Rapidly disintegrating effervescent tablets and methods of making the same

Information

  • Patent Grant
  • 10912733
  • Patent Number
    10,912,733
  • Date Filed
    Wednesday, April 3, 2019
    5 years ago
  • Date Issued
    Tuesday, February 9, 2021
    3 years ago
Abstract
An effervescent tablet that exhibits rapid disintegration is disclosed. The effervescent tablet includes an effervescent agent that includes an acid and a base, a directly compressible sugar binder, a sweetener that includes at least one of Stevia and Monk fruit, a flavor agent that includes a gum Arabic carrier, and a lubricant derived from rice hulls.
Description
BACKGROUND

The invention is directed to decreasing the disintegration time of tableted effervescent compositions.


Formulating a commercially viable effervescent tablet is more art than science. Whether components can be formulated into an effervescent tablet that disintegrates in water in a relatively short period of time and exhibits sufficient integrity as a tablet that it can be manufactured, packaged and shipped without falling apart or exhibiting die wall etching, capping, lamination or picking is often unpredictable. The components of an effervescent composition impact the ability of the composition to form a tablet, tablet hardness, tablet disintegration time in water, and the clarity of the resulting solution once the tablet has disintegrated. The components of an effervescent composition also impact the taste of a beverage made therefrom, which is relevant to the consumer when the effervescent composition intended to be used to form a beverage.


A common ingredient in effervescent tablets is a binder. A variety of binders have been used in tableted effervescent compositions including compressible sugar alcohols (e.g., sorbitol), compressible dextrose, and compressible sucrose. Compressible sugars are prepared in a variety of ways including co-crystallizing and co-precipitating sugar with an excipient such as maltodextrin, maltose, maltriose, starch, starch hydrolysates, gelatin, polysaccharides, corn syrup, and combinations thereof.


Many effervescent tablet compositions also include a sweetener. Recently consumers have had a preference for the sweetener Stevia due to the fact that it is found in nature, is derived from natural origins, and is low in calories. Effervescent tablets formulated with Stevia exhibit a significant increase in disintegration time relative to tablets formulated with artificial low-calorie sweeteners such as sucralose or acesulfame potassium. It is difficult to formulate an effervescent tablet that includes Stevia and disintegrates rapidly.


Some effervescent tablets also include a lubricant. However, effervescent compositions are inherently difficult to lubricate due to the nature of the raw materials used in the formulations and the desire to achieve a tablet that disintegrates rapidly in water and forms a clear solution. In order for many substances to be effective as a lubricant, they must be present in the tablet in very high concentrations. These high concentrations cause the lubricant to significantly inhibit the tablet's ability to disintegrate. In addition, many lubricants are not water soluble. Magnesium stearate, for example, is not water soluble, can impede disintegration in water, and can produce a cloudy aqueous liquid.


There is a need for improving the disintegration time of effervescent tablets that include natural sweeteners.


SUMMARY

In one aspect, the invention features an effervescent tablet that includes an effervescent agent comprising an acid and a base, a sweetener comprising Stevia, Monk fruit, or a combination thereof, a first directly compressible sugar binder, a flavor agent comprising gum Arabic, and a lubricant derived from rice hulls, the effervescent tablet having a weight of at least 4 grams and a hardness of at least 5 kiloponds, and exhibiting a disintegration time of no greater than 4 minutes and 20 seconds when tested according to the Disintegration Time Test Method.


In one embodiment, the effervescent tablet includes at least 1.5% by weight of a flavor agent comprising gum Arabic. In another embodiment, the effervescent tablet includes at least 2% by weight of a flavor agent comprising gum Arabic. In other embodiments, the effervescent is free of flavor agents that are free of gum Arabic.


In some embodiments, the lubricant is a multi-component integral lubricant that comprises rice hull particles, gum Arabic, sunflower oil, and at least one extract of rice. In another embodiment, the tablet includes from 0.8% by weight to 4% by weight of the lubricant derived from rice hulls. In one embodiment, the tablet includes from 0.8% by weight to 1.5% by weight of the lubricant derived from rice hulls.


In other embodiments, the directly compressible sugar binder is selected from the group consisting of directly compressible dextrose, directly compressible sucrose, and combinations. In some embodiments, the directly compressible sugar binder includes dextrose. In another embodiment, the directly compressible sugar binder comprises a mixture of dextrose and a polysaccharide.


In another embodiment, the effervescent tablet disintegrates in 25° C. water in no greater than 4 minutes. In another embodiment, the effervescent tablet disintegrates in 25° C. water in no greater than 3.5 minutes.


In some embodiments, the effervescent tablet includes at least 20% by weight of the effervescent agent, and from 20% by weight to 55% by weight of the directly compressible sugar binder. In other embodiments, the effervescent tablet includes from 0.4% by weight to 2% by weight of the sweetener.


In one embodiment, the lubricant is a multi-component integral lubricant that includes rice hull particles, gum Arabic, sunflower oil, and at least one extract of rice, and the effervescent tablet includes at least 20% by weight of the effervescent agent, and from 20% by weight to 55% by weight of the directly compressible sugar binder. In other embodiments, the lubricant is a multi-component integral lubricant that includes rice hull particles, gum Arabic, sunflower oil, and at least one extract of rice, and the effervescent tablet includes at least 20% by weight of the effervescent agent, from 20% by weight to 55% by weight of the directly compressible sugar binder, and from 0.4% by weight to 2% by weight of the sweetener.


In some embodiments, the second lubricant is a multi-component integral lubricant that includes rice hull particles, gum Arabic, sunflower oil, and at least one extract of rice, and the effervescent tablet includes at least 20% by weight of the effervescent agent, and from 20% by weight to 55% by weight of the directly compressible sugar binder. In other embodiments, the lubricant is a multi-component integral lubricant that includes rice hull particles, gum Arabic, sunflower oil, and at least one extract of rice, and the effervescent tablet includes at least 20% by weight of the effervescent agent, from 20% by weight to 55% by weight of the directly compressible sugar binder, from 0.4% by weight to 2% by weight of the sweetener, and at least 1.5% by weight of a flavor agent that includes gum Arabic, and optionally is free of flavor agents that are free of gum Arabic.


In other embodiments, the lubricant is a multi-component integral lubricant that includes rice hull particles, gum Arabic, sunflower oil, and at least one extract of rice, and the effervescent tablet includes at least 20% by weight of the effervescent agent, and from 20% by weight to 55% by weight of the directly compressible sugar binder. In other embodiments, the lubricant is a multi-component integral lubricant that includes rice hull particles, gum Arabic, sunflower oil, and at least one extract of rice, and the effervescent tablet includes at least 20% by weight of the effervescent agent, from 20% by weight to 55% by weight of the directly compressible sugar binder, from 0.4% by weight to 2% by weight of the sweetener, and is free of flavor agents that are free of gum Arabic.


In another embodiment, the effervescent tablet further includes oil.


In some embodiments, the effervescent tablet has a hardness of at least 6 kiloponds.


In another aspect, the invention features a method of making an effervescent tablet, the method that includes forming an effervescent composition by combining ingredients with mixing, the ingredients that include an effervescent agent that includes an acid and a base, a sweetener that includes Stevia, Monk fruit, or a combination thereof, a first directly compressible sugar binder, a flavor agent that includes gum Arabic, a lubricant derived from rice hulls, and tableting the effervescent composition on a tableting press to form an effervescent tablet that has a mass of at least 4 grams and a hardness of at least 5 kiloponds and that disintegrates in 25° C. water in less than 5 minutes. In one embodiment of the method the lubricant is a multi-component integral lubricant that includes rice hull particles, gum Arabic, sunflower oil and at least one extract of rice. In another embodiment of the method, the resulting tablet includes at least 1.5% by weight of a flavor agent that includes gum Arabic. In another embodiment of the method, the resulting tablet includes at least 2% by weight of a flavor agent that includes gum Arabic. In other embodiments of the method, the resulting tablet is free of flavor agents that are free of gum Arabic.


The invention features an effervescent composition that exhibits good tableting properties and, when formed into an effervescent tablet, disintegrates rapidly in water.


Other features and advantages will be apparent from the following description of the preferred embodiments and from the claims.


GLOSSARY

In reference to the invention, these terms have the meanings set forth below:


The term “multi-component integral lubricant” means a lubricant that includes at least two components intimately associated with one another such that they form a single substance.


The term “directly compressible” means the ability to be compressed into a compact form in a defined volume by a compression force, to remain in the compact form once the compression force has been removed, and to remain in the intact compact form when removed from the defined volume.


The term “Stevia” means a sweetener derived from the plant species Stevia rebaudiana.


The term “Monk Fruit” means a sweetener derived from the fruit of the plant species Siraitia grosvenorii.


The term “botanical oil” means an oil derived from a part of a plant.







DETAILED DESCRIPTION

The method of making an effervescent tablet includes combining an effervescent agent, a first directly compressible sugar binder, a natural sweetener such as Stevia or Monk fruit, a flavor agent that includes a gum Arabic carrier to form an effervescent composition, and a lubricant derived from rice hulls, and tableting the effervescent composition. The resulting effervescent composition can be tableted to a hardness of at least 3 kiloponds (Kp), at least 4 Kp, at least 5 Kp, at least 6 Kp, at least 7 Kp, or even at least 8 Kp and the resulting tablets can disintegrate in water having a temperature of 72° F. (degrees Fahrenheit) (about 25° C. (degrees Celsius)) in less than 6 minutes, less than 5 minutes, less than 5 minutes 18 seconds, less than 4 minutes 20 seconds, less than 4 minutes 10 seconds, less than 4 minutes, less than 220 seconds, less than 200 seconds, less than 180 seconds, or even no greater than 150 seconds.


The directly compressible sugar binder includes a sugar (e.g., a monosaccharide (e.g., dextrose and fructose), a disaccharide (e.g., sucrose), and mixtures thereof) and an excipient integrally associated with the sugar. The directly compressible sugar binder optionally includes moisture (e.g., a moisture content of from 0% by weight to 10% by weight, from 0.1% by weight to 9% by weight, 7% by weight to 9% by weight, or even less than 1% by weight moisture). The term “integrally associated with” in reference to the compressible sugar binder means that the sugar and the excipient are intimately associated with one another such that they form a single substance. Examples of suitable excipients include maltodextrin, maltose, maltriose, starch, a starch hydrolysate, microcrystalline cellulose, invert sugar, corn syrup solids, and combinations thereof. The sugar of the directly compressible sugar binder has been altered by the manufacturer of the compressible sugar to render it compressible. Such processes include co-crystallizing the sugar with excipients, coprecipitating the sugar with excipients, and co-granulating the sugar with excipients. These processes occur at the manufacturer of the compressible sugar binder and the excipients are present in the directly compressible sugar binder prior to its addition to the other components of the effervescent composition. The directly compressible sugar binder includes from 0.5% by weight to 10% by weight, from 1% by weight to 7% by weight, 1.5% by weight to 5% by weight, or even from 1.5% by weight to 4% by weight excipient.


Useful commercially available directly compressible sugar binders include, e.g., CANTAB dextrose from Stauber (Fullerton, Calif.), DI-PAC direct compacting and tableting sucrose from Domino Specialty Ingredients (West Palm Beach, Florida), which includes 97% sucrose and 3% modified dextrin, and the compressible sugar binders commercially available under the EZ-PRESS series of trade designations from Watson Inc. (West Haven, Conn.) including, e.g., EZ-PRESS Sucrose DC sucrose having a mean particle size of 250 microns (μm), a bulk density of 0.56 grams/cubic centimeters (g/cm3), a tapped bulk density of 0.69 g/cm3, and 0.4% moisture, EZ-PRESS Dextrose DC having a mean particle size of 220 microns, a bulk density of 0.52 g/cm3, a tapped bulk density of 0.62 g/cm3, and 8.7% moisture, EZ-PRESS Fructose DC having a mean particle size of 340 μm, a bulk density of 0.56 g/cm3, a tapped bulk density of 0.65 g/cm3, and 0.8% moisture, EZ-PRESS Mannitol DC having a mean particle size of 270 microns, a bulk density of 0.48 g/cm3, a tapped bulk density of 0.59 g/cm3, and 0.5% moisture, EZ-PRESS Sorbitol DC having a mean particle size of 260 μm, a bulk density of 0.47 g/cm3, a tapped bulk density of 0.57 g/cm3, and 0.4% moisture, and EZ-PRESS Xylitol DC having a bulk density of 0.54 g/cm3, a tapped bulk density of 0.64 g/cm3, and 0.2% moisture.


The effervescent composition preferably includes at least 20% by weight, at least 22% by weight, no greater than 55% by weight, no greater than 50% by weight, from 20% by weight to 50% by weight, from 22% by weight to 47% by weight, or even from 25% by weight to 35% by weight of the directly compressible sugar binder.


For ease of discussion, throughout this specification the % by weight values provided for each ingredient present in the effervescent composition are provided with respect to the effervescent composition; it is to be understood these same values are also suitable for the effervescent tablet.


The effervescent agent of the effervescent composition includes an acid and a base. The effervescent agent is activated when contacted with an aqueous liquid, e.g., when the effervescent agent is placed in a glass of water. The water liberates the acid and base and enables the acid and base to react with each other to produce a gas (e.g., carbon dioxide). The effervescent composition preferably includes at least 30% by weight, at least 35% by weight, at least 40% by weight, from 35% by weight to 75% by weight, or even from 40% by weight to 70% by weight effervescent agent.


Acids suitable for use in the effervescent agent include, e.g., citric acid, aspartic acid, malic acid, adipic acid, tartaric acid, fumaric acid, succinic acid, sodium acid pyrophosphate, lactic acid, hexamic acid, amino acid hydrochlorides, and acid salts and acid anhydrides thereof, and mixtures thereof. Preferably the effervescent tablet includes at least 10% by weight, at least 15% by weight, at least 20% by weight, from 20% by weight to 50% by weight, from 20% by weight to 45% by weight, or even from 25% by weight to 45% by weight acid.


The base of the effervescent agent preferably is capable of generating a gas such as carbon dioxide in the presence of an acid source and water. Examples of suitable bases include potassium bicarbonate, sodium bicarbonate, sodium carbonate, sodium sesquicarbonate, potassium carbonate, calcium carbonate, magnesium carbonate, zinc carbonate, and mixtures thereof. Particularly useful bases include potassium carbonates, sodium carbonates, and bicarbonates thereof, and combinations thereof. The effervescent composition includes at least 10% by weight, at least 12% by weight, at least 15% by weight, from 10% by weight to 35% by weight, from 12% by weight to 30% by weight, or even from 15% by weight to 30% by weight base.


The effervescent composition includes at least one natural sweetener such as Stevia or Monk fruit. As used herein a “sweetener” is a compound other than the crystalline sugar binders set forth above. Useful sweeteners include, e.g., natural sweeteners (e.g., Stevia, Monk fruit, and combinations thereof), invert sugar, ribose, isomalt, tagatose, sucralose, and mixtures thereof, saccharin and its various salts (e.g., sodium and calcium salt of saccharin), cyclamic acid and its various salts, acesulfame potassium, dihydrochalcone, glycyrrhizin, and sugar alcohols including, e.g., erythritol, xylitol, sorbitol, sorbitol syrup, lactitol, maltitol, and mannitol, and combinations thereof. When present, the effervescent composition preferably includes at least 0.8% by weight, at least 1% by weight, at least 2% by weight, at least 4% by weight, less than 10% by weight, less than 8% by weight, less than 5% by weight, from 1% by weight to 10% by weight, from 2% by weight to 8% by weight, or even from 3% by weight to 5% by weight sweetener.


The effervescent composition preferably includes from 0% by weight to 2% by weight, 0.1% by weight to 2% by weight, from 0.1% by weight to 1.5% by weight, or even from 0.2% by weight to 1% by weight of a natural sweetener such as Stevia, Monk fruit, or a combination thereof.


The effervescent composition also includes a flavor agent that includes a flavor integrally associated with a gum Arabic carrier (gum Arabic is also known as Acacia gum). The term “integrally associated with” means that the flavor and the carrier are intimately associated with one another such that they form a single substance. Useful flavor agents exist in a variety of forms including, e.g., solids (e.g., powders, granulations, spherical and non-spherical particles, nano-particles, and combinations thereof), liquids (e.g., oils), pastes, and combinations thereof. The flavor agent can be used to impart any desired flavor to the effervescent composition including, e.g., lemon (e.g., lemonade), lime, orange, mango-orange, citrus orange, grape, tropical punch, citrus lime, citrus fruit, grapefruit, apple, pear, peach, grape, strawberry, raspberry, cherry, plum, pineapple, apricot, guava, mango, papaya, watermelon, musk melon, pineapple, grapefruit, blueberry, pomegranate, blackberry, tri-berry, ginger, tangerine, cantaloupe, tea, mint, cocoa, vanilla, almond, coffee, and combinations thereof (e.g., multiple berry flavors, watermelon-lemonade, strawberry-lemonade, lemon-lime, cherry-limeade, and combinations thereof).


Useful flavors include natural and artificial (i.e., synthetic) flavors including, e.g., oil-based flavors (e.g., flavors based on natural oils, synthetic oils, and combinations thereof), aromatics, oleoresins, fatty acids, small molecules, alcohols, aldehydes, ketones, esters (e.g., alkadienyl esters, alkyl esters, and alkenyl esters), ethers, acetals, ketals, nitriles, aliphatic carbocyclic compounds, heterocyclic compounds, extracts derived from plants, leaves, flowers, fruits, and stems, organic solvent-based flavors, and combinations thereof.


Although at least one of the flavor agents present in the effervescent composition includes a flavor integrally associated with a gum Arabic carrier, the flavor agent optionally includes at least one additional integrally associated carrier other than gum Arabic. In addition or alternatively, the composition can optionally include at least one other flavor agent that includes a flavor and a carrier other than gum Arabic. Examples of other suitable carriers include, e.g., sucrose, dextrose, lactose, fructose, maltose, ribose, dextrose, arabinose, pentose, xylose, galactose, and isomalt (e.g., a mixture of glucopyranosylmannitol dihydrate and glucopyranosylsorbitol), and combinations thereof, sugar alcohols (e.g., sorbitol, mannitol, xylitol, lactitol, maltitol, and pentatol, and combinations thereof), casein, starches (e.g., natural and modified starches (e.g., octenyl succinate starch)), hydrolyzed starches (e.g., maltodextrin), dextrin (e.g., water soluble and partially water soluble dextrins), cyclodextrin, and emulsifying polymers, pectins, xanthans, alginates, hydrocolloids, cellulose (e.g., carboxymethyl cellulose, methyl cellulose, ethyl cellulose, hydroxyethylcellulose, and hydroxypropyl cellulose), corn syrup (e.g., corn syrup solids), silicon dioxide, soy lecithin, modified starch (e.g., sodium starch octenyl succinates), proteins (e.g., whey protein), monosaccharides, disaccharides, trisaccharides, gelatin, agar, alginate, carrageenan, tragacanth, butylated hydroxyanisole, butylated hydroxytoluene, and combinations thereof.


The integral association of the flavor and the carrier can exist in a variety of forms including, e.g., flavor fully or partially encapsulated by the carrier, flavor plated on the carrier, flavor in a uniform mixture with the carrier, and combinations thereof. The flavor and carrier become integrally associated with one another as a result of the process of making the flavor agent. Such processes include, e.g., plating, encapsulation (e.g., coacervation and complex coacervation techniques), emulsification, mixing, spray drying, granulating, agglomeration, extrusion, and combinations thereof.


A number of suitable flavor agents are commercially available including, e.g., PRINOVA flavors from Prinova Group LLC. (Carol Stream, Ill.), SIMPLY NATURAL flavors from Edgar Weber & Co. (Wheeling, Ill.), FONA flavors from Fona International Inc. (Geneva, Ill.), Symrise Inc. (Teterboro, N.J.), and from DRIZOOM flavors from Zoomessence (Hebron, Ky.).


The flavor agent can be present in the effervescent composition in any suitable amount. The effervescent composition preferably includes at least 0.1% by weight, at least 1% by weight, at least 1.5% by weight, at least 2% by weight, less than 6% by weight, less than 5% by weight, from 1% by weight to 6% by weight, from 1.5% by weight to 6% by weight, or even from 2% by weight to 5% by weight of a flavor agent that includes gum Arabic.


The effervescent composition optionally is free of a flavor agent that does not include gum Arabic (i.e., free of a flavor agent that is free of gum Arabic).


The lubricant is derived from rice hulls. The lubricant preferably is in the form of a free-flowing powder that includes particles derived from rice hull, which can be produced by any suitable process including, e.g., grinding rice hulls, crushing rice hulls, and combinations thereof. Useful lubricant include multi-component integral lubricant that include rice hull particles and a variety of components combined in the form of a single substance. Suitable components for the multi-component integral lubricant include, e.g., extracts of rice (e.g., lipids, proteins, complex carbohydrates, and combinations thereof), rice hull particles, gum Arabic, silica derived from rice (e.g., free flowing silica powder derived from rice), oil (e.g., sunflower oil, avocado oil, and combinations thereof), polysaccharide (e.g., starch, amylopectin, and combinations thereof), and combinations thereof. One particularly useful example of a multi-component integral lubricant is commercially available under the NUMAG trade designation from Ribus Inc. (St. Louis, Mo.) and includes an integral mixture of extracts of rice, ground rice hulls in the form of particles, gum Arabic and sunflower oil.


The effervescent composition preferably includes at least 0.1% by weight, at least 0.2% by weight, at least 0.5% by weight, from 0.1% by weight to 4% by weight, from 0.8% by weight to 4% by weight, from 0.8% by weight to 2% by weight, or even from 0.8% by weight to 1.5% by weight of a lubricant derived from rice hulls.


The effervescent composition also optionally includes oil (e.g., botanical oil, mineral oil, synthetic oil, or a combination thereof). Useful botanical oils include, e.g., avocado oil, wheat germ oil, coconut oil, an oil, safflower oil, sesame oil, sunflower oil, flax seed oil, canola oil, cotton seed oil, corn oil, palm oil, olive oil, and combinations thereof. The effervescent composition preferably includes less than 2% by weight, less than 1% by weight, less than 0.8% by weight, at least 0.1% by weight, at least 0.2% by weight, at least 0.3% by weight, at least 0.4% by weight, at least 0.5% by weight, at least 0.6% by weight, from 0.3% by weight to 1% by weight, from 0.3% by weight to 0.8% by weight, or even from 0.5% by weight to 0.8% by weight oil.


The effervescent composition optionally includes additional ingredients including, e.g., additional lubricants, additional binders, color agents, nutritional ingredients (e.g., nutritional supplements), surfactant, and combinations thereof.


The oils mentioned above can provide a lubricant function by enabling the effervescent composition to be tableted without sticking to the tablet press or creating other tableting problems. The composition can optionally include a variety of other lubricants including, e.g., water insoluble, water dispersible, and water soluble lubricants, and combinations thereof. Examples of useful water soluble lubricants include sodium benzoate, polyethylene glycol, L-leucine, adipic acid, and combinations thereof. Water insoluble lubricants include, e.g., animal fats, polyoxyethylene monostearate, talc, and combinations thereof. When a lubricant other than a lubricant derived from rice hulls is present in the effervescent composition, it preferably is present in an amount less than 2% by weight, less than 1% by weight, less than 0.8% by weight, from 0.05% by weight to 1% by weight, or even from 0.05% by weight to 0.8% by weight.


Other binders that can optionally be present as a secondary binders in the composition include, e.g., amorphous binders, agglomerated dextrose, starches, natural gums, cellulose gums, microcrystalline cellulose, methylcellulose, cellulose ethers, sodium carboxymethylcellulose, ethyl cellulose, gelatin, sorbitol, mannitol, polyethylene glycol, polyvinylpyrrolidone, pectins, alginates, polyacrylamides, polyvinyloxoazolidone, polyvinylalcohols, multi-component integral binders, non-compressible crystalline sugar binders, and mixtures thereof.


Suitable optional non-compressible crystalline sugar binders are monosaccharides or disaccharides or mixtures thereof that are in the form of crystals that include flat faces (i.e., facets) and sharp angles, are not directly compressible, and do not include an integral binder other than the monosaccharide or disaccharide. Suitable non-compressible crystalline sugar binders include monosaccharides, disaccharides, and mixtures thereof including, e.g., crystalline dextrose (e.g., dextrose monohydrate, and monohydrate α-dextrose), crystalline fructose, crystalline sucrose, and combinations thereof. Useful non-compressible crystalline sugar binders optionally include moisture and preferably include no greater than 11% by weight, no greater than 10% by weight, no greater than 9.5% by weight, from 0% by weight to 9.5% by weight, from 6.5% by weight to 9% by weight, or even from 7.5% by weight to 9% by weight moisture. Useful crystalline sugar binders are at least 95%, at least 96%, at least 97%, at least 98%, at least 99%, at least 99.5%, at least 99.7%, at least 99.8%, at least 99.9%, or even 100% pure crystalline sugar on a dry weight basis (dwb) based on the total weight of the solids in the crystalline sugar binder as supplied by the manufacturer. Suitable non-compressible crystalline sugar binders include less than 0.3% by weight, or are even free of, excipients including such excipients as maltodextrin, maltose, maltriose, starch, invert sugar, corn syrup, a starch hydrolysate, and microcrystalline cellulose. Suitable non-compressible crystalline sugar binder also are essentially free of, or even free of, co-crystallized excipients, coprecipitated excipients, and co-granulated excipients prior to its addition to the effervescent composition. Useful non-compressible crystalline sugar binders exhibit an average particle size of from 140 microns (μm) to 440 μm, from 200 μm to 400 μm, or even from 200 μm to 300 μm.


Useful commercially available non-compressible crystalline sugar binders include, e.g., organic crystalline sugar binders available from Ciranda, Inc. (Hudson, Wis.) including, e.g., ORGANIC CRYSTAL DEXTROGRAPE crystallized dextrose derived from organic grapes, ORGANIC CRYSTAL FRUCTOGRAPE crystallized fructose derived from organic grapes, and ORGANIC CRYSTAL SWEETGRAPE a mixture of crystallized fructose and crystallized dextrose derived from organic grapes, crystalline sugars available from Batory Foods including Velvet Baker's Special Cane Sugar (Chicago, Ill.), crystalline sucrose available from Domino Foods, Inc., (Baltimore, Md.), crystalline dextrose monohydrate available from Meelunie B.V. (The Netherlands), and ADM crystalline dextrose and crystalline sucrose available from Archer Daniels Midland Company (Chicago, Ill.).


When present, the effervescent composition includes from 0% by weight to no greater than 55% by weight, from 1% by weight to no greater than 50% by weight, from 1% by weight to no greater than 25% by weight, or even from 1% by weight to no greater than 35% by weight non-compressible crystalline sugar binder.


Useful color agents include, e.g., food, drug and cosmetic (FD&C) colors including, e.g., dyes, pigments, lakes, natural colorants, and derived colorants. Useful naturally derived color agents include color agents derived from beet root, yellow beet root, riboflavin, spirulina, vegetable juice color agent, and combinations thereof. Useful lakes include dyes absorbed on aluminum hydroxide and other suitable carriers. Examples of suitable colors include FD&C Red No. 3, FD&C Red No. 40, FD&C Blue No. 1, FD&C Blue No. 2, FD&C Yellow No. 5, FD&C Yellow No. 6, FD&C Green No. 3, and combinations thereof.


The color agent optionally includes a carrier integrally associated with the coloring component such that the color component is fully or partially encapsulated by the carrier, plated on the carrier, in a uniform mixture with the carrier, or a combination thereof. Useful carriers include, e.g., sucrose, dextrose, lactose, fructose, maltose, ribose, arabinose, pentose, xylose, galactose, and isomalt (e.g., a mixture of glucopyranosylmannitol dihydrate and glucopyranosylsorbitol), and combinations thereof, and sugar alcohols including, e.g., sorbitol, mannitol, xylitol, lactitol, maltitol, and pentatol, and combinations thereof. Other carriers include, e.g., starch, modified starch, hydrolyzed starches (e.g., maltodextrin), dextrin (e.g., water soluble and partially water soluble dextrins), and emulsifying polymers (e.g., gum arabic), pectins, xanthans, alginates, cellulose (e.g., carboxymethyl cellulose, methyl cellulose, ethyl cellulose, hydroxyethylcellulose, and hydroxypropyl cellulose), corn syrup (e.g., corn syrup solids), silicon dioxide, soy lecithin, butylated hydroxyanisole, butylated hydroxytoluene, and combinations thereof. Starch is an example of a water insoluble carrier.


The effervescent composition can include any suitable amount of the optional color agent including, e.g., less than 3% by weight, less than 2% by weight, less than 1% by weight, less than 0.5% by weight, at least 0.05% by weight, or even from 0.1% by weight to 0.5% by weight color agent.


Active agents that are optionally present in the effervescent composition include, e.g., medicaments, vitamins, minerals, amino acids, other dietary supplements, herbs, and combinations thereof. Examples of useful vitamins include, e.g., ascorbic acid (vitamin C), aspartic acid, thiamin, riboflavin, nicotinic acid, pantothenic acid, pyridoxine, biotin, folic acid, niacin, vitamin B12, lipoic acid, vitamin A, vitamin D, vitamin E and vitamin K and coenzymes thereof, choline, carnitine, and alpha, beta, and gamma carotenes.


Examples of coenzymes include thiamine pyrophosphates, flavin mononucleotide, flavin adenine dinucleotide, nicotinamide adenine dinucleotide, nicotinamide adenine dinucleotide phosphate coenzyme A pyridoxal phosphate, biocytin, tetrahydrofolic acid, coenzyme B12, lipoyllysine, 11-cis-retinal, and 1,25-dihydroxycholecalciferol, and mixtures thereof.


Examples of useful minerals include iron, zinc, calcium, sodium, potassium, manganese, selenium, copper, iodine, magnesium, phosphorus, and chromium and combinations thereof.


Useful amino acids include, e.g., L-tyrosine, isoleucine, ornithine, glutamine, phenylalanine, leucine, lysine, methionine, threonine, taurine, tryptophan, valine, alanine, glycine, arginine, histidine, cysteine, asparagine, proline and serine, and combinations thereof. Other dietary supplements include, e.g., bee pollen, bran, wheat germ, kelp, cod liver oil, ginseng, fish oils, proteins, and combinations thereof.


Useful herbs and extracts of herbs include, e.g., ginger, sage, thyme, red clover, black cohosh, and combinations thereof, ginseng, Echinacea, elderberry extract, and extracts thereof.


The ingredients of the effervescent composition can be sieved as necessary prior to combining with mixing.


The effervescent composition can be formed into tablets of any useful size and dimension including, e.g., tablets having a diameter of at least 10 mm, at least 15 mm, at least 20 mm, from 15 mm to 30 mm, from 20 mm to 30 mm, or even 25 mm, and a weight of at least 1 g, at least 3 g, at least 4 g, from 1 g to 7 g, from 2 g to 6.5 g, from 3 g to 6 g, or even from 4 g to 6 g.


The effervescent composition is well-suited to the mass production of effervescent tablets. The effervescent composition preferably can be tableted on a high speed tableting press to form tablets. Any suitable tablet mass production equipment and processes can be used. Examples of useful tableting processes for effervescent compositions are described in Pharmaceutical Dosage Forms, Vol. 1, (Herbert A. Lieberman et al. eds, 2nd ed. 1989) and incorporated herein. The tablets can then be manufactured in an automated process in which multiple dies of a tablet press are filled sequentially or simultaneously with the effervescent composition, two punches compress the effervescent composition to form the tablet(s), and then the tablet(s) is ejected from the die. The dies optionally include a lubricant.


The tablet is then placed in packaging material, which is then sealed to form an air tight sealed package. The packaged tablet can be further processed by conveying it to other processing stations including, e.g., additional packaging stations for further packaging, e.g., boxing and bagging.


The tablet manufacturing and initial packing operations are preferably performed in a controlled environment in which the temperature and humidity are controlled. Preferably the controlled environment has less than 18 grains, less than 16 grains, or even less than 15 grains of moisture per pound of air at a temperature of 72° F. (22.2° C.).


The effervescent tablets are preferably stored in a moisture-proof package. Useful moisture proof packages are in a variety of forms, including, e.g., sealed metal foil pouches, blister packs, and desiccant capped tubes. Useful packaging materials also include, e.g., plastic, metal foil, plastic films, capped tubes, and blister packaging.


A useful method of using the effervescent tablets includes dissolving a tablet in excess water, e.g., an eight-ounce, twelve-ounce or sixteen-ounce glass of water, a bottle of water and combinations thereof, to form an aqueous solution, and then ingesting the resulting composition. After addition of the effervescent composition to an aqueous liquid, the composition optionally can be stirred to further facilitate disintegration in the aqueous liquid.


The invention will now be described by way of the following examples. All parts, ratios, percentages and amounts stated in the Examples are by weight unless otherwise specified.


EXAMPLES

Test Procedures


Test procedures used in the examples are set forth below. All ratios and percentages are by weight unless otherwise indicated. The procedures are conducted at room temperature (i.e., an ambient temperature of from 20° C. to 25° C.) unless otherwise specified.


Hardness Test Method


The hardness of the tablets is measured using a Dr. Schleuniger Pharmatron hardness tester according to USP <1217> Tablet Breaking Force test method.


Disintegration Time Test Method


A timer is started simultaneously with adding one tablet to 500 mL of 25° C.+/−2° C. water and is stopped either when the tablet is fully disintegrated or no tablet pieces having a dimension of at least 0.25 inches (0.635 cm) are present. The time reflected on the timer is recorded in units of seconds.


% Moisture Test Method


The percent moisture present in a crystalline sugar binder is determined using a standardized Karl Fischer Moisture Analyzer according to USP 2018 Water Determination test method <921> 1a.


Base 1


Base 1 was prepared by combining, with mixing, 52.09% by weight sodium bicarbonate No. 5, 16.35% by weight sodium carbonate, 19.15% by weight potassium carbonate, 6.10% by weight potassium chloride, 3.53% by weight magnesium oxide, and 2.78% by weight calcium carbonate.


Base 2


Base 1 was prepared by combining, with mixing, 28.84% by weight sodium bicarbonate No. 5, 36.22% by weight sodium carbonate, 21.20% by weight potassium carbonate, 6.76% by weight potassium chloride, 3.91% by weight magnesium oxide, and 3.07% by weight calcium carbonate.


Examples E1-E6 and Controls C1-C11

The effervescent compositions of Examples E1-E6 and Controls C1-C11 were prepared by combining, with mixing, citric acid fine granular and then each of the ingredients set forth in Table 1, with the exception of the Avocado oil, in a KITCHEN AID mixer. The order of addition was from the ingredient present in the composition in the smallest amount to the largest amount. The amount of each ingredient set forth in Tables 1 and 2 is in units of % by weight based on the total weight of the formulation. When necessary, an ingredient was sieved using a number 12 sieve prior to addition to the mixture. After mixing the composition for ten minutes, the oil was added over a period of five minutes with mixing. The resulting compositions were then screened through a six mesh sieve.


The compositions were then tableted on a Cadmach rotary compression machine using 1 inch diameter stainless steel tools with a bisect. The average weight (in grams), thickness (in inches), and hardness (in kiloponds) of ten tablets was measured and is reported in Tables 1 and 2. The tablets were then tested according to the Disintegration Time Test Method and the average tablet disintegration time is reported in Table 1 in units of minutes and seconds (min: sec).













TABLE 1






C1
E1
C2
E2



















CANTAB Dextrose1
29.79
29.51
29.79
29.51


Citric Acid, Fine Granular
35.86
35.52
35.86
35.52


Citrus Orange Flavor2
2.11
2.09
0.00
0.00


Orange Flavor3
1.91
1.89
1.91
1.89


Citrus Orange Flavor4
0.00
0.00
2.11
2.09


Malic Acid
1.84
1.82
1.84
1.82


Stevia 95%
0.51
0.51
0.51
0.51


Avocado Oil
0.51
0.50
0.51
0.50


NuMag5 Natural
0.00
0.95
0.00
0.95


Base #1
27.46
27.20
27.46
27.20


Weight (g)
5.44
5.49
5.44
5.49


Thickness (in)
0.296
0.293
0.296
0.294


Hardness (kp)
9.3
8.4
9.3
8.2


Disintegration Time
4:04
3:56
3:59
3:43


(min: sec)






1= CANTAB compressible dextrose, which includes 97% crystalline dextrose monohydrate and 3% maltodextrin (Stauber Performance Ingredients, Inc., Fullerton, California)




2= Citrus Orange Flavor 188-65-C including maltodextrin, modified food starch and natural flavors (Edgar A. Weber & Co., Wheeling, Illinois)




3= NGP N-C Orange WONF Flavor 884.2186U greater than 50% by weight gum Arabic, from 25% by weight to 50% by weight natural flavor, from 2% by weight to 5% by weight medium chain trigylcerides, and less than 2% by weight DL-alpha tocopherol (Fona International, Geneva, Illinois)




4= 28-17-0224SD Citrus Orange Flavor MWNI SD from 89% by weight to 93% by weight gum Arabic and from 7% by weight to 11% by weight natural flavor (Edgar A. Weber & Co., Wheeling, Illinois)




5= Nu-MAG certified organic fine powder (Ribus, Inc., St. Louis, Missouri)


















TABLE 2






C3
C4
C5
E4



















CANTAB Dextrose
30.05
29.74
30.05
29.74


Citric Acid, Fine Granular
40.80
40.39
40.80
40.39


Natural TriBerry Flavor6
2.32
2.30
0.00
0.00


Natural TriBerry Flavor7
0.00
0.00
2.32
2.30


Malic Acid
0.74
0.73
0.74
0.73


Stevia 95%
0.56
0.55
0.56
0.55


Avocado Oil
0.52
0.51
0.52
0.51


NuMag Natural
0
1.01
0
1.01


Base #2
25.01
24.76
25.01
24.76


Weight (g)
5.39
5.45
5.39
5.45


Thickness (in)
0.3
0.293
0.301
0.295


Hardness (kp)
9
9.4
9.2
9.5


Disintegration Time
10:19
9:38
4:09
3:39


(min: sec)






6= Natural tri-berry-type flavor 31672 including modified com starch, natural flavor and tocopherol (Prinova Group LLC, Carol Stream, Illinois)




7= Natural tri-berry-type flavor 23339 including from 45% by weight to 55% by weight gum Arabic, from 30% by weight to 40% by weight maltodextrin, and from 10% by weight to 20% by weight natural flavor (Prinova Group LLC, Carol Stream, Illinois)


















TABLE 3






C6
C7
C8
E5



















CANTAB Dextrose
29.38
29.08
29.38
29.08


Citric Acid, Fine Granular
40.39
39.99
40.39
39.99


Strawberry Lemonade Flavor8
1.65
1.64
0.00
0.00


Natural Strawberry Lemonade
0.00
0.00
1.65
1.64


Flavor9






Stevia 95%
0.66
0.65
0.66
0.65


Avocado Oil
0.50
0.50
0.50
0.50


NuMag Natural
0.00
1.00
0.00
1.00


Base #1
27.41
27.14
27.41
27.14


Weight (g)
5.45
5.5
5.45
5.5


Thickness (in)
0.3
0.296
0.296
0.294


Hardness (kp)
8.8
8.5
8.9
7.6


Disintegration Time (min:sec)
8:21
7:51
4:21
3:29






8= 193-17-A Strawberry Lemonade Flavor 68% by weight modified food starch (waxy maize), 9% by weight maltodextrin, 5% by weight citric acid, and natural flavors (Edgar A. Weber & Co., Wheeling, Illinois)




9= 28-18-0118SD Strawberry Lemonade Flavor MWNI SD from 71% by weight to 81% by weight gum Arabic, 15% by weight to 25% by weight, and from 1% by weight to 5% by weight (Edgar A. Weber & Co., Wheeling, Illinois)


















TABLE 4






C9
C10
C11
E6



















CANTAB Dextrose
28.02
27.77
28.02
27.77


Citric Acid, Fine Granular
39.78
39.42
39.78
39.42


Orange Flavor10
2.42
2.40
0.00
0.00


Natural Orange Flavor11
0.00
0.00
2.42
2.40


Malic Acid
0.26
0.26
0.26
0.26


Stevia 95%
0.52
0.51
0.52
0.51


Avocado Oil
0.48
0.48
0.48
0.48


NuMag Natural
0.00
0.91
0.00
0.91


Base #1
28.51
28.25
28.51
28.25


Weight (g)
5.78
5.83
5.78
5.83


Thickness (in)
0.315
0.31
0.307
0.312


Hardness (kp)
9.9
9.6
9.6
8.4


Disintegration Time (min:sec)
7:07
6:44
4:48
4:08






10= Natural Orange Flavor WONF 16936 from 40% by weight to 50% by weight modified corn starch, from 40% by weight to 50% by weight maltodextrin, 10% by weight to 20% by weight natural flavors (Prinova Group LLC, Carol Stream, Illinois)




11= Natural Orange Flavor 23338 gum Arabic and natural flavor (Prinova Group LLC)







Other embodiments are within the claims. Documents referred to herein are hereby incorporated to the extent they do not conflict.


1. An effervescent tablet comprising: an effervescent agent comprising an acid and a base; a sweetener comprising Stevia, Monk fruit, or a combination thereof; a first directly compressible sugar binder; a flavor agent comprising gum Arabic; and a lubricant derived from rice hulls, the effervescent tablet having a weight of at least 4 grams and a hardness of at least 5 kiloponds, and exhibiting a disintegration time of no greater than 4 minutes and 20 seconds when tested according to the Disintegration Time Test Method.


2. The effervescent tablet of paragraph 1 comprising at least 1.5% by weight of a flavor agent comprising gum Arabic.


3. The effervescent tablet of paragraph 1 comprising at least 2% by weight of a flavor agent comprising gum Arabic.


4. The effervescent tablet of any one of paragraphs 1-3, wherein the tablet is free of flavor agents that are free of gum Arabic.


5. The effervescent tablet of any one of paragraphs 1-4, wherein the lubricant is a multi-component integral lubricant that comprises rice hull particles, gum Arabic, sunflower oil, and at least one extract of rice.


6. The effervescent tablet of any one of paragraphs 1-5, wherein the directly compressible sugar binder is selected from the group consisting of directly compressible dextrose, directly compressible sucrose, and combinations.


7. The effervescent tablet of any one of paragraphs 1-6, wherein the directly compressible sugar binder comprises dextrose.


8. The effervescent tablet of any one of paragraphs 1-6, wherein the directly compressible sugar binder comprises a mixture of dextrose and a polysaccharide.


9. The effervescent tablet of any one of paragraphs 1-8, wherein the effervescent tablet disintegrates in 25° C. water in no greater than 4 minutes.


10. The effervescent tablet of any one of paragraphs 1-8, wherein the effervescent tablet disintegrates in 25° C. water in no greater than 3.5 minutes.


11. The effervescent tablet of any one of paragraphs 1-10 comprising at least 20% by weight of the effervescent agent; and from 20% by weight to 55% by weight of the directly compressible sugar binder.


12. The effervescent tablet of any one of paragraphs 1-11 comprising from 0.4% by weight to 2% by weight of the sweetener.


13. The effervescent tablet of paragraph 12, wherein the tablet comprises at least 20% by weight of the effervescent agent; and from 20% by weight to 55% by weight of the directly compressible sugar binder.


14. The effervescent tablet of paragraph 13, wherein the tablet comprises from 0.8% by weight to 4% by weight of a multicomponent integral lubricant derived from rice hulls.


15. The effervescent tablet of any one of paragraphs 1-14, wherein the tablet comprises at least 1.5% by weight of a flavor agent comprising gum Arabic.


16. The effervescent tablet of any one of paragraphs 1-15, wherein the tablet is free of flavor agents that are free of gum Arabic.


17. The effervescent tablet of any one of paragraphs 1-16 further comprising oil.


18. The effervescent tablet of any one of paragraphs 1-17 having a hardness of at least 6 kiloponds.


19. The effervescent tablet of any one of paragraphs 1-18 comprising from 0.8% by weight to 4% by weight of the lubricant derived from rice hulls.


20. The effervescent tablet of any one of paragraphs 1-18 comprising from 0.8% by weight to 1.5% by weight of the lubricant derived from rice hulls.


21. A method of making an effervescent tablet, the method comprising: forming an effervescent composition by combining ingredients with mixing, the ingredients comprising an effervescent agent comprising an acid and a base, a sweetener comprising Stevia, Monk fruit, or a combination thereof, a first directly compressible sugar binder, a flavor agent comprising gum Arabic, a lubricant derived from rice hulls; and tableting the effervescent composition on a tableting press to form an effervescent tablet that has a mass of at least 4 grams and a hardness of at least 5 kiloponds and that disintegrates in 25° C. water in less than 5 minutes.


22. The method of paragraph 21, wherein the lubricant is a multi-component integral lubricant that comprises rice hull particles, gum Arabic, sunflower oil and at least one extract of rice.


23. The method of any one of paragraphs 21 and 22, wherein the tablet comprises at least 1.5% by weight of a flavor agent that comprises gum Arabic.


24. The method of any one of paragraphs 21 and 22, wherein the tablet comprises at least 2% by weight of a flavor agent that comprises gum Arabic.


25. The method of any one of paragraphs 21-24, wherein the tablet is free of flavor agents that are free of gum Arabic.


26. The method of any one of paragraphs 21-25, wherein the ingredients comprising from 0.8% by weight to 4% by weight of the lubricant derived from rice hulls.


27. The method of any one of paragraphs 21-25, wherein the ingredients comprising from 0.8% by weight to 4% by weight of a multicomponent integral lubricant derived from rice hulls.

Claims
  • 1. An effervescent tablet comprising: an effervescent agent comprising an acid and a base;a sweetener selected from the group consisting of Stevia, Monk fruit, and combinations thereof;a first directly compressible sugar binder;a flavor agent comprising gum Arabic; anda lubricant derived from rice hulls,the effervescent tablet having a weight of at least 4 grams and a hardness of at least 5 kiloponds, and exhibiting a disintegration time of no greater than 4 minutes and 20 seconds when tested according to the Disintegration Time Test Method.
  • 2. The effervescent tablet of claim 1 comprising at least 1.5% by weight of a flavor agent comprising gum Arabic.
  • 3. The effervescent tablet of claim 1 comprising at least 2% by weight of a flavor agent comprising gum Arabic.
  • 4. The effervescent tablet of claim 1, wherein the tablet is free of flavor agents that are free of gum Arabic.
  • 5. The effervescent tablet of claim 1, wherein the lubricant is a multi-component integral lubricant that comprises rice hull particles, gum Arabic, sunflower oil, and at least one extract of rice.
  • 6. The effervescent tablet of claim 1, wherein the directly compressible sugar binder is selected from the group consisting of directly compressible dextrose, directly compressible sucrose, and combinations.
  • 7. The effervescent tablet of claim 1, wherein the directly compressible sugar binder comprises dextrose.
  • 8. The effervescent tablet of claim 1, wherein the directly compressible sugar binder comprises a mixture of dextrose and a polysaccharide.
  • 9. The effervescent tablet of claim 1, wherein the effervescent tablet disintegrates in 25° C. water in no greater than 4 minutes.
  • 10. The effervescent tablet of claim 1, wherein the effervescent tablet disintegrates in 25° C. water in no greater than 3.5 minutes.
  • 11. The effervescent tablet of claim 1 comprising at least 20% by weight of the effervescent agent; andfrom 20% by weight to 55% by weight of the directly compressible sugar binder.
  • 12. The effervescent tablet of claim 11 comprising from 0.4% by weight to 2% by weight of the sweetener.
  • 13. The effervescent tablet of claim 5, wherein the tablet comprises at least 20% by weight of the effervescent agent; andfrom 20% by weight to 55% by weight of the directly compressible sugar binder.
  • 14. The effervescent tablet of claim 13, wherein the tablet comprises from 0.4% by weight to 2% by weight of the sweetener.
  • 15. The effervescent tablet of claim 13, wherein the tablet comprises at least 1.5% by weight of a flavor agent comprising gum Arabic.
  • 16. The effervescent tablet of claim 13, wherein the tablet is free of flavor agents that are free of gum Arabic.
  • 17. The effervescent tablet of claim 1 further comprising oil.
  • 18. The effervescent tablet of claim 1 having a hardness of at least 6 kiloponds.
  • 19. The effervescent tablet of claim 1 comprising from 0.8% by weight to 4% by weight of the lubricant derived from rice hulls.
  • 20. A method of making an effervescent tablet, the method comprising: forming an effervescent composition by combining ingredients with mixing, the ingredients comprising an effervescent agent comprising an acid and a base,a sweetener selected from the group consisting of Stevia, Monk fruit, and combinations thereof,a first directly compressible sugar binder,a flavor agent comprising gum Arabic,a lubricant derived from rice hulls; andtableting the effervescent composition on a tableting press to form an effervescent tablet that has a mass of at least 4 grams and a hardness of at least 5 kiloponds and that disintegrates in 25° C. water in less than 5 minutes.
  • 21. The method of claim 20, wherein the lubricant is a multi-component integral lubricant that comprises rice hull particles, gum Arabic, sunflower oil and at least one extract of rice.
  • 22. The method of claim 20, wherein the tablet comprises at least 1.5% by weight of a flavor agent that comprises gum Arabic.
  • 23. The method of claim 20, wherein the tablet comprises at least 2% by weight of a flavor agent that comprises gum Arabic.
  • 24. The method of claim 20, wherein the tablet is free of flavor agents that are free of gum Arabic.
US Referenced Citations (12)
Number Name Date Kind
3642535 Graham et al. Feb 1972 A
4013775 Nelson et al. Mar 1977 A
4059460 Schollmeier et al. Nov 1977 A
4297146 Mise et al. Oct 1981 A
5037657 Jones Aug 1991 A
6527868 Moraly et al. Mar 2003 B2
8865948 Duflot Oct 2014 B2
20110281008 Gootenilleke Nov 2011 A1
20120031533 Onda et al. Feb 2012 A1
20120058236 Fosdick et al. Mar 2012 A1
20130309389 Carlson et al. Nov 2013 A1
20140037814 Quinlan et al. Feb 2014 A1
Foreign Referenced Citations (6)
Number Date Country
103098926 May 2013 CN
WO2005072759 Aug 2005 WO
WO2010057372 May 2010 WO
WO-2011058336 May 2011 WO
WO2011130440 Oct 2011 WO
WO2014018569 Jan 2014 WO
Non-Patent Literature Citations (2)
Entry
Ribus, 2nd Generation Clean Label Lubricant, Oct. 5, 2016, www.ribus.com/nu-mag/ (Year: 2016).
Dauqan, “Utilization of Gum Arabic for Industries and Huan Health,” Am. J. of Applied Sciences, vol. 10, No. 10, Oct. 1, 2013, pp. 1270-1279.
Related Publications (1)
Number Date Country
20200170936 A1 Jun 2020 US
Provisional Applications (1)
Number Date Country
62774112 Nov 2018 US