EP0989807A1 - Procede de preparation de confiserie par hydratation positive et produit obtenu - Google Patents
Procede de preparation de confiserie par hydratation positive et produit obtenuInfo
- Publication number
- EP0989807A1 EP0989807A1 EP98924947A EP98924947A EP0989807A1 EP 0989807 A1 EP0989807 A1 EP 0989807A1 EP 98924947 A EP98924947 A EP 98924947A EP 98924947 A EP98924947 A EP 98924947A EP 0989807 A1 EP0989807 A1 EP 0989807A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- saccharide
- ingredients
- water
- mass
- component
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
Classifications
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23G—COCOA; COCOA PRODUCTS, e.g. CHOCOLATE; SUBSTITUTES FOR COCOA OR COCOA PRODUCTS; CONFECTIONERY; CHEWING GUM; ICE-CREAM; PREPARATION THEREOF
- A23G3/00—Sweetmeats; Confectionery; Marzipan; Coated or filled products
- A23G3/34—Sweetmeats, confectionery or marzipan; Processes for the preparation thereof
- A23G3/36—Sweetmeats, confectionery or marzipan; Processes for the preparation thereof characterised by the composition containing organic or inorganic compounds
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23G—COCOA; COCOA PRODUCTS, e.g. CHOCOLATE; SUBSTITUTES FOR COCOA OR COCOA PRODUCTS; CONFECTIONERY; CHEWING GUM; ICE-CREAM; PREPARATION THEREOF
- A23G3/00—Sweetmeats; Confectionery; Marzipan; Coated or filled products
- A23G3/02—Apparatus specially adapted for manufacture or treatment of sweetmeats or confectionery; Accessories therefor
- A23G3/0205—Manufacture or treatment of liquids, pastes, creams, granules, shred or powder
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23G—COCOA; COCOA PRODUCTS, e.g. CHOCOLATE; SUBSTITUTES FOR COCOA OR COCOA PRODUCTS; CONFECTIONERY; CHEWING GUM; ICE-CREAM; PREPARATION THEREOF
- A23G3/00—Sweetmeats; Confectionery; Marzipan; Coated or filled products
- A23G3/34—Sweetmeats, confectionery or marzipan; Processes for the preparation thereof
- A23G3/36—Sweetmeats, confectionery or marzipan; Processes for the preparation thereof characterised by the composition containing organic or inorganic compounds
- A23G3/362—Sweetmeats, confectionery or marzipan; Processes for the preparation thereof characterised by the composition containing organic or inorganic compounds containing inorganic compounds
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23G—COCOA; COCOA PRODUCTS, e.g. CHOCOLATE; SUBSTITUTES FOR COCOA OR COCOA PRODUCTS; CONFECTIONERY; CHEWING GUM; ICE-CREAM; PREPARATION THEREOF
- A23G3/00—Sweetmeats; Confectionery; Marzipan; Coated or filled products
- A23G3/34—Sweetmeats, confectionery or marzipan; Processes for the preparation thereof
- A23G3/36—Sweetmeats, confectionery or marzipan; Processes for the preparation thereof characterised by the composition containing organic or inorganic compounds
- A23G3/42—Sweetmeats, confectionery or marzipan; Processes for the preparation thereof characterised by the composition containing organic or inorganic compounds characterised by the carbohydrates used, e.g. polysaccharides
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23G—COCOA; COCOA PRODUCTS, e.g. CHOCOLATE; SUBSTITUTES FOR COCOA OR COCOA PRODUCTS; CONFECTIONERY; CHEWING GUM; ICE-CREAM; PREPARATION THEREOF
- A23G3/00—Sweetmeats; Confectionery; Marzipan; Coated or filled products
- A23G3/34—Sweetmeats, confectionery or marzipan; Processes for the preparation thereof
- A23G3/36—Sweetmeats, confectionery or marzipan; Processes for the preparation thereof characterised by the composition containing organic or inorganic compounds
- A23G3/48—Sweetmeats, confectionery or marzipan; Processes for the preparation thereof characterised by the composition containing organic or inorganic compounds containing plants or parts thereof, e.g. fruits, seeds, extracts
Definitions
- the present invention relates to the art of unique delivery systems for comestibles, especially to confectionery manufacturing and particularly to novel methods of making a functionalized confectionery mass which do not require cooking to dehydrate and products therefrom. More particularly, the invention relates to comestible delivery systems, uncooked confectioneries and nougats, and methods for making same.
- nougats It is generally considered a necessity in the art of preparing food or drug delivery systems like confectionery masses such as nougats to use water as a mixing medium and source of hydration for ingredients.
- a typical recipe calls for soaking egg albumen in water over a period of time, such as overnight, in order to fully hydrate the protein. Following hydration the egg albumen is stirred and strained before being beaten into a stiff foam.
- Other ingredients such as sugar, honey, and corn syrup are separately cooked with water to a relatively high cooking temperature of from about 135°C to about 138°C to achieve the necessary interaction among the ingredients. The cooked mixture is then poured into the egg and beaten with a nougat mixer, which is similar to a marshmallow mixer but generally more robust.
- water remains as a separate phase in the end product.
- This water is not bound to other ingredients and can be referred to as free moisture or unbound water.
- Free moisture can detract from the end product because it weakens the structural integrity and/or reduces the quality of organoleptic perception.
- excessive free moisture results in higher water activity, and thereby provides an environment in which microorganisms can grow.
- Microbiological growth in food products has also been used to measure the existence of free moisture. Free moisture has been identified in food art by the term water activity. Water activity is defined as the ratio of the vapor pressure of water in an enclosed chamber containing a food to the saturation vapor pressure of water at the same temperature. Water activity is an indication of the degree to which unbound water is found and, consequently, is available to act as a solvent or to participate in destructive chemical and microbiological reactions.
- the present invention overcomes the difficulties set forth above as well as other difficulties generally associated with the prior art.
- both the necessity of cooking the confection to obtain desired physical properties and using excessive water to mix and hydrate one or more ingredients is eliminated, and the method and product of the invention are obtained without any need for dehydration. Heating at high temperatures and mixing to drive off excessive moisture are no longer required. Consequently, the detrimental heat history generally associated with energy-intensive procedures is also eliminated. Separation of the water from the resulting product is avoided and the lowered water activity results in a product having superior physical, storage, and organoleptic properties with reduced microbial growth problems.
- the present invention is a method of making a unique food and drug delivery system, and especially a novel confectionery delivery system, especially a nougat, by a positive hydrating step and without the need for dehydrating in order to produce the confectionery mass.
- the present invention also includes the product resulting from the new method of preparation.
- a saccharide-based component is combined with a hydrated hydrobinding component.
- a primary part of the saccharide-based component is a saccharide material such as sucrose, corn syrup solids, polydextrose, and mixtures thereof.
- a preferred saccharide-based ingredient is polydextrose.
- Other highly preferred saccharide materials include sucrose and corn syrup solids. Maltodextrin is also highly desirable, as well as mixtures of any of the foregoing.
- a saccharide ingredient can also be included as part of the hydrobinding component, as for example, a sweetener.
- the hydrobinding component can include a proteinaceous material such as a gelatin, or a food grade gum such as gum arabic, carrageenan, locust bean gum, guar gum, and mixtures thereof.
- a proteinaceous material such as a gelatin
- a food grade gum such as gum arabic, carrageenan, locust bean gum, guar gum, and mixtures thereof.
- One preferred hydrobinding component includes a mixture of a gelatin and gum arabic.
- Another preferred hydrobinding ingredient includes a mixture of carrageenan, locust bean gum, and a crosslinking agent.
- the gelatin and/or food grade gum imparts viscoelasticity to the confectionery mass, possibly as a result of cross-linking in these materials.
- the hydrobinding component can also be aerated, preferably in the presence of an aerating agent, prior to or after combining it with the saccharide-based component.
- Aerating agents include, among other things, egg whites, soy protein
- hydrobinding component oleaginous materials, such as hydrogenated vegetable oils, emulsifiers, and mixtures thereof.
- oleaginous materials such as hydrogenated vegetable oils, emulsifiers, and mixtures thereof.
- the hydrobinding component is further employed with a wetting agent or humectant, such as polyol like glycerin or other commercially available material having similar functionality.
- active ingredients can be included in the confectionery mass which is formed as a result of the present invention.
- the active ingredients are typically ones which are intended to produce a biological and/or chemical response in the body.
- the active ingredients can be quite varied, and a non-exhaustive list has been set forth hereinbelow.
- Especially preferred actives include antacid materials or bioassimilable sources of calcium.
- a nougat mass is prepared which has a frappe consistency and is made with nutritional ingredients so that a health product can be produced.
- vegetable and/or fruit components can be added to provide a nutritious food product. If desired, a product having the minimum daily nutritional requirements can be produced.
- the recommended human adult dietary serving of nutrients is defined by the Consumer Affairs Division of the United States Food and Drug Administration.
- a health bar has been prepared which contains the nutritional equivalent of up to five (5) recommended human adult dietary servings of vegetable and/or fruit.
- ingredients which have strong olfactory characteristics e.g., aroma and flavor, can be treated to enhance control of potency before incorporating into a health product prepared in accordance with the invention.
- the product resulting from the present invention is unique because it requires no cooking and no dehydration by traditional heating at high temperatures to produce, and has substantially no phase separation of moisture.
- the only moisture present is an amount sufficient to functionalize the mass.
- the product can be prepared without cooking.
- the product can also be prepared using low or high shear mixing, i.e. with no flash-flow processing is required.
- the water activity is not greater than about 60% ERH, and is preferably not greater than about 55% ERH.
- Another measure of free moisture in foodstuffs is the amount of biological growth within the composition.
- the biological activity is less than about 100 ppm, preferably less than about 25 ppm, and most preferably less than about 10 ppm.
- the present invention also provides the ability to formulate confectionery masses with a significantly reduced fat and calorie content. This result is quite unexpected, since fat has traditionally been used to assist in functionalizing food masses by providing internal lubrication without water.
- Other features of the method of the invention include improved processing, intimate mixing and enhanced dispersion of dissimilar ingredients.
- the final product furthermore exhibits improved content uniformity and improved taste perception qualities. In fact, consumers consistently rate the product of the invention higher than many commercially-prepared similar formulations for such qualities as firmness, flavor, bite, sweetness, chewiness, melt characteristics, stickiness, juiciness, freedom from grit, and aftertaste. Overall, the formulated confectionery delivery system herein described is more palatable than many of the current products available in the art.
- the method for making confectionery-mass delivery systems in accordance with the present invention includes combining a saccharide-based component and a hydrobinding component, the latter component being hydrated sufficiently to provide controlled water delivery to the saccharide-based component and/or other ingredients.
- Controlled water delivery means delivery of water in an amount and at a rate which is sufficient to provide internal viscosity and cohesivity to the saccharide-based component.
- the word hydrated as used in the term hydrated hydrobound component herein means containing sufficient water to provide the requisite controlled water delivery.
- the system created by the combination of the present invention is a water-starved system, which means that the system has only enough moisture to bind the ingredients together and provide internal lubricity. Since the ingredients are competing for moisture due to enhanced wettability, there is virtually no free moisture available to separate from the mass.
- the saccharide-based component can be advantageously provided in the form of a shearform matrix, as that term is defined hereunder, as a shearform matrix has significantly enhanced wettability because of a randomized structure resulting from flash-flow processing.
- Shearform matrix refers to the product prepared by a method of flash-flow processing, a method which mixes and conditions ingredients for intimate contacting and enhanced hydration described, for example, in US 5,587,198.
- the invention can benefit from subjecting the saccharide-based component to such flash-flow processing to provide a saccharide based shearform matrix.
- the hydrobinding component can, if desired, also be subjected to flash-flow processing before hydrating.
- the hydrobinding component can also be aerated, preferably in the presence of an aerating agent, before or after combining with the shearform matrix.
- One embodiment of the present invention also includes flash-flow processing of certain ingredients prior to combining with other ingredients as set forth hereinabove.
- Flash-flow processing and pre-flash-flow processing results in increased surface area and increased solubility of the ingredients subjected thereto, and contributes to actual binding of the ingredients to each other.
- the saccharide-based component could be first prepared by flash-flow, and then combined with the hydrating component by shear mixing.
- high shear mixing refers to relatively intensive mixing action concentrated in a localized area.
- the high speed impact of mixing mechanisms such as blades or choppers results in shearing action. This in turn creates localized high shear force and a fluidizing effect at the point of contact, which causes particular scale diffusion and disagglomeration and faster mixing in a relatively small area of the entire mixing volume.
- High shear mixing may also result in increased temperature at the point of impact of the shearing apparatus with the mix, thereby further contributing to the effective mixing action.
- High shear mixing should be contrasted with low shear mixing in which the main action of mixing is due to the relative motion of a much larger volume of mix being circulated by the spinning or churning action of a lower impact type mechanism, such as a paddle-blade typically found in a Sigma or Hobart mixer.
- a lower impact type mechanism such as a paddle-blade typically found in a Sigma or Hobart mixer.
- the resultant product can be referred to as both uncooked and unspun.
- the present invention provides a method and composition for preparing a functionalized confectionery mass without the use of excess water.
- Functionalization of a confectionery mass means providing the ingredients with sufficient internal cohesivity to be handled without losing its integrity as a mass. In order to be handled in the context of functionalization, the mass must also possess internal lubricity which permits inter- and intra-particle movement without loss of cohesiveness.
- Functionalized food masses have been described as having the consistency of a dough or paste, or as chewy, etc. However, the present invention is not to be limited by any short-hand description of the consistency. Functionalization of food masses has in the past relied upon the use of significant amounts of added fat, but the present invention enables the artisan to functionalize a confectionery mass without need for added fat if so desired. Functionalization is achieved in the present invention by using certain ingredients, as specified herein. Nonetheless, selected amounts of fat may be added to obtain a confection having desirable perceived texture and/or flavor characteristics.
- a hydrobinding component is used to provide a functionalized hydrobound confectionery mass.
- a functionalized hydrobound confectionery mass as used herein is a functionalized mass of confectionery ingredients which contains substantially no excessive free moisture or unbound water.
- a functionalized hydrobound confectionery mass of the present invention does not require dehydration, e.g., by cooking at high temperatures, to remove excess water. The method of the invention, therefore, is substantially more efficient than previously known methods. Less energy costs are expended in the methods herein set forth, while the resulting product is a markedly improved confectionary delivery system.
- hydrobinding While applicants do not wish to be bound by theory, it is believed that water is tightly bound to surface polar sites through chemisorption. These sites may include the hydroxyl groups of hydrophilic materials such as proteins, gums, starches, and sugar. Regardless of the actual mechanism, however, this phenomenon is referred to herein as hydrobinding.
- a hydrobinding component is an ingredient which imbibes, delivers and maintains water in an amount sufficient to functionalize the resulting mass.
- the water which is hydrobound does not separate and become a separate phase.
- a hydrobinding component cooperates with other ingredients to deliver and maintain water sufficient to functionalize the mass of ingredients, including those ingredients which have been subjected to flash-flow processing.
- flash-flow processing is used to prepare other ingredients for use in the confectionery mass. Flash-flow processing not only ensures intimate mixing of ingredients without the use of water as a medium, but also conditions the ingredients for wetting with a minimum of water. It has now been further found that shear mixing, and preferably high shear mixing, can achieve the beneficial results of flash-flow processing, but without the extra time and cost associated therewith.
- a hydrobinding component can be hydrated and mixed with a shearform matrix (i.e., ingredients which have been subjected to flash-flow processing) or shear mixed with the ingredients '(making up the saccharide-based feedstock) to form a functionalzedt hydrobound confectionery-mass delivery system.
- a shearform matrix i.e., ingredients which have been subjected to flash-flow processing
- shear mixed with the ingredients '(making up the saccharide-based feedstock) to form a functionalzedt hydrobound confectionery-mass delivery system.
- the hydrobinding component and saccharide-based component acting in concert with one another, capture or bind sufficient moisture to functionalize the total mass.
- the ingredients capture the moisture by some mechanism as yet unelucidated, possibly physically, chemically, and/or even biologically. Whatever the binding mechanism may be, water is held and made available for absorption by the remainder of the ingredients. The addition of considerable excess water is thus avoided, as is cooking to subsequently drive off the added moisture.
- Hydrobinding ingredients useful in the present invention include, for example, proteinaceous materials known to those skilled in the art, and preferably gelatins of various grades and types. Also preferred are food grade gums such as gum arabic, carrageenan, guar gum, and locust bean gum, and mixtures thereof. Hydrobinding ingredients comprising a mixture of components are desirable in some situations. Highly preferred hydrobinding ingredients include, for example, a mixture of gelatin and gum arabic, or a mixture of carrageenan and locust bean gum with a crosslinking agent, such as potassium citrate or potassium chloride, which induces crosslinking between these materials. These mixed hydrobinding materials are advantageous not only for their hydrobinding capacities, but also because they impart viscoelasticity to the resulting confectionery.
- hydrobinding material can also benefit from inclusion of a wetting agent or humectant such as a polyol known in the art, desirably glycerin, or other functionally similar materials which are commercially available.
- a wetting agent or humectant such as a polyol known in the art, desirably glycerin, or other functionally similar materials which are commercially available.
- the hydrobinding component will comprise about 0.5-20% of the comestible delivery system of the invention. Preferably, the hydrobinding component will be within the range of about 5-15%, and even more desirably within the range of about 5-10%. Of the foregoing hydrobinding component, water will comprise about 30 - 80% thereof, and preferably about 40 - 70% of the hydrobinding component.
- the proteinaceous material or the gum, or combination thereof will make up about 0.5 to 60% of the hydrobinding component, and more preferably be within the range of about 3 to 50%, more desirably about 5 to 20%) (unless otherwise set forth, all %s herein are percentages by weight, or weight percent).
- a wetting or softening agent such as a polyol, preferably glycerin, which may be included in amounts equal to about 0 - 15%, preferably about 0.1 - 10% of the composition of the invention, even more desirably about 5-10%.
- the glycerin (or other selected material) can also function as a humectant, and thereby keep moisture in the system.
- ingredients which are used in the hydrobinding component may instead be added as part of the saccharide-based component.
- gelatins and food grade gums such as gum arabic, carrageenan, guar gum, locust bean gum, etc., can be used to prepare the saccharide-based component, e.g., by being included in the feedstock used to prepare that component.
- the invention also employs a saccharide-based material as another major component (the hydrobinding material being the first major component).
- the saccharide- based material can include any of a large variety of saccharide materials, such as small sugars, e.g., dextrose, sucrose, fructose, etc., and larger saccharides such as corn syrup solids and polydextrose, as well as mixtures of two or more of these materials.
- Corn syrup solids are highly preferred for use as the saccharide-based material in the composition of the invention.
- Corn syrup solids are commonly known as maltodextrins.
- Maltodextrins are composed of water soluble glucose polymers obtained from the reaction of the starch with acid or enzymes in the presence of water.
- the hydrolysis reaction produces a carbohydrate mixture of saccharides having a controllable dextrose equivalence (D.E.), commonly a D.E. of less than 20.
- D.E. dextrose equivalence
- the FDA calls the resulting materials corn syrup solids.
- Polydextrose is a non-sucrose, essentially non-nutritive, carbohydrate substitute. It can be prepared from polymerization of glucose in the presence of polycarboxylic acid catalysts and polyols. Generally, polydextrose is known to be commercially available in three forms: Polydextrose A and Polydextrose K, which are powdered solids, and Polydextrose N supplied as a 70%> solution. Each of these products can also contain some low molecular weight components, such as glucose, sorbitol, and oligomers. Sugars can also be used as saccharide-based materials according to the invention.
- Sugars are those substances which are based on simple crystalline mono- and di-saccharide structures, i.e., based on C 5 (pentose) and C 6 (hexose) sugar structures.
- Sugars include dextrose, sucrose, fructose, lactose, maltose, etc., and sugar alcohols such as sorbitol, mannitol, maltitol, etc.
- the foregoing saccharide-based component can comprise about 30 - 99.5%) of the comestible delivery system according to the embodiments herein set forth.
- saccharide-based component or other ingredients herein set forth, will produce a suitable final product, depending upon the final characteristics, e.g. texture, mouth feel, product consistency, etc., which are desired.
- a highly preferred saccharide-based material will comprise a mixture of corn syrup solids and sucrose in a ratio of approximately 50/50 or 40/60.
- Other materials which can be incorporated into the material of the invention, to enhance its appearance, taste, texture, and other perceptions of the consumer include, for example, flavors, sweeteners, colorants, surfactants or emulsifiers, and fats or oils. Any one or a combination of more than one of the foregoing may comprise from about 0 - 20%) of the confectionery mass, and more desirably be within the range of about 5 - 10%) or even up to 15%) of the comestible mass.
- Flavors may be chosen from natural and synthetic flavoring liquids.
- An illustrative list of such agents includes volatile oils, synthetic flavor oils, flavoring aromatics, oils, liquids, oleoresins or extracts derived from plants, leaves, flowers, fruits, stems and combination thereof.
- a non-limiting representative list of examples includes citrus oils such as lemon, orange, grape, lime, and grapefruit, as well as fruit essences including, for example, apple, pear, peach, grape, strawberry, raspberry, cherry, plum, pineapple, apricot, or other fruit flavors.
- aldehydes and esters such as benzaldehyde (cherry, almond), citralm, i.e., alphacitral (lemon, lime), neural, i.e., betacitral (lemon, lime) decanal (orange, lemon), aldehyde C g (citrus fruits), aldehyde C 9
- flavorings may include whole and partial fruits and nuts, peanut butter, candy bits, chocolate chips, bran flakes, etc.
- Sweeteners may be added to the comestible delivery system of the invention. These may be chosen from the following non-limiting list: glucose (corn syrup), dextrose, invert sugar, fructose, and mixtures thereof (when not used as a carrier); saccharin and its various salts such as the sodium salt; dipeptide sweeteners such as aspartame; dihydrochalcone compounds, glycyrrhizin; Stevia Rebaudiana (Stevioside); chloro derivatives of sucrose such as sucralose; sugar alcohols such as sorbitol, mannitol, xylitol, and the like.
- sweeteners are also contemplated.
- the sweeteners are added in amounts equal to about 0 - 10%) of the composition, and preferably about 0.1 - 5%.
- Surfactants or emulsifiers may also be included in the composition of the invention. These may be any food grade emulsifying material, for example, lecithin or other phospholipid material, monoglycerides and/or diglycerides, and mixtures thereof in amounts of from about 0 - 3%>, more desirably about 0.1 - 1%>.
- Fats may also be included in the composition, and these can include partially or entirely unsaturated fats such as palm oil and cocoa butter.
- the texture and mouth feel of the resulting confection can be influenced by selecting the types and amounts of fats included in the saccharide-based component. Fats marketed under such trade names as Durem and Paramount have been found to be useful. Those skilled in the art will find that fats are optional as part of the composition of the invention, and may be eliminated altogether if so desired. Thus, fats will comprise about 0 - 10% of the product herein set forth, preferably less than about 7%>, and even more preferably less than about 5%>.
- Additional materials which can be incorporated into the composition include, for example, biologically active ingredients such as medicinal substances, e.g. drugs, pharmaceuticals and antacids. These are referred to herein as active ingredients. Active ingredients may make up from about 0 - 50%> of the product of the invention, and may be more depending upon the needs and abilities of those skilled in the art. It is preferred, however, to include up to about 40%) of active substance in the compositions set forth herein. As active ingredients, the medicinal substances capable of incorporation and delivery according to the invention are extremely varied (those skilled in the art may conceive of others than those herein described, and these are certainly within the scope of the invention).
- An exemplary, non-limiting list of such medicinal substances includes: antitussives, antihistamines, decongestants, alkaloids, mineral supplements, laxatives, vitamins, e.g. vitamin D3, antacids, ion exchange resins, anti-cholesterolemics, anti-lipid agents, antiarrhythmics, antipyretics, analgesics, appetite suppressants, expectorants, anti-anxiety agents, anti-ulcer agents, anti-inflammatory substances, coronary dilators, cerebral dilators, peripheral vasodilators, anti-infectives, psycho-tropics, antimanics, stimulants, gastrointestinal agents, sedatives, antidiarrheal preparations, anti-anginal drugs, vasodialators, anti -hypertensive drugs, vasoconstrictors, migraine treatments, antibiotics, tranquilizers, anti-psychotics, antitumor drugs, anticoagulants, antithrombotic drugs, hypnotics, anti-eme
- Analgesics include, for example, aspirin, acetaminophen, and acetaminophen plus caffeine.
- antidiarrheals such as IMMODIUM AD®, antihistamines, antitussives, decongestants, vitamins, and breath fresheners.
- H 2 -antagonists which are contemplated for use in the present invention include cimetidine, ranitidine hydrochloride, famotidine, nizatidine, ebrotidine, mifentidine, roxatidine, pisatidine and aceroxatidine.
- active ingredients include antiplaque medicaments and medicaments for veterinary use.
- antacids Especially preferred active ingredients contemplated for use in the present invention are antacids, H 2 -antagonists, and analgesics.
- antacid dosages can be prepared using the ingredients calcium carbonate (CaC0 3 ), either alone or in combination with magnesium hydroxide, and/or aluminum hydroxide.
- antacids can be used in combination with H 2 -antagonists.
- Active antacid ingredients include, but are not limited to, aluminum hydroxide, dihydroxyaluminum aminoacetate, aminoacetic acid, aluminum phosphate, dihydroxyaluminum sodium carbonate, bicarbonate, bismuth aluminate, bismuth carbonate, bismuth subcarbonate, bismuth subgallate, bismuth subnitrate, calcium carbonate, calcium phosphate, citrate ion (acid or salt), amino acetic acid, hydrate magnesium aluminate sulfate, magaldrate, magnesium aluminosilicate, magnesium carbonate, magnesium glycinate, magnesium hydroxide, magnesium oxide, magnesium oxide, magnesium trisilicate, milk solids, aluminum monobasic or dibasic calcium phosphate, tricalcium phosphate, potassium bicarbonate, sodium tartrate, sodium bicarbonate, magnesium aluminosilicates, and tartaric acids and salts.
- Calcium supplement products can also be prepared by incorporation of a bioassimilable calcium source in the comestible delivery system confectionary of the invention.
- the calcium source is calcium carbonate, but other sources of calcium capable of absorption or bioassimilation can be employed, including finely divided bone meal or oyster shell materials and the like.
- the calcium-containing material is preferably very finely divided so as not to impart any unnecessary chalkiness or other unpalatable characteristic to the confection. Finely ground calcium materials are commercially available, e.g., from Specialty Minerals, for use either in the antacid products or calcium supplement products.
- a calcium supplement product is prepared which incorporates 500 mg. Of bioassimable calcium, along with 200 I.U.'s of vitamin D3 into a single dosage form of the final product, which represents 50%> of the RDA of those nutrients.
- One of the advantages of the present invention is that a large proportion of the product can be displaced by a bulky material such as calcium sources. For example, up to about 25-35%) or even more of the total weight of the resulting product can be an added bioassimilable calcium source, without imparting undesirable taste or texture to the product.
- the product according to several embodiments of the invention exhibits improved taste and texture characteristics as compared with similar commercially- available products. "Improved" means that individual consumers rate the product overall to be superior when such characteristics as firmness, flavor, bite, sweetness, chewiness, melt characteristics, stickiness, juiciness, freedom from grit, and aftertaste are analyzed.
- a nutritional component can include ingredients which have vitamins and minerals required to maintain good health.
- a health bar product has been prepared in accordance with the present invention which includes a dry residue of whole vegetables and/or fruits. In fact, a health bar product has been made which includes the nutritional equivalent of up to five (5) times the U.S. recommended human adult dietary serving of vegetables and/or fruit by incorporation of the dry residue of such fruits and vegetables. Sources of minerals and fiber can also be included.
- a preferred embodiment of the nutritional form of the product contemplates treating ingredients having strong olfactory characteristics, e.g., flavor and aroma, to reduce such characteristics.
- the hydrobinding component e.g., the gelatin and/or gum
- aerating agents include egg whites and soy protein.
- Aerating agents are desirably added in amounts within the range of about 0 - 5%>, more desirably 0.1 - 3%.
- the products resulting from the present invention are unique, in part because they require no dehydration to produce, i.e., the product can be prepared without cooking.
- the hydrobound system of the present invention is a mass which has been hydrated by adding moisture to provide hydrocolloidal stability, but which does not have measurable free water, e.g., syneresis is substantially halted.
- Syneresis refers to as the phenomenon of separation of water from a mass of material as a distinct phase. When the moisture is so minimal in a mass or sufficiently bound to other components in the mass that phase separation does not occur, syneresis is stopped or halted. When syneresis occurs, free water is available within the system. Free water is generally unwanted in confectionery products of the type disclosed herein because of product deterioration and micro-organic growth. A correlation between free water and water activity has been made as a measure of product stability.
- Water activity is measured as the ratio between the vapor pressure of water in an enclosed chamber containing a food and the saturation vapor pressure of water at the temperature. Water activity indicates the degree to which water is bound and, subsequently, available to act as a solvent or participate in destructive chemical and microbiological reactions.
- Water activity is defined as:
- P eq is the partial vapor pressure of water in equilibrium with the solution and P 0 is the vapor pressure of pure water at the same temperature and pressure as the solution.
- P 0 is the vapor pressure of pure water at the same temperature and pressure as the solution.
- solutes tie up or bind water to varying degrees depending on the nature of the solute, such as its level of dissociation, extent and nature of intramolecular binding, solubility and chemical components.
- a portion of total water content present in foods is strongly bound to specific sites on the chemicals that comprise the foodstuff. These sites may include the hydroxyl groups of polysaccharides, the carboxyl, amino groups of proteins, and other polar sites that may hold water by hydrogen bonding or other strong chemical bonds.
- sites may include the hydroxyl groups of polysaccharides, the carboxyl, amino groups of proteins, and other polar sites that may hold water by hydrogen bonding or other strong chemical bonds.
- some of the water in foods is usually bound less firmly but is still not available as a solvent for various water-soluble food component.
- water activity is low when water is tightly bound to surface polar sites through chemisorption.
- the sites can include hydroxyl groups of hydrophilic material which are effective in controlling water activity.
- water activity is significantly lower than water activity of similar products found in the candy bar industry.
- candy bars usually have a water activity of 62%> - 68%> equilibrium relative humidity (ERH).
- ERH equilibrium relative humidity
- the confectionery product of the invention has at most only about a 60% ERH, and is preferably not greater than about 55% ERH.
- Another measure of free water in foodstuffs can be provided by the amount of biological growth within the composition.
- the biological activity is less than about 100 ppm, preferably less than about 25 ppm, and most preferably less than 10 ppm.
- Another distinctive feature of the present invention is the ability to reduce fat and calories in confectionery products.
- a confectionery nougat product can be made which has little or no fat content.
- This product qualifies under industry standards to be referred to as Reduced Fat (which means the fat content is reduced by 1/3) and as Low Fat (which means the fat content is reduced by 50%).
- at least some of the components useful according to the invention can be advantageously provided in the form of a shearform matrix, as that term is defined hereunder, as shearform matrix materials can exhibit significantly enhanced wettability because of a randomized structure resulting from flash-flow processing or shear mixing.
- shearform matrix refers to the product prepared by a method of flash-flow processing, a method which mixes and conditions ingredients for intimate contacting and enhanced hydration.
- One embodiment of the present invention may also include pre-flash-flow processing of certain ingredients prior to combining with other ingredients as set forth hereinabove.
- Pre-flash-flow processing is simply flash-flow processing of the ingredients which comprise either the hydrobinding component or the saccharide-based component.
- a saccharide material e.g., polydextrose
- Flash-flow processing results in increased surface area and increased solubility of the ingredients subjected thereto, and contributes to actual binding of the ingredients to each other.
- the hydrobinding component is an ingredient which imbibes, delivers and maintains water in an amount sufficient to functionalize the resulting mass. The water which is hydrobound does not separate and become a separate phase.
- the hydrobinding component cooperates with other ingredients to deliver and maintain water sufficient to functionalize the mass of ingredients, including those ingredients which have been subjected to flash-flow processing.
- a hydrobinding component can be hydrated and mixed with the saccharide- based component (the latter being in the form of a shear form matrix as a result of pre- flash-flow processing, or as a result of low or high-shear mixing) to form a functionalized hydrobound confectionery mass.
- the hydrobinding component can itself, if desired, also be subjected to pre-flash-flow processing prior to hydration in order to enhance wettability. It is often preferred to include a saccharide material with the hydrobinding component when it is subjected to either flash-flow processing or shear mixing.
- Flash-flow processing can be advantageous in the present invention since it is useful for preparing ingredients to be easily and quickly hydrated.
- Another very important result of flash-flow processing is intimate mixing of the ingredients. Intimate mixing has traditionally been achieved by the use of water as a mixing medium. Flash-flow processing, however, intimately contacts ingredients and randomizes ingredient location and structure of the resulting matrix. Randomizing the structure can be thought of as opening the physical and/or chemical structure for hydration.
- flash-flow has become recognized in the art as referring to a process which uses conditions of temperature and force to transform a solid feedstock to a new solid having a different morphological and/or chemical structure. The term flash-flow is described in commonly-owned U.S.
- Flash-flow processing can be accomplished either by a flash-heat method or via the less preferred flash-shear method, as described further herein.
- the feedstock is heated sufficiently to create an internal flow condition, which permits internal movement of the feedstock at subparticle level, and to exit openings provided in the perimeter of a spinning head.
- the centrifugal force created in the spinning head flings the flowing feedstock material outwardly from the head so that it reforms with a changed structure.
- the force necessary to separate and discharge flowable feedstock is provided by centrifugal force and the force of the ambient atmosphere impinging on feedstock exiting the spinning head.
- One apparatus for implementing a flash-heat process is a cotton candy fabricating type machine, such as the Eocene-floss model 3017 manufactured by Gold Medal Products company of Cincinnati, Ohio. Other apparatus which provides similar forces and temperature gradient conditions can also be used.
- a spinning machine developed and patented by Fuisz Technologies Ltd. of Chantilly, VA and patented under US 4,458,823 may be especially preferred.
- shearform matrix is produced by raising the temperature of the feedstock, which includes a non-solubilized carrier such as a saccharide material, until the carrier undergoes internal flow upon application of a fluid shear force.
- the feedstock is advanced and ejected while in internal flow condition, and subjected to disruptive fluid shear force to form multiple parts or masses which have a morphology different from that of the original feedstock.
- the flash-shear process can be carried out in an apparatus which has means for increasing the temperature of a non-solubilized feedstock and means for simultaneously advancing it for ejection.
- a multiple heating zone twin screw extruder can be used for increasing the temperature of the non-solubilized feedstock.
- a second element of the apparatus is an ejector which reduces the feedstock to a condition for shearing.
- the ejector is in fluid communication with the means for increasing the temperature and is arranged at a point to receive the feedstock while it is in internal flow condition. See commonly-owned U.S. Patent No. 5,380,473, issued on January 10, 1995 and entitled Process for Making Shear-Form Matrix.
- flash-heat appears to be much more readily adaptable to the process of the invention. However, those skilled in the art may find that flash-shear methodology can be adjusted to their particular needs.
- the time during which the feedstock material is subjected to elevated temperature is very short.
- the feedstock is subjected to elevated temperature usually for only tenths of a second, and in the flash-shear method the feedstock is subjected to elevated temperatures for a time on the order of seconds.
- the saccharide-based component feedstock for producing a shearform matrix includes a carrier material.
- the carrier material can be selected from material which is capable of undergoing both physical and/or chemical change associated with flash-flow processing.
- Materials which can be used as carrier materials in the feedstock include, for example, saccharide ingredients such as sucrose, corn syrup solids, polydextrose, and mixtures thereof.
- Sugars can also be used as an ingredient in the feedstock.
- Sugars are those substances which are based on simple crystalline mono- and di-saccharide structures, i.e., based on C 5 (pentose) and C 6 (hexose) sugar structures.
- Sugars include sucrose, fructose, lactose, maltose, etc., and sugar alcohols such as sorbitol, mannitol, maltitol, etc.
- compositions which can be incorporated into the feedstock to enhance the shearform matrix include, for example, flavors, sweeteners, colorants, surfactants or emulsifiers, and oleaginous materials such as fats and oils.
- Any of the adjunct materials described herein above can be included in the preparation of a suitable shearform matrix. It has now been further discovered that while preparation of a shearform matrix as a result of flash-flow processing as described above may often be desirable, the same attributes in the final product, e.g. intimate mixing, can also be attained by shear mixing, preferably high shear mixing, of the components making up the aforesaid feedstock prior to combining the thus prepared feedstock with the hydrobinding component, e.g. gum or gelatin.
- the hydrobinding component e.g. gum or gelatin.
- a combination of flash-flow process and shear mixing may be advantageously utilized to produce the product of the invention.
- certain ingredients making up the saccharide-based feedstock may be subjected to flash-flow procedures (such as pre-flash-flow processing) in order to combine them. Once combined, then the feedstock can then be shear mixed with the hydrobinding component to produce the food and/or drug delivery system of the invention.
- An especially preferred high-shear mixer is known as a Littleford FKM 1200.
- This device provides high shear mixing by proximal shearing blades which are at right angles to one another.
- the shearing blades consist of "plowers” and choppers, both of which are utilized for high shear mixing action. While not wishing to be bound by any particular theory, it is believed that high shear action provides both mixing and heating at the localized points of blade contact with the mix ingredients, thereby resulting in excellent dispersibility without the undesired effects of lumping etc.
- Other high shear mixers (with one or more mixing blades), currently available or yet to be developed, are also contemplated by the method of the invention.
- the high shear mixer can be further equipped with a jacket heater to provide the benefits of additional warming.
- a preferred temperature range is from about 30 degrees C to about 60 degrees C, more desirably within the range of about 30 degrees to about 45 degrees C.
- a preferred procedure for high shear mixing is as follows: The jacket heater on the high shear mixer is first activated and allowed to warm to a temperature of about 40 degrees C. Next, the saccharide-based component and other dry ingredients, e.g. calcium carbonate, are fed through the open hopper and allowed to mix using the plowers. For an 18 pound mixture, for example, the device is first run for about 2 minutes. Any added fat, along with emulsifiers, and the liquid-based hydrobinding component (together with any flavorings, sweeteners and coloring) are then fed into the mixer, and the choppers or high shear blades are activated to further complete the mixing.
- the saccharide-based component and other dry ingredients e.g. calcium carbonate
- the jacket temperature may be increased to within the range of about 50-60 degrees C, preferably about 58-60 degrees to assist in the mixing, especially if fat is present in the mixture.
- the mixer is then run for about 5-10 minutes more, perhaps longer, to complete the mixing of the saccharide-based component and the hydrobinding component. Once mixing is complete, the entire matrix is then emptied into an appropriate container for slicing, sorting and shipping etc., e.g. is extruded and cut into dosage size pieces.
- a low shear mixing apparatus can also provide the product of the invention.
- a Sigma mixer and/or Hobart industrial paddle mixer may be suitable.
- the dry ingredients saccharide-based component and any additional materials
- the liquid ingredients hydrobinding components
- the dry ingredients are mixed in a Hobart mixer, and then added to the Sigma mixer with the dry ingredients. The whole mixture is then run in the Sigma mixer for about 3 minutes. Variations of the foregoing process are certainly within the scope of the invention, depending upon the characteristics of the individual ingredients, and the attributes desired within the final product.
- Another method of formulating the product of the invention utilizes both highland low-shear mixing apparatus. Dry ingredients such as corn syrup solids and sucrose (polysaccharide component) are first mixed together with other dry ingredients, e.g. calcium carbonate, as well as any fat-based component and any emulsifier(s), in a high shear mixer, preferably a Littleford FKM 1200, according to the procedure described above (plowers first, followed by shearing blades for about 5-10 minutes). Next, in a low shear mixer (e.g. Hamilton) the liquid ingredients, i.e., the hydrobinding component along with any sweeteners, flavorings, colors and if desired, vitamin D3 formulation dissolved in corn syrup, are mixed together for a few minutes.
- a high shear mixer e.g. Hamilton
- This resulting mixture is then added to the dry mix (which has now been transferred from the high shear mixer to another low shear mixer, e.g. Guittard). All ingredients are then mixed in this second low shear mixer for a few more minutes ( ⁇ 3 minutes), with the resulting mass then sent through an extruder for final processing such as slicing, sorting and shipping, etc.
- another low shear mixer e.g. Guittard
- the polysaccharide component along with the calcium carbonate and vitamin D3 are first mixed together in the high shear mixer.
- the resulting formulation is then added to the extruder together with the liquid ingredients for final mixing, and extrusion.
- the extruder would of course be of the type which is adapted to receive the liquid components.
- a series of confectionery-type masses was prepared according to the invention, for the delivery of a bioassimilable calcium source, in this case powdered calcium carbonate.
- the hydrobinding material was selected to be a mixture of medium weight gelatin (250 Bloom) and gum arabic.
- the saccharide-based material was selected to be sucrose (6X) or a mixture of sucrose and corn syrup solids. The components and the preparation conditions for these batches are given below in Table 1.
- a nougat composition was prepared without cooking or removal of water.
- the ingredients set forth in Table 2-A were mixed using a high shear mixer for 5 min at 40-50 cycles/min.
- This mixed composition was then mixed with colors and flavors in a Sigma mixer, again for 5 min at 40-50 cycles/min.
- the resulting mass was removed from the mixer, and rolled to the desired thickness, e.g., about 3 cm. This product was completely homogeneous, and had a chewy texture.
- Example 2 Another chewy nougat product was made using the same materials and proportions described in Example 1 , except that the components described there as being part of the primary mixture were processed together using flash flow processing (described in the specification as pre-flash flow processing) to provide a shearform matrix. This shearform matrix was then added to the coloring and flavoring, and used as described. Again, the resulting product was homogenous, chewy in texture, and flavorful.
- flash flow processing described in the specification as pre-flash flow processing
- the primary mixture prepared according to the method described in Example 1 was used to make a gelatin-free confection product suitable for use as a calcium supplement.
- the primary mixture, together with flavorant, colorant, and an artificial sweetener, were mixed together in a kettle for 5 min. Potassium citrate was then dissolved in water with warming to ⁇ 85 degrees C.
- the hot solution was immediately added to a mixture of locust bean gum, carrageenan, and glycerin in a beaker and mixed, to provide a warm paste. This paste was then added to the pre-mixed primary mixture, and mixed for about 5 min.
- the final temperature of the resulting nougat was -50 degrees C.
- the amounts of the ingredients in this chewy nougat confection are given in Table 3.
- This pleasant-tasting and chewy gelatin-free nougat material was cut into approximately 5.3 g pieces, each of which provided 500 mg of calcium.
- Example 1 An additional chewy nougat product was made according to the method set forth in Example 1 which delivered 500 mg of calcium and 200 I.U.'s of vitamin D3 in both chocolate and mint flavors as follows:
- Vitamin D3 was dissolved in a small amount of corn syrup and added with the liquid components. **Flavorings included the following: Peppermint, Spearmint, Vanilla, Cream, Chocolate, and Cocoa Powder.
- a mint-flavored chewy nougat formulation according to the foregoing embodiment was compared with three leading commercially-available (store bought) calcium supplement preparations in a random taste test.
- 100 consumers between the ages of 30 - 70 were chosen to participate and evaluate a total of four products according to the following criteria on a scale of 1 - 9: bite, firmness, flavor, sweetness, chewiness, melt, stickiness, juiciness, grit, aftertaste and coolness (the higher the score, the more positively the consumer judged each attribute).
- Each consumer was given an identical bite-size serving of each one of the four products in the same order (with crackers and a sip of water in between each serving). Consumers were not told the source or identity of the products they were evaluating, other than that each was a calcium supplement. Results are indicated below:
- a health bar was prepared containing powdered dried whole carrot and zucchini as using low shear mixing as follows: In a Hobart mixer, ingredients 1 - 11 were mixed for 5 minutes at Speeds 1 and 2. Preblended mixes of ingredients 12 and 13 were then mixed in for 1 minute, and ingredients 14 and 15 were then added to the resulting mix and further blended for 1 minute. Ingredients 16 and 17 were next added and mixed for 1 minute. The resulting mass was removed from the mixer, laid down on a flat surface and rolled to a fairly uniform V. inch thickness. The mixture was allowed to set at room temperature, and then cut into single serving bars. (If desired, the resulting bars can then be coated with a commercial yogurt preparation.)
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Abstract
La présente invention concerne un nouveau procédé de fabrication d'une masse de confiserie, telle qu'un nougat, par une hydratation suffisante pour former la masse sans cuisson et faire évaporer l'humidité. L'invention concerne également un produit préparé par hydratation positive d'un mélange d'ingrédients de confiserie comprenant un composant de liaison en milieu aqueux et une matière à base de saccharide.
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
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US88185397A | 1997-06-24 | 1997-06-24 | |
US881853 | 1997-06-24 | ||
PCT/US1998/010869 WO1998058549A1 (fr) | 1997-06-24 | 1998-05-26 | Procede de preparation de confiserie par hydratation positive et produit obtenu |
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EP0989807A1 true EP0989807A1 (fr) | 2000-04-05 |
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EP98924947A Withdrawn EP0989807A1 (fr) | 1997-06-24 | 1998-05-26 | Procede de preparation de confiserie par hydratation positive et produit obtenu |
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Country | Link |
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EP (1) | EP0989807A1 (fr) |
JP (1) | JP2002509434A (fr) |
AU (1) | AU7700198A (fr) |
CA (1) | CA2295238A1 (fr) |
WO (1) | WO1998058549A1 (fr) |
Families Citing this family (8)
Publication number | Priority date | Publication date | Assignee | Title |
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US6337082B1 (en) * | 1991-10-25 | 2002-01-08 | Biovail Tech Ltd | Saccharide-based matrix |
US6482465B1 (en) * | 1997-06-24 | 2002-11-19 | Biovail Technologies Ltd. | Positive hydration method of preparing confectionery and product therefrom |
US6517886B1 (en) * | 1997-06-24 | 2003-02-11 | Biovail Corporation International | Positive hydration method of preparing confectionery and the resulting product |
US6673380B2 (en) | 1998-11-17 | 2004-01-06 | Mcneil-Ppc, Inc. | Fortified confectionery delivery systems and methods of preparation thereof |
WO1999048379A1 (fr) * | 1998-03-23 | 1999-09-30 | Fuisz Technologies Ltd. | Preparation de nougat mou a base de calcium avec magnesium |
WO2000001245A2 (fr) * | 1998-07-07 | 2000-01-13 | Fuisz Technologies Ltd. | Formulation de confiserie a macher multivitaminee |
US6824808B2 (en) * | 2001-05-09 | 2004-11-30 | Nestec S.A. | Chewy candy analogue, method of making, and composite ice confections containing same |
JP5169882B2 (ja) * | 2009-01-30 | 2013-03-27 | ユーハ味覚糖株式会社 | ノンシュガーグミキャンディおよびその製造方法 |
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US4444799A (en) * | 1981-08-18 | 1984-04-24 | Nabisco, Inc. | Method and composition for producing soft edible baked products and an edible firm gel for use therein |
US5456932A (en) * | 1987-04-20 | 1995-10-10 | Fuisz Technologies Ltd. | Method of converting a feedstock to a shearform product and product thereof |
US5654003A (en) * | 1992-03-05 | 1997-08-05 | Fuisz Technologies Ltd. | Process and apparatus for making tablets and tablets made therefrom |
US5518730A (en) * | 1992-06-03 | 1996-05-21 | Fuisz Technologies Ltd. | Biodegradable controlled release flash flow melt-spun delivery system |
US5380473A (en) * | 1992-10-23 | 1995-01-10 | Fuisz Technologies Ltd. | Process for making shearform matrix |
US5534286A (en) * | 1994-06-01 | 1996-07-09 | Monsanto Company | No-fat gellan gum spread |
US5587198A (en) * | 1995-05-31 | 1996-12-24 | Fuisz Technologies Ltd. | Positive hydration method of preparing confectionery and product therefrom |
TW442287B (en) * | 1995-06-13 | 2001-06-23 | American Home Produits Corp | Organoleptically acceptable oral pharmaceutical composition comprising the S(+)1,8-diethyl-1-1,3,4,9-tetrahydropyrano[3,4-b] indole-1-acetic acid (Etodolac) |
-
1998
- 1998-05-26 CA CA002295238A patent/CA2295238A1/fr not_active Abandoned
- 1998-05-26 AU AU77001/98A patent/AU7700198A/en not_active Abandoned
- 1998-05-26 EP EP98924947A patent/EP0989807A1/fr not_active Withdrawn
- 1998-05-26 JP JP50444099A patent/JP2002509434A/ja active Pending
- 1998-05-26 WO PCT/US1998/010869 patent/WO1998058549A1/fr not_active Application Discontinuation
Non-Patent Citations (1)
Title |
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See references of WO9858549A1 * |
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JP2002509434A (ja) | 2002-03-26 |
WO1998058549A1 (fr) | 1998-12-30 |
AU7700198A (en) | 1999-01-04 |
CA2295238A1 (fr) | 1998-12-30 |
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