then extruded, recovered and dried to yield a stable product.
Another alternative process, melt extrusion, can be utilized for flavor fixation and encapsulation. In this process, a melting system, i.e. an extruder, is employed to form the carrier melt in a continuous process. The encapsulated flavor is either admixed or injected into the molten carbohydrate carrier. U.S. Pat. No. 4,420,534 discloses the use of a matrix composition consisting of 10-30% of a low molecular weight component chosen from a series of mono- and disaccharides, corn syrup solids, or organic acid with a balance of the mixture being maltodextrin. The matrix is dry blended with an anhydrous liquid flavoring component and melted in a single screw extruder to yield a solid matrix characterized as a glass with a glass transition temperature greater than 40° C.
U.S. Pat. No. 5,972,395 discloses use of a matrix composed of 15 to 40% of a high molecular weight carrier, preferably a maltodextrin and at least 40% of a low molecular weight carbohydrate, sugar polyol or adipic acid. The matrix is extruded to yield a solid matrix characterized as a glass.
U.S. Pat. Nos. 5,087,461 and 5,009,900 disclose a similar approach utilizing a composition consisting of a modified food starch, maltodextrin, polyol and mono- and disaccharide components. The starch is a chemically modified water-soluble starch and is used in the amount of 40 to 80% of the total mixture. The balance of the composition is comprised of 10 to 40% maltodextrin, 5 to 20% corn syrup solids or polydextrose and 5 to 20% mono- or disaccharide. This matrix is made to balance processing response with glass matrix character.
U.S. Pat. Nos. 6,187,351, 5,603,971, and 5,987,897 disclose the use of a series of matrix compositions utilizing modified starch with mono- or disaccharides, modified starch with polyol, and food polymer plus carbohydrates. The use of water to plasticize the matrix in the extrusion process yields an encapsulated flavor matrix characterized by glass transition temperatures greater than 40° C. In U.S. Pat. No. 6,187,351, the use of 2 to 45% of a food polymer, 25 to 80% of a maltodextrin, and 10 to 30% of a mono- or disaccharide or 24 D.E. to 42 D.E. corn syrup solids is disclosed. The matrix is dry blended, fed into the extruder with the required water plasticizer and flavor, and the resulting encapsulate is obtained as a glassy solid exhibiting a glass transition temperature greater than 40° C. The disclosed polymers include modified celluloses, high methoxy pe

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