CA2158867A1 - Beverage stabilizing system - Google Patents
Beverage stabilizing systemInfo
- Publication number
- CA2158867A1 CA2158867A1 CA002158867A CA2158867A CA2158867A1 CA 2158867 A1 CA2158867 A1 CA 2158867A1 CA 002158867 A CA002158867 A CA 002158867A CA 2158867 A CA2158867 A CA 2158867A CA 2158867 A1 CA2158867 A1 CA 2158867A1
- Authority
- CA
- Canada
- Prior art keywords
- beverage
- gellan gum
- carboxymethylcellulose
- stabilizing
- blend
- 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.)
- Abandoned
Links
Classifications
-
- 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
- A23G9/00—Frozen sweets, e.g. ice confectionery, ice-cream; Mixtures therefor
- A23G9/32—Frozen sweets, e.g. ice confectionery, ice-cream; Mixtures therefor characterised by the composition containing organic or inorganic compounds
- A23G9/34—Frozen sweets, e.g. ice confectionery, ice-cream; Mixtures therefor characterised by the composition containing organic or inorganic compounds characterised by carbohydrates used, e.g. polysaccharides
-
- 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
- A23G1/00—Cocoa; Cocoa products, e.g. chocolate; Substitutes therefor
- A23G1/30—Cocoa products, e.g. chocolate; Substitutes therefor
- A23G1/56—Cocoa products, e.g. chocolate; Substitutes therefor making liquid products, e.g. for making chocolate milk drinks and the products for their preparation, pastes for spreading, milk crumb
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L2/00—Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
- A23L2/52—Adding ingredients
- A23L2/62—Clouding agents; Agents to improve the cloud-stability
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
- A23L29/20—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
- A23L29/206—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin
- A23L29/262—Cellulose; Derivatives thereof, e.g. ethers
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
- A23L29/20—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
- A23L29/269—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of microbial origin, e.g. xanthan or dextran
- A23L29/272—Gellan
-
- 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
- A23G2200/00—COCOA; COCOA PRODUCTS, e.g. CHOCOLATE; SUBSTITUTES FOR COCOA OR COCOA PRODUCTS; CONFECTIONERY; CHEWING GUM; ICE-CREAM; PREPARATION THEREOF containing organic compounds, e.g. synthetic flavouring agents
- A23G2200/06—COCOA; COCOA PRODUCTS, e.g. CHOCOLATE; SUBSTITUTES FOR COCOA OR COCOA PRODUCTS; CONFECTIONERY; CHEWING GUM; ICE-CREAM; PREPARATION THEREOF containing organic compounds, e.g. synthetic flavouring agents containing beet sugar or cane sugar if specifically mentioned or containing other carbohydrates, e.g. starches, gums, alcohol sugar, polysaccharides, dextrin or containing high or low amount of carbohydrate
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Health & Medical Sciences (AREA)
- Dispersion Chemistry (AREA)
- Nutrition Science (AREA)
- Molecular Biology (AREA)
- Inorganic Chemistry (AREA)
- Non-Alcoholic Beverages (AREA)
- Devices For Dispensing Beverages (AREA)
- Dairy Products (AREA)
- Food Preservation Except Freezing, Refrigeration, And Drying (AREA)
- Jellies, Jams, And Syrups (AREA)
- Beverage Vending Machines With Cups, And Gas Or Electricity Vending Machines (AREA)
- Devices That Are Associated With Refrigeration Equipment (AREA)
- General Preparation And Processing Of Foods (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
A beverage stabilizing system which is a blend of gellan gum and carboxymethylcellulose. The blend provides a weak, stabilizing gel structure suitable for beverage products.
Description
~5886'1 TITLE OF THE INVENTION
BEVERAGE STABILIZING SYSTEM
BACKGROUND OF THE INVENTION
5Many commercially available beverages are unstable and require stabilizing additives to m~in~in beverage homogeneity over an extended period of time. Citrus juices, for example, contain pulp material which remain suspended over a period of time only with the assistance of additives such as propylene glycol alginates or other food 10 additives known to stabilize and/or thicken. Beverages cont~ining powder additives such as cocoa powder also require suspending agents to prevent premature settling.
In the past, hydrocolloids such as gum arabic, xanthan gum, pectin, starch and modified starch, and carboxymethylcellulose have 15 been used to stabilize beverages. Relatively large quantities of these materials are required in order to achieve an effective degree of stabilization. While stabilizing the beverage, these materials unfortunately affect beverage flavor and feel. Sometimes, as with xanthan gum, the beverage stabilizing material reacts with other 20 beverage components, including proteins (such as milk proteins or beer proteins), affecting beverage flavor and stabilizer efficacy.
McGinley, et al., United States Patent 4,980,193, describe~
a stabilizing agent which is useful as a rapid dispersing agent for suspending solids in an aqueous medium, which contains colloidal 25 microcrystalline cellulose, starch, and a non-thickening water soluble diluent such as maltodextrin, whey or non-fat dry milk.
The present invention is a beverage stabilizing system which forms a weak, stabilizing gel structure particularly suitable for beverage stabilization.
wo 94/24887 215 8 ~ 6 7 PCT/US94/04023 SUMMARY OF THE INVENTION
The invention is a beverage stabilizing blend composition consisting of carboxymethylcellulose and gellan gum in the carboxymethylcellulose:gellan gum weight ratio range of between about 3:1 to 20:1, preferably 4:1 to 15:1, and more preferably 5:1 to 10:1. The o invention also includes beverages cont~ining the beverage stabilizing blend.
The amount of stabilizing blend used in the beverages, based on weight % of the beverage, is between about 0.06% and 0.3%, preferably 0.06% and 0.2%, and more preferably 0.06% and 0.1%.
In some beverages, it is advantageous, although not necessary, to include, in the stabilizing blend, an amount of propylene glycol alginate. Thus, the invention contemplates preferred beverage stabilizing blends which include carboxymethylcellulose, gellan gum, and propylene glycol alginate, as well as beverages cont~ining these beverage stabilizing blends. These blends can include amounts of propylene glycol alginate up to and equivalent to the amounts of carboxymethylcellulose. The propylene glycol alginate:gellan gum weight ratio is between about 3:1 to 20:1, preferably 4:1 to 15:1, and more preferably 5:1 to 10:1.
The invention also includes a method for stabilizing a beverage which comprises adding to the beverage a stabilizing blend composition consisting of carboxymethylcellulose and gellan gum in the carboxymethylcellulose:gellan gum weight ratio range of between about 3:1 to 20:1.
DETAILED DESCRIPTION OF THE INVENTION
The beverage stabilizing blend composition of the present invention provides a unique gel structure which is particularly suited for beverages. The gel structure provides a system which suspends materials, such as solid powder materials or solid pulp materials, that are present in beverages and that otherwise separate from the beverage over time. Advantageously, the gel is weak and breaks under low shear conditions, allowing convenient consumption of the beverage. Thus the stabilizing blends of the invention acheive the objectives of maintaining beverage homogeneity and providing low viscosity at moderate shear o conditions.
The combination of gellan gum and carboxymethylcellulose provides a uniquely effective stabilizing system that cannot be effected with gellan gum or carboxymethylcellulose alone.
Beverages cont~ining blends of the invention display rheological properties of a weak gel system when measured using dynamic viscoelastic measurements. One characteristic of a gelled system is a constant elastic (storage) modulus over a range of strain values up to a critical strain value, at which critical strain value the modulus drops significantly.
In beverage systems, gel networks created by gellan gum alone are susceptible to breakdown even at low levels of shear strain.
Gentle stirring can result in complete loss of suspending abilities. The gel is so delicate that it can only be detected through the use of sensitive instrumentation.
The addition of carboxymethylcellulose to gellan gum provides an effective beverage stabilizing system. Indications are that CMC, and other materials with a similar ~ 1 ~ 4 backbone, can modify gellan gum gel formation behavior. In beverages, where low levels of gellan gum are used, this combination with CMC results in a product 3 0 that is much less sensitive to strain, has gel properties that are able to re-form with time and imparts a greater viscous modulus. All of these are important for product stability and mouthfeel.
In some instances, the addition of propylene glycol alginate enhances the beverages stabilized by gellan gum and CMC. PGA
imparts flavor benefits which have been quantified with extensive 2ls8~6~
sensory testing. It also adds to the background of ~"plain" or non-gelled viscosity that helps give a smooth feeling in the mouth. Thus, stabilizing systems which also include polyethylene gly~col alginate are preferred stabilizing systems. `7 Beverages which are stabilized by blends of the invention include pulp-cont~inin~, oil emulsion-cont~ining or other particle-cont~ining beverages, including citrus juices such as orange juice, fruit nectars, and milk-based beverages such as chocolate milk.
Gellan gum is a heteropolysaccharide prepared by fermentation of Pseudomonas elodea ATCC 31461. Gellan gum is available from Kelco Division of Merck & Co., Inc., under various names, including KELCOGEL and KELCOGEL F. Processes for preparing gellan gum include those described in United States Patents 4,326,052 and 4,326,053. It is useful for a variety of gelling, texturizing, stabilizing and film forming applications, particularly as a gelling agent in foods, personal care products and industrial applications.
Carboxymethylcellulose, e.g. CMC 7HF, is a cellulose derivative which is commercially available and known to be useful in drilling muds, as a soil-suspending agent in detergents, in resin emulsion paints, adhesives, printing inks, textile sizes, and as a food stabilizer.
Propylene glycol alginates are water-soluble, hydrophilic colloids used as secondary emulsifiers to thicken and stabilize food and pharmaceutical systems. They provide a range of viscosities from very low to very high, depending on type and concentration. These alginates combine emulsifying and thickening properties to provide excellent emulsion stability with good body. Propylene glycol alginates are useful 3 0 in acidic solutions, since they are soluble and stable in solutions of pH
3.0 to 6Ø Specific food applications include syrups, sauces, icings, frozen foods, salad dressings, relish, batters, citrus concentrates and food emulsions. Propylene glycol alginates are commercially available from Kelco, Division of Merck & Co., Inc., San Diego, CA, under product WO 94/24887 PCTtUS94/04023 21~8867 names KELCOLOID(~) HVF, KELCOLOID@~) LVF, KELCOLOID( DH, KELCOLOID@~) S, and KELCOLOID(~) O.
Typical pH modifiers, such as citric acid or maleic acid, sweeteners, such as natural and artificial sweeteners, preservatives, such as sodium benzoate, flavorings such as flavor emulsion oil bases, other common beverage additives such as sodium citrate and ascorbic acid, and colorings, may also be added to beverages of the present invention KELCOGEL F was used in the following examples. The presence of sodium citrate improves the solubility of the gellan gum by sequestering divalent ions present in the system. CMC 7HF (Aqualon) and KELCOLOID LVF propylene glycol alginate were also used.
EXAMPLE l Stabilized Chocolate Milk Commercially available Alta Dena low fat chocolate milk, which contains lc-carrageenan, was examined using the Vilastic V-E
rheometer. Specifically, elastic modulus and viscous modulus were measured.
A basic low fat chocolate milk formulation cont~ining 6.3%
sugar and 1.0% ~lk~1i7ed low fat cocoa powder type S from Cacao De Zaan (Holland), was stabilized with the beverage stabilizing system of the invention. The stabilizer blend was thoroughly mixed with the sugar and cocoa powder and added directly to the cold milk before heating the product. The final formulation and procedures are given 3 below:
i~ ~
Chocolate Milk Forrnulation Quantity Ingredients Grams Percent Non fat milk 370.3 92.575 Sugar 25.2 6.30 Cocoa powder 4.0 1.00 Sodium citrate 0.01 0.00 CarboxymethylcelluloseCMC 7HF 0.30 0.075 KELCOLOID LVF 0.15 0.0375 KELCOGEL F gellan gum 0.04 0.01 Total 400.0 100.00 Procedure 1. Thoroughly blend the sugar, cocoa powder, CMC, KELCOLOID
LVF and KELCOGEL F and sodium citrate and disperse them with good agitation into the cold milk.
BEVERAGE STABILIZING SYSTEM
BACKGROUND OF THE INVENTION
5Many commercially available beverages are unstable and require stabilizing additives to m~in~in beverage homogeneity over an extended period of time. Citrus juices, for example, contain pulp material which remain suspended over a period of time only with the assistance of additives such as propylene glycol alginates or other food 10 additives known to stabilize and/or thicken. Beverages cont~ining powder additives such as cocoa powder also require suspending agents to prevent premature settling.
In the past, hydrocolloids such as gum arabic, xanthan gum, pectin, starch and modified starch, and carboxymethylcellulose have 15 been used to stabilize beverages. Relatively large quantities of these materials are required in order to achieve an effective degree of stabilization. While stabilizing the beverage, these materials unfortunately affect beverage flavor and feel. Sometimes, as with xanthan gum, the beverage stabilizing material reacts with other 20 beverage components, including proteins (such as milk proteins or beer proteins), affecting beverage flavor and stabilizer efficacy.
McGinley, et al., United States Patent 4,980,193, describe~
a stabilizing agent which is useful as a rapid dispersing agent for suspending solids in an aqueous medium, which contains colloidal 25 microcrystalline cellulose, starch, and a non-thickening water soluble diluent such as maltodextrin, whey or non-fat dry milk.
The present invention is a beverage stabilizing system which forms a weak, stabilizing gel structure particularly suitable for beverage stabilization.
wo 94/24887 215 8 ~ 6 7 PCT/US94/04023 SUMMARY OF THE INVENTION
The invention is a beverage stabilizing blend composition consisting of carboxymethylcellulose and gellan gum in the carboxymethylcellulose:gellan gum weight ratio range of between about 3:1 to 20:1, preferably 4:1 to 15:1, and more preferably 5:1 to 10:1. The o invention also includes beverages cont~ining the beverage stabilizing blend.
The amount of stabilizing blend used in the beverages, based on weight % of the beverage, is between about 0.06% and 0.3%, preferably 0.06% and 0.2%, and more preferably 0.06% and 0.1%.
In some beverages, it is advantageous, although not necessary, to include, in the stabilizing blend, an amount of propylene glycol alginate. Thus, the invention contemplates preferred beverage stabilizing blends which include carboxymethylcellulose, gellan gum, and propylene glycol alginate, as well as beverages cont~ining these beverage stabilizing blends. These blends can include amounts of propylene glycol alginate up to and equivalent to the amounts of carboxymethylcellulose. The propylene glycol alginate:gellan gum weight ratio is between about 3:1 to 20:1, preferably 4:1 to 15:1, and more preferably 5:1 to 10:1.
The invention also includes a method for stabilizing a beverage which comprises adding to the beverage a stabilizing blend composition consisting of carboxymethylcellulose and gellan gum in the carboxymethylcellulose:gellan gum weight ratio range of between about 3:1 to 20:1.
DETAILED DESCRIPTION OF THE INVENTION
The beverage stabilizing blend composition of the present invention provides a unique gel structure which is particularly suited for beverages. The gel structure provides a system which suspends materials, such as solid powder materials or solid pulp materials, that are present in beverages and that otherwise separate from the beverage over time. Advantageously, the gel is weak and breaks under low shear conditions, allowing convenient consumption of the beverage. Thus the stabilizing blends of the invention acheive the objectives of maintaining beverage homogeneity and providing low viscosity at moderate shear o conditions.
The combination of gellan gum and carboxymethylcellulose provides a uniquely effective stabilizing system that cannot be effected with gellan gum or carboxymethylcellulose alone.
Beverages cont~ining blends of the invention display rheological properties of a weak gel system when measured using dynamic viscoelastic measurements. One characteristic of a gelled system is a constant elastic (storage) modulus over a range of strain values up to a critical strain value, at which critical strain value the modulus drops significantly.
In beverage systems, gel networks created by gellan gum alone are susceptible to breakdown even at low levels of shear strain.
Gentle stirring can result in complete loss of suspending abilities. The gel is so delicate that it can only be detected through the use of sensitive instrumentation.
The addition of carboxymethylcellulose to gellan gum provides an effective beverage stabilizing system. Indications are that CMC, and other materials with a similar ~ 1 ~ 4 backbone, can modify gellan gum gel formation behavior. In beverages, where low levels of gellan gum are used, this combination with CMC results in a product 3 0 that is much less sensitive to strain, has gel properties that are able to re-form with time and imparts a greater viscous modulus. All of these are important for product stability and mouthfeel.
In some instances, the addition of propylene glycol alginate enhances the beverages stabilized by gellan gum and CMC. PGA
imparts flavor benefits which have been quantified with extensive 2ls8~6~
sensory testing. It also adds to the background of ~"plain" or non-gelled viscosity that helps give a smooth feeling in the mouth. Thus, stabilizing systems which also include polyethylene gly~col alginate are preferred stabilizing systems. `7 Beverages which are stabilized by blends of the invention include pulp-cont~inin~, oil emulsion-cont~ining or other particle-cont~ining beverages, including citrus juices such as orange juice, fruit nectars, and milk-based beverages such as chocolate milk.
Gellan gum is a heteropolysaccharide prepared by fermentation of Pseudomonas elodea ATCC 31461. Gellan gum is available from Kelco Division of Merck & Co., Inc., under various names, including KELCOGEL and KELCOGEL F. Processes for preparing gellan gum include those described in United States Patents 4,326,052 and 4,326,053. It is useful for a variety of gelling, texturizing, stabilizing and film forming applications, particularly as a gelling agent in foods, personal care products and industrial applications.
Carboxymethylcellulose, e.g. CMC 7HF, is a cellulose derivative which is commercially available and known to be useful in drilling muds, as a soil-suspending agent in detergents, in resin emulsion paints, adhesives, printing inks, textile sizes, and as a food stabilizer.
Propylene glycol alginates are water-soluble, hydrophilic colloids used as secondary emulsifiers to thicken and stabilize food and pharmaceutical systems. They provide a range of viscosities from very low to very high, depending on type and concentration. These alginates combine emulsifying and thickening properties to provide excellent emulsion stability with good body. Propylene glycol alginates are useful 3 0 in acidic solutions, since they are soluble and stable in solutions of pH
3.0 to 6Ø Specific food applications include syrups, sauces, icings, frozen foods, salad dressings, relish, batters, citrus concentrates and food emulsions. Propylene glycol alginates are commercially available from Kelco, Division of Merck & Co., Inc., San Diego, CA, under product WO 94/24887 PCTtUS94/04023 21~8867 names KELCOLOID(~) HVF, KELCOLOID@~) LVF, KELCOLOID( DH, KELCOLOID@~) S, and KELCOLOID(~) O.
Typical pH modifiers, such as citric acid or maleic acid, sweeteners, such as natural and artificial sweeteners, preservatives, such as sodium benzoate, flavorings such as flavor emulsion oil bases, other common beverage additives such as sodium citrate and ascorbic acid, and colorings, may also be added to beverages of the present invention KELCOGEL F was used in the following examples. The presence of sodium citrate improves the solubility of the gellan gum by sequestering divalent ions present in the system. CMC 7HF (Aqualon) and KELCOLOID LVF propylene glycol alginate were also used.
EXAMPLE l Stabilized Chocolate Milk Commercially available Alta Dena low fat chocolate milk, which contains lc-carrageenan, was examined using the Vilastic V-E
rheometer. Specifically, elastic modulus and viscous modulus were measured.
A basic low fat chocolate milk formulation cont~ining 6.3%
sugar and 1.0% ~lk~1i7ed low fat cocoa powder type S from Cacao De Zaan (Holland), was stabilized with the beverage stabilizing system of the invention. The stabilizer blend was thoroughly mixed with the sugar and cocoa powder and added directly to the cold milk before heating the product. The final formulation and procedures are given 3 below:
i~ ~
Chocolate Milk Forrnulation Quantity Ingredients Grams Percent Non fat milk 370.3 92.575 Sugar 25.2 6.30 Cocoa powder 4.0 1.00 Sodium citrate 0.01 0.00 CarboxymethylcelluloseCMC 7HF 0.30 0.075 KELCOLOID LVF 0.15 0.0375 KELCOGEL F gellan gum 0.04 0.01 Total 400.0 100.00 Procedure 1. Thoroughly blend the sugar, cocoa powder, CMC, KELCOLOID
LVF and KELCOGEL F and sodium citrate and disperse them with good agitation into the cold milk.
2. Heat the milk to 71C (160F). M~int~in this temperature for several minutes while mixing.
25 3. Rapidly cool the mixture while stirring.
4. Package and store under refrigerated conditions.
Shear rate of 50 s- 1 was used as a standard rate to evaluate 30 the behavior of beverages containing various blends. 50 s l is used as a standard because it has been found to closely represent mouth shear conditions.
A blend of 7.5 parts CMC (0.075% wt. based on total beverage weight) to 1 part KELCOGEL F gellan gum (0.01 % wt. based on total beverage weight) was evaluated for beverage stabilization. The PCT/~JS 94/04023 IPE.4/US 1 4 NOV 199 5 KELCOLOID LVF was present at 0.0375% wt. based on total beverage weight. l lis blend formed a beverage product having good rheology and moutl~el.
Figure 1 c4~ A~s V;scGsilics of milk based beverages cont~ining one of the stabilizing blend conlpol-ents with the viscosity of a milk based beverage cont~ining the stabilizing blend of the invention.
Also represente~ is a co.. ercially available low fat chocolate milk product cont~ining carrageenan, and a milk based beverage cont~ining none of the components of the stabilizing blend.
20 \\\~
A~O ~E~
K.2130YP Fc7i(~ ~ 9 4 / G - J ' 3 IPEA/U~S 1~ N~V 199 - 8 21~8867 The CMC/ICELCOGEL PC bleDd both with and without PGA
produced viscosilics equal to the eo.-~...er~ial ehocolate miLk. Stability tests found both blends are able to s~spen~ the eocoa powder for 7 days, while the individual cGI~lyo..e.lls began to separate after being stored for on~y 24 hours at refrigerated te.ll~la~ s (~4C). Stabilizcr level was varied to identify suitable ranges. The "eontrol" beverage contain~
0.075% CMC, 0.0375% KELCOLO~D LVF and 0.0125% KELCOGEL F
(i.e. 0.1 125% total stabilizer blend). Levels of these blend components were inereased or decreased unifomlly. The viseosities of these various milk based beverages are sho~,vn in Figure 2.
2s ,~DE~ S~
Results showed that the gum stabilizer blend would form a strong, uniform gel at a 100% increase in concentration (i.e. 0.15%
CMC, 0.075% KELCOLOID LVF and 0.02% KELCOGEL F, corresponding to 0.245% total stabilizer blend). The control beverage, as well as beverages with 50% and 100% increased levels of stabilizer blend, displayed no signs of separation. Beverages with 30% and 60%
decreased levels of stabilizer displayed separation of the cocoa after 24 hours at refrigerated temperatures.
Peach Nectar A peach nectar produced by Kerns was evaluated for soluble solids (14.2% solids), pH (3.7) and viscosity. Because of the pulp present in the peach nectar, a Brookfield RVT with a UL adapter, rather than the Vilastic V-E was used for viscosity determinations. The viscosity at a shear rate of 50 s-l was 32 cP @ 6C.
The ingredient statement for the Kerns product along with the solids, pH and viscosity were used to develop a nectar formulation Peach Nectar Formulation Ouantity 2 5 Ingredients Grams Percent Water deionized 187.42 62.47 Peach pulp puree 63.00 21.0 High fructose corn syrup 55DE48.00 16.0 Citric acid 0.73 0.24 Sodium Citrate 0.406 0.14 Carboxymethylcellulose CMC 7HF 0.15 0.05 KELCOLOID LVF 0.15 0.05 Ascorbic acid 0.12 0.04 KELCOGEL F gellan gum 0.024 0.01 Total 300.0 100.00 PCrQ~; 94 / 0 4 0 2 3 K2 1 30YP ' IPEAIUS 7 4 NOV 199~
- '~158867 Procedure 1. Blend the CMC,KELCOLOII)LVF and the KELCOGEL F
together and add to the deionized water while mi~ing under high 5 shear. Mi~ for 5 minlltes.
2. Add the com syrup to the gurn solution and CO.~ C mi~in~ for 2 more ...i~ cs o 3. Blend the citric acid, sodiurn citrate and ascorbic acid together.
Mix this blend into the peach puree.
4. Add the peach puree to the gum com syrup solution and miX for 3 .~.utes.
5. Bottle and store nectar under refrigerated conditions.
Peach puree was oht~i~.c~ by ble~in& canned cling peaches in a food proccssor. The com syrup used was 5S DE high fructose com 20 syrup produc~ by Staley. Tbe levels of citric acid and com syrup were chosen to match the solids and pH of the Kcms product. Ascorbic acid was added to slow o~idation discoloration of thc product.
A viscosity of about 32 cP at S0 s-l @ 6C is desirable for a peach ncctar bcvcrage.
2s Five parts CMC to I part KELCOGEL F was uscd to stabilizc tbc ncctar. KELCOLOID LVF was uscd at a level cqual to ~e CMC for background ~,iscosity and flavor ~hqnc~ t~ No h~tin~ was ~qu~d.
Wbcn thc blcnd was uscd at 0.1 1% total Co~ ,ation, a 30 viscosity of 3S cP at S0 s-l and 6C ~s~lte~ Visc~sit~ of tbc bcverage, as a function of shcar ratc, is sbown in Figure 3.
~D ~E~
PCT1~S 94l 0~ 0 ~ 3 K~130YP
-- ~PEA/Us l4 N~
1 5 \
Significant settling (>20%) wa~i observed in the control with no 25 stabilizer co~ e.lt, as wcll as the samples c~ ing either CMC alone or KELCOLOID LVF alone. Approximately 2% scttling was measured in the ncctar CG..~ .& KELCOGEL F alone. Gellan gum alone does not provide cnough structure to prevent settling.
Aftcr 100 hours, no ~nlin~ was obscrved in the beverage 30 co..~;..;..g ~e blcnd of KELCOGEL PC and CMC. Also, aft~r 100 hours, no settling was observed` in the beverage col,t~ .g the blend of KELCOGEL PC/CMC/PGA.
,~ 9HE~
Citrus Punch Formulation Ouantity Ingredients GramsPercent Water deionized 381.09176.2182 High fructose corn syrup 55DE 64.4012.8800 Citrus Juice Concentrate 50.0010.0000 Citric acid 3.03 0.6060 Sodium Citrate 0.795 0.1590 Carboxymethylcellulose CMC 7HF 0.24 0.0480 Concentrated Orange Flavor 0.115 0.0230 Ascorbic acid 0.19 0.0380 KELCOLOID LVF 0.12 0.0240 KELCOGEL F gellan gum 0.019 0.003 Total 500.0100.000 Procedure 1. Dry blend the CMC, KELCOLOID LVF and the KELCOGEL F
together and add to the deionized water while mixing under high shear. Mix for 5 minutes.
2. Add the corn syrup to the gum solution and continue mixing for 2 more minutes.
3. Add the concentrated orange flavor to the solution and mix for 1 minute.
25 3. Rapidly cool the mixture while stirring.
4. Package and store under refrigerated conditions.
Shear rate of 50 s- 1 was used as a standard rate to evaluate 30 the behavior of beverages containing various blends. 50 s l is used as a standard because it has been found to closely represent mouth shear conditions.
A blend of 7.5 parts CMC (0.075% wt. based on total beverage weight) to 1 part KELCOGEL F gellan gum (0.01 % wt. based on total beverage weight) was evaluated for beverage stabilization. The PCT/~JS 94/04023 IPE.4/US 1 4 NOV 199 5 KELCOLOID LVF was present at 0.0375% wt. based on total beverage weight. l lis blend formed a beverage product having good rheology and moutl~el.
Figure 1 c4~ A~s V;scGsilics of milk based beverages cont~ining one of the stabilizing blend conlpol-ents with the viscosity of a milk based beverage cont~ining the stabilizing blend of the invention.
Also represente~ is a co.. ercially available low fat chocolate milk product cont~ining carrageenan, and a milk based beverage cont~ining none of the components of the stabilizing blend.
20 \\\~
A~O ~E~
K.2130YP Fc7i(~ ~ 9 4 / G - J ' 3 IPEA/U~S 1~ N~V 199 - 8 21~8867 The CMC/ICELCOGEL PC bleDd both with and without PGA
produced viscosilics equal to the eo.-~...er~ial ehocolate miLk. Stability tests found both blends are able to s~spen~ the eocoa powder for 7 days, while the individual cGI~lyo..e.lls began to separate after being stored for on~y 24 hours at refrigerated te.ll~la~ s (~4C). Stabilizcr level was varied to identify suitable ranges. The "eontrol" beverage contain~
0.075% CMC, 0.0375% KELCOLO~D LVF and 0.0125% KELCOGEL F
(i.e. 0.1 125% total stabilizer blend). Levels of these blend components were inereased or decreased unifomlly. The viseosities of these various milk based beverages are sho~,vn in Figure 2.
2s ,~DE~ S~
Results showed that the gum stabilizer blend would form a strong, uniform gel at a 100% increase in concentration (i.e. 0.15%
CMC, 0.075% KELCOLOID LVF and 0.02% KELCOGEL F, corresponding to 0.245% total stabilizer blend). The control beverage, as well as beverages with 50% and 100% increased levels of stabilizer blend, displayed no signs of separation. Beverages with 30% and 60%
decreased levels of stabilizer displayed separation of the cocoa after 24 hours at refrigerated temperatures.
Peach Nectar A peach nectar produced by Kerns was evaluated for soluble solids (14.2% solids), pH (3.7) and viscosity. Because of the pulp present in the peach nectar, a Brookfield RVT with a UL adapter, rather than the Vilastic V-E was used for viscosity determinations. The viscosity at a shear rate of 50 s-l was 32 cP @ 6C.
The ingredient statement for the Kerns product along with the solids, pH and viscosity were used to develop a nectar formulation Peach Nectar Formulation Ouantity 2 5 Ingredients Grams Percent Water deionized 187.42 62.47 Peach pulp puree 63.00 21.0 High fructose corn syrup 55DE48.00 16.0 Citric acid 0.73 0.24 Sodium Citrate 0.406 0.14 Carboxymethylcellulose CMC 7HF 0.15 0.05 KELCOLOID LVF 0.15 0.05 Ascorbic acid 0.12 0.04 KELCOGEL F gellan gum 0.024 0.01 Total 300.0 100.00 PCrQ~; 94 / 0 4 0 2 3 K2 1 30YP ' IPEAIUS 7 4 NOV 199~
- '~158867 Procedure 1. Blend the CMC,KELCOLOII)LVF and the KELCOGEL F
together and add to the deionized water while mi~ing under high 5 shear. Mi~ for 5 minlltes.
2. Add the com syrup to the gurn solution and CO.~ C mi~in~ for 2 more ...i~ cs o 3. Blend the citric acid, sodiurn citrate and ascorbic acid together.
Mix this blend into the peach puree.
4. Add the peach puree to the gum com syrup solution and miX for 3 .~.utes.
5. Bottle and store nectar under refrigerated conditions.
Peach puree was oht~i~.c~ by ble~in& canned cling peaches in a food proccssor. The com syrup used was 5S DE high fructose com 20 syrup produc~ by Staley. Tbe levels of citric acid and com syrup were chosen to match the solids and pH of the Kcms product. Ascorbic acid was added to slow o~idation discoloration of thc product.
A viscosity of about 32 cP at S0 s-l @ 6C is desirable for a peach ncctar bcvcrage.
2s Five parts CMC to I part KELCOGEL F was uscd to stabilizc tbc ncctar. KELCOLOID LVF was uscd at a level cqual to ~e CMC for background ~,iscosity and flavor ~hqnc~ t~ No h~tin~ was ~qu~d.
Wbcn thc blcnd was uscd at 0.1 1% total Co~ ,ation, a 30 viscosity of 3S cP at S0 s-l and 6C ~s~lte~ Visc~sit~ of tbc bcverage, as a function of shcar ratc, is sbown in Figure 3.
~D ~E~
PCT1~S 94l 0~ 0 ~ 3 K~130YP
-- ~PEA/Us l4 N~
1 5 \
Significant settling (>20%) wa~i observed in the control with no 25 stabilizer co~ e.lt, as wcll as the samples c~ ing either CMC alone or KELCOLOID LVF alone. Approximately 2% scttling was measured in the ncctar CG..~ .& KELCOGEL F alone. Gellan gum alone does not provide cnough structure to prevent settling.
Aftcr 100 hours, no ~nlin~ was obscrved in the beverage 30 co..~;..;..g ~e blcnd of KELCOGEL PC and CMC. Also, aft~r 100 hours, no settling was observed` in the beverage col,t~ .g the blend of KELCOGEL PC/CMC/PGA.
,~ 9HE~
Citrus Punch Formulation Ouantity Ingredients GramsPercent Water deionized 381.09176.2182 High fructose corn syrup 55DE 64.4012.8800 Citrus Juice Concentrate 50.0010.0000 Citric acid 3.03 0.6060 Sodium Citrate 0.795 0.1590 Carboxymethylcellulose CMC 7HF 0.24 0.0480 Concentrated Orange Flavor 0.115 0.0230 Ascorbic acid 0.19 0.0380 KELCOLOID LVF 0.12 0.0240 KELCOGEL F gellan gum 0.019 0.003 Total 500.0100.000 Procedure 1. Dry blend the CMC, KELCOLOID LVF and the KELCOGEL F
together and add to the deionized water while mixing under high shear. Mix for 5 minutes.
2. Add the corn syrup to the gum solution and continue mixing for 2 more minutes.
3. Add the concentrated orange flavor to the solution and mix for 1 minute.
4. Blend the citric acid, sodium citrate and ascorbic acid together.
Mix this blend into the citrus juice concentrate.
Mix this blend into the citrus juice concentrate.
5. Add the citrus concentrate to the gum corn syrup solution and mix for 3 minlltes.
6. Bottle and store under refrigerated conditions.
This beverage, cont~ining gellan gum, CMC and PGA, o demonstrated good stability.
This beverage, cont~ining gellan gum, CMC and PGA, o demonstrated good stability.
Claims (13)
1. A beverage stabilizing blend composition comprising carboxymethylcellulose and gellan gum in a carboxymethylcellulose:gellan gum weight ratio range of between about 3:1 to 20:1.
2. A beverage stabilizing blend composition of claim 1 comprising carboxymethylcellulose and gellan gum in a carboxymethylcellulose:gellan gum weight ratio range of between about 4:1 to 15:1.
3. A beverage stabilizing blend composition of claim 2 comprising carboxymethylcellulose and gellan gum in a carboxymethylcellulose:gellan gum weight ratio range of between about 5:1 to 10:1.
4. A beverage stabilizing blend composition of claim 1 comprising carboxymethylcellulose, gellan gum, and propylene glycol alginate, wherein the weight ratio of propylene glycol alginate:gellan gum is in the range of between about 3:1 to 20:1.
5. A beverage stabilizing blend composition of claim 4 comprising carboxymethylcellulose, gellan gum, and propylene glycol alginate, wherein the weight ratio of propylene glycol alginate:gellan gum is in the range of between about 4:1 to 15:1.
6. A beverage stabilizing blend composition of claim 5 comprising carboxymethylcellulose, gellan gum, and propylene glycol alginate, wherein the weight ratio of propylene glycol alginate:gellan gum is in the range of between about 5:1 to 10:1.
7. A beverage composition comprising between about 0.06% and 0.3% beverage stabilizing blend of claim 1.
8. A beverage composition comprising between about 0.06% and 0.3% beverage stabilizing blend of claim 2.
9. A beverage composition comprising between about 0.06% and 0.3% beverage stabilizing blend of claim 3.
10. A beverage composition comprising between about 0.06% and 0.3% beverage stabilizing blend of claim 4.
11. A beverage composition comprising between about 0.06% and 0.3% beverage stabilizing blend of claim 5.
12. A beverage composition comprising between about 0.06% and 0.3% beverage stabilizing blend of claim 6.
13. A method for stabilizing a beverage which comprises adding to the beverage a stabilizing blend composition comprising carboxymethylcellulose and gellan gum in a carboxymethylcellulose:gellan gum weight ratio range of between about 3:1 to 20:1.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US053,574 | 1993-04-27 | ||
| US08/053,574 US5376396A (en) | 1993-04-27 | 1993-04-27 | Beverage stabilizing system and process thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA2158867A1 true CA2158867A1 (en) | 1994-11-10 |
Family
ID=21985193
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA002158867A Abandoned CA2158867A1 (en) | 1993-04-27 | 1994-04-12 | Beverage stabilizing system |
Country Status (13)
| Country | Link |
|---|---|
| US (1) | US5376396A (en) |
| EP (1) | EP0697818B1 (en) |
| JP (1) | JPH08509611A (en) |
| AT (1) | ATE195056T1 (en) |
| AU (1) | AU680495B2 (en) |
| CA (1) | CA2158867A1 (en) |
| DE (1) | DE69425433T2 (en) |
| DK (1) | DK0697818T3 (en) |
| ES (1) | ES2149268T3 (en) |
| GR (1) | GR3034560T3 (en) |
| NO (1) | NO954280L (en) |
| PT (1) | PT697818E (en) |
| WO (1) | WO1994024887A1 (en) |
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| FR2714420B1 (en) * | 1993-12-24 | 1996-03-15 | Inst Francais Du Petrole | Process using gellan as a filtrate reducer for water-based drilling fluids. |
| US5736177A (en) * | 1994-03-08 | 1998-04-07 | Fmc Corporation | Cellulose composition, its preparation, and its use in a lipid |
| US5456937A (en) * | 1994-06-24 | 1995-10-10 | Chalupa; William F. | Gellan gum flavor beads |
| CA2191350A1 (en) * | 1994-06-24 | 1996-01-04 | William Fritsche Chalupa | Gellan gum beverage |
| US5576039A (en) * | 1995-02-03 | 1996-11-19 | Bush Boake Allen Inc. | Colored jelly-type substance, method of preparation, and composition containing same |
| US5562939A (en) * | 1995-01-27 | 1996-10-08 | Bush Boake Allen Inc. | Method of suspending inclusions and compositions produced thereby |
| US6106883A (en) * | 1995-01-27 | 2000-08-22 | Bush Boake Allen, Inc. | Method of suspending inclusions |
| EP0861035B1 (en) * | 1995-01-27 | 2004-12-22 | Bush Boake Allen Inc. | Colored jelly-type substance, method of preparation, and composition containing same |
| US5654027A (en) * | 1995-06-06 | 1997-08-05 | Nutrasweet Company | Concentrated gellan gum dispersion for use in fluid gel applications |
| US5641532A (en) * | 1995-12-15 | 1997-06-24 | The Procter & Gamble Company | Beverages having stable flavor/cloud emulsions in the presence of polyphosphate-containing preservative systems by including gellan gum |
| WO1997034502A1 (en) * | 1996-03-19 | 1997-09-25 | Bush Boake Allen Inc. | Shelf-stable pre-gel solution |
| US5869118A (en) * | 1996-11-13 | 1999-02-09 | Abbott Laboratories | Gellan gum to improve physical stability of liquid nutritional products |
| DE19703469C2 (en) * | 1997-01-31 | 2003-10-30 | Wolfgang Von Rhein | Process for the preparation of an oxidation-protected vitamin C preparation |
| US6733780B1 (en) | 1999-10-19 | 2004-05-11 | Genzyme Corporation | Direct compression polymer tablet core |
| US6365218B1 (en) | 2000-02-04 | 2002-04-02 | Abbott Laboratories | Pediatric formula and methods for providing nutrition and improving tolerance |
| US6699977B1 (en) | 2000-06-09 | 2004-03-02 | Cp Kelco Aps | Low methoxyl pectins, processes thereof, and stabilized aqueous systems comprising the same |
| US20020192350A1 (en) * | 2001-04-30 | 2002-12-19 | Hynes Michael P. | Food products |
| US20040062845A1 (en) * | 2001-11-30 | 2004-04-01 | Krawczyk Gregory R. | Beverage emulsion stabilizer |
| US6887508B2 (en) * | 2002-02-20 | 2005-05-03 | Solae, Llc | Protein stabilizing agent |
| JP2003339354A (en) * | 2002-05-23 | 2003-12-02 | Dai Ichi Kogyo Seiyaku Co Ltd | Mineral dispersant, and mineral-dispersed slurry containing the same and mineral-enhanced food |
| DE60305331T8 (en) * | 2002-07-29 | 2009-07-16 | Otsuka Pharmaceutical Co., Ltd. | JELLY BEVERAGE COMPOSITION |
| NZ521401A (en) * | 2002-09-13 | 2005-02-25 | Hawkins Watts Technology Ltd | Stabilised composition adapted to flavour or colour dairy products |
| US20040170739A1 (en) * | 2003-02-27 | 2004-09-02 | Tropicana Products, Inc. | Gelled juice product and method of making the same |
| WO2004110168A1 (en) * | 2003-06-11 | 2004-12-23 | Pepsico, Inc. | Blend comprising gellan, xanthan and pectin, beverages comprising said blend and their preparation |
| US7985418B2 (en) | 2004-11-01 | 2011-07-26 | Genzyme Corporation | Aliphatic amine polymer salts for tableting |
| US8153180B2 (en) | 2005-09-06 | 2012-04-10 | Pepsico, Inc. | Method and apparatus for making beverages |
| BRPI0616078B8 (en) * | 2005-09-15 | 2021-05-25 | Genzyme Corp | powder of an amine polymer pharmaceutical formulation, use of such powder and sachet formulation for amine polymers |
| US20080008814A1 (en) * | 2006-06-22 | 2008-01-10 | Philip Henry Jackson | Acidified Protein Beverages Containing Suspended Particulates and Methods of Making Same |
| US20080227892A1 (en) * | 2007-03-13 | 2008-09-18 | Van Der Wielen Maarten | Paint formulations comprising cellulose ether/network building polymer fluid gel thickeners |
| US20110135786A1 (en) * | 2007-10-26 | 2011-06-09 | The Hershey Company | Cocoa-based exercise recovery beverages |
| US20090110774A1 (en) * | 2007-10-26 | 2009-04-30 | The Hershey Company | High antioxidant levels in cocoa-based beverages |
| US8399039B2 (en) | 2007-11-29 | 2013-03-19 | Nestec S.A. | Shelf stable liquid whitener and process of making thereof |
| JP5627284B2 (en) * | 2010-05-18 | 2014-11-19 | 旭化成ケミカルズ株式会社 | Emulsion dressing |
| AU2011276628B2 (en) | 2010-07-08 | 2014-07-10 | Tropicana Products, Inc. | Stabilizer system for a ready-to-drink whole grain beverage |
| US20120116841A1 (en) * | 2010-11-05 | 2012-05-10 | The Coca-Cola Company | System for modeling drink supply and demand |
| BR112015012219A2 (en) * | 2012-12-03 | 2017-07-11 | Nestec Sa | ready-to-drink chocolate milk drinks comprising stabilizer system |
| US20170105435A1 (en) * | 2014-05-22 | 2017-04-20 | Nestec S.A. | Low-sugar dairy beverages |
| CN106974265A (en) * | 2016-01-19 | 2017-07-25 | 江苏恒瑞医药股份有限公司 | A kind of enteral nutritional composition |
| JP2019004749A (en) * | 2017-06-23 | 2019-01-17 | 日本製紙株式会社 | Cocoa beverage |
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| US3619205A (en) * | 1968-11-20 | 1971-11-09 | Gen Foods Corp | Process of preparing a slush ice beverage concentrate |
| US3736149A (en) * | 1970-11-09 | 1973-05-29 | Monsanto Co | Stabilized flavoring compositions |
| US4326053A (en) * | 1978-12-04 | 1982-04-20 | Merck & Co., Inc. | Polysaccharide S-60 and bacterial fermentation process for its preparation |
| KR830002802B1 (en) * | 1978-12-04 | 1983-12-16 | 제임스 에프 · 너우톤 | Method for preparing polysaccharide S-60 by bacterial fermentation |
| CA1171728A (en) * | 1980-11-19 | 1984-07-31 | Joe R. Deleon | Method for preventing separation in fruit juice containing products |
| US4503084A (en) * | 1983-05-31 | 1985-03-05 | Merck & Co., Inc. | Non-heated gellan gum gels |
| US4980193A (en) * | 1988-06-17 | 1990-12-25 | Fmx Corporation | Microcrystalline cellulose-based stabilizer system for dry mix instant chocolate drink |
| US5112445A (en) * | 1989-06-23 | 1992-05-12 | Merck & Co., Inc. | Gellan gum sizing |
| JPH053773A (en) * | 1991-06-27 | 1993-01-14 | Morinaga & Co Ltd | Production of granular food-containing beverage |
-
1993
- 1993-04-27 US US08/053,574 patent/US5376396A/en not_active Expired - Fee Related
-
1994
- 1994-04-12 ES ES94913407T patent/ES2149268T3/en not_active Expired - Lifetime
- 1994-04-12 AU AU65583/94A patent/AU680495B2/en not_active Ceased
- 1994-04-12 AT AT94913407T patent/ATE195056T1/en not_active IP Right Cessation
- 1994-04-12 PT PT94913407T patent/PT697818E/en unknown
- 1994-04-12 CA CA002158867A patent/CA2158867A1/en not_active Abandoned
- 1994-04-12 WO PCT/US1994/004023 patent/WO1994024887A1/en active IP Right Grant
- 1994-04-12 DE DE69425433T patent/DE69425433T2/en not_active Expired - Fee Related
- 1994-04-12 EP EP94913407A patent/EP0697818B1/en not_active Expired - Lifetime
- 1994-04-12 JP JP6524309A patent/JPH08509611A/en not_active Ceased
- 1994-04-12 DK DK94913407T patent/DK0697818T3/en active
-
1995
- 1995-10-26 NO NO954280A patent/NO954280L/en not_active Application Discontinuation
-
2000
- 2000-10-04 GR GR20000402250T patent/GR3034560T3/en not_active IP Right Cessation
Also Published As
| Publication number | Publication date |
|---|---|
| EP0697818B1 (en) | 2000-08-02 |
| WO1994024887A1 (en) | 1994-11-10 |
| EP0697818A4 (en) | 1996-05-08 |
| AU680495B2 (en) | 1997-07-31 |
| GR3034560T3 (en) | 2001-01-31 |
| US5376396A (en) | 1994-12-27 |
| ES2149268T3 (en) | 2000-11-01 |
| NO954280D0 (en) | 1995-10-26 |
| JPH08509611A (en) | 1996-10-15 |
| DK0697818T3 (en) | 2000-09-04 |
| ATE195056T1 (en) | 2000-08-15 |
| DE69425433D1 (en) | 2000-09-07 |
| AU6558394A (en) | 1994-11-21 |
| EP0697818A1 (en) | 1996-02-28 |
| NO954280L (en) | 1995-10-26 |
| DE69425433T2 (en) | 2001-12-06 |
| PT697818E (en) | 2001-01-31 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| EEER | Examination request | ||
| FZDE | Discontinued | ||
| FZDE | Discontinued |
Effective date: 20040413 |