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`revetement est constitue de plusieurs couches de compositions differentes.
`
`8. Forme de presentation selon Ia revendication 7, caracterisee en ce que des principes actifs incompati·
`bles entre eux sont appliques successivement sur le materiau support, dans des couches separees.
`
`,
`
`5
`
`9. Forme de presentation selon Ia revendication 7, caracterisee en ce qu'une couche de principe actif est
`placee entre au moins deux autres couches qui reglent, par des moyens connus par eux-memes, Ia
`resorption du principe actif dans l'estomaclle tractus intestinal.
`
`10 10. Forme de presentation selon Ia revendication 7, caracterisee en ce que l'on etale, sur Ia couche de
`principe actif, une couche supplementaire qui preserve le principe actif, une couche supplementaire qui
`preserve le lumiere.
`11. Forme de presentation selon l'une quelconque des revendications 1 a 10, caracterisee en ce que l'on
`peut imprimer au verso du materiau support Ia composition du principe actif etfou des informations
`concernant sa prise.
`12. Procede pour pn§parer Ia forme de presentation de medicament des revendications 1 a 11 , caracterise
`en ce que l'on etale, a !'aide de cylindres, une composition contenant le principe actif sur le cote laisse
`non adhesif d'un papier detachable, d'un film detachable ou d'une feuille detachable.
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`

`
`Europaisches Patentamt
`
`European Patent Office
`
`Office european des brevets
`
`@ Publication number:
`
`111111111111111111111111111111111111111111111111111111111111111111111111111
`0 273 069 81
`
`EUROPEAN PATENT SPECIFICATION
`
`@ Date of publication of patent specification: 14.10.92 @ Int. Cl.5: COSB 37/14, A22C 13/00,
`A61 L 15/28, 801 D 71/08
`
`@ Application number: 86118163.4
`
`@ Date of filing: 30.12.86
`
`The file contains technical information submitted
`after the application was filed and not included in
`this specification
`
`@ Glucomannan/polyhydric alcohol composition and film prepared therefrom.
`
`@ Proprietor: UNI COLLOID KABUSHIKI KAISHA
`No. 7-8, Sakurayama 1-chome
`Zushi-shi Kanagawa-ken(JP)
`
`@ Inventor: Kubodera, Masao
`203, Shiba-cho Kanazawa-ku
`Yokohama-shi Kanagawa-ken(JP)
`
`@ Representative: Glawe, Delfs, Moll & Partner
`Patentanwa lte
`Postfach 26 01 62 Liebherrstrasse 20
`W-8000 MUnchen 26(DE)
`
`@ Date of publication of application:
`06.07.88 Bulletin 88/27
`
`@ Publication of the grant of the patent:
`14.10.92 Bulletin 92/42
`
`@ Designated Contracting States:
`DE FR GB
`
`@ References cited:
`EP-A- 0 109 269
`DE-B- 2 148 159
`GB-A- 853 378
`GB-A- 2 048 642
`
`CHEMICAL ABSTRACTS, vol. 97, 1982, page
`487, abstract no. 4931 e, Columbus, Ohio, US
`
`CHEMICAL ABSTRACTS, vol. 100, 1984, page
`530, abstract no. 137715q, Columbus, Ohio,
`us
`
`PATENT ABSTRACTS OF JAPAN, vol. 6, no.
`98 (C-106)[976], 8th June 1982
`
`0
`Note: Within nine months from the publication of the mention of the grant of the European patent, any person
`D.. may give notice to the European Patent Office of opposition to the European patent granted. Notice of opposition
`w
`shall be filed in a written reasoned statement. It shall not be deemed to have been filed until the opposition fee
`has been paid (Art. 99(1) European patent convention).
`
`Rank Xerox (UK) Business Services
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`Description
`
`BACKGROUND OF THE INVENTION
`
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`The present invention relates to a composition having a complex network structure that is formed by
`mixing glucomannan and optionally another natural polysaccharide with a polyhydric alcohol such as
`glycerin or a concentrated solution thereof in the presence of absence of an alkali. The present invention
`also relates to a film prepared from this composition.
`The composition of the present invention can be dissolved in water to form a viscous solution. A film
`formed of this composition is water-resistant and may be given greater strengthand heat-resisting property.
`The film finds utility in various applications such as edible films, semipermeable membranes for separating
`low-molecular weight materials from those having high molecular weights ; wound dressings, and the shells
`of soft capsules.
`The principal use of glucomannan has been to produce konjak by reacting it with an alkali in an
`15 aqueous solution, then heating the reaction product to form a gel. The gel formed bythis method has an
`inhomogeneous structure and finds no utility other than as konjak. Other natural polysaccharides have been
`used in an aqueous solution as thickeners, gelling agents, water retainers, stabilizers, dispersants, emulsifi(cid:173)
`ers, binders, etc.
`Compounds having multiple hydroxyl groups as exemplified by polyhydric alcohols, sugar alcohols,
`20 monosaccharides, dissaccharides and oligosaccharides have been used solely as additives such as
`sweeteners, humectants, softening agents and plasticizers. Moreover, these compounds have been used
`singly and no attempt has been made to allow the natural polysaccharidesto react directly with polyhydric
`alcohols in the presence of a small amount of water.
`Edible films currently available include starch-based waters, gelatin-based collagen film, and pullulan
`films. All of these films except those based on gelatin lack resistance to water. Even gelatin films lack high
`resistance to acid, alkalies and heat. Films formed of cyclodextrins or special proteins obtained by
`extracting nucleic acids, cell membranes, etc. from yeasts are expensive and their high cost is not justified
`by corresponding improvements in water resistance, heat resistance and strength.
`In the production of smoked meat products such as hams and sausages, semipermeable membranes
`such as those made of animal guts, regenerated cellulose or cellulose derivatives are used to allow the
`fragrant and seasoning components in the smoke to penetrate into the meat. However, the supply of animal
`guts is not abundant and, in addition, they lack strength and are not uniform in size. The supply of
`regenerated cellulose and cellulose derivatives is also limited because strict regulations against pollution
`has rendered the construction of new plants practically impossible.
`Gelatin has heretofore been used as the shell matereal of soft capsules for cunfining drugs, flavors or
`seasonings but the user of gelatin is limited to applications where oily substances are employed.
`Electrolytes or low-molecular weight materials have been separated from high-molecular weight materi(cid:173)
`als by such means as electrodialysis, reverse osmosis, and ion-exchange membrane technology. However,
`these methods use a large number of electrodes or require high pressures so that the equipment for
`40 practicing these methods is becoming more and more complex. In order to desalt foods by these methods,
`large-sized equipmentis necessary and it often occurs that other seasoning componentsare eliminated as
`well as the sodium salt with the result that the taste of the food is impaired.
`In the treatment of skin losses due to burns or other external injuries, the affected area is temporarily
`covered to prevent loss of water or body fluids from the wound, or any exudate from the wound is
`45 desplaced to prevent bacterial infection so that the formation of granulations and the epidermis is promoted.
`The films which have been used or attempted to be used for these purposes are formed of such materials
`as silicone rubber, poly -E -caprolactone, poly (vinyl alcohol) , polyamino acids,fibrin membranes, collagen,
`polyurethane and pigskin.
`However, freeze-dried pigskin and other polyamino acid based wound dressings are all made of
`50 polypeptides which are subject to biochemical decomposition. In order to avoid the adverse effects of the
`degradation products which are liberated, these wound dressings have to be replaced at short intervals,
`typically every other day. However, replacement of the wound dressing involves much pain for the patient.
`Furthermore, the film itself has insufficient strength to attain satisfactory coverage. Wound dressings made
`of synthetic resins such as polyurethane and silicone rubber do not have sufficient affinity for the wound
`surface to achieve satisfactory permeation to oxygen and water. Nomal skin generally allows water to be
`evaporated in an approximate amount of 350g/m2 per day, but it has been difficult to prepare synthetic resin
`films that exhibit this amount of water evaporation and which yet has sufficient strength.
`It has been proposed to prepare a composite wound dressing by laminating a polyamino acid based
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`film with a synthetic resin film but this composite film still suffers from the defects of the respective film
`components.
`
`SUMMARY OF THE INVENTION
`
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`The present inventors have found that if glucomannan, either independently or in combination with other
`natural polysaccharides, is mixed with a compound having multiple hydroxyl groups or with a concentrated
`solution thereof in the presence of absence ofan alkali, the respective components react with each other to
`form a composition having a dense three-dimensional structure. The present inventors have also found that
`10 a viscous solution formed by dissolving this composition in water has unique physicochemical properties
`that have been unattainable by glucomannan, other natural polysaccharides or polyhydric alcohols, and that
`various products having the characteristics shown below can be prepared from this composition. The
`present invention has been accomplished on the basis of these findings.
`Firstly, edible films having desirable properties s such as water resistance, heat resistance and strength
`can be prepared from the above-described viscous aqueous solution either directly or after being mixed
`with other foods or food materials. The so prepared films may be eaten as such or used as edible food
`packages.
`Secondly, the viscous aqueous solution may be dried into film form and the resulting film may be used
`in the production of processed meat products (e.g. hams and sausages) as semipermeable membranes
`20 having sufficient strength and heat resistance to withstand smoking condition.
`Thirdly, the viscous aqueous solution may be processed to form a film that is suitable for use as the
`shell of a soft capsule, and using this film, soft capsules capable of confining non-oily drugs, health foods,
`seasonings or flavors can be prepared.
`Fourthly, the film made from the viscous aqueous solution also serves as a high-performance filter
`25 medium that is capable of efficient separation of low-molecular weight substances from high-molecular
`weight substances at reasonably low pressures.
`Fifthly, the membrane formed by drying the viscous aqueous solution into film form is a superior wound
`dressing that achieves close contact with the skin and exhibits superior vapor and oxygen permeation
`without undergoing any biodegradation during prolonged attachment to the skin.
`Sixthly, the viscous aqueous solution cools to provide a gel-like or semifluid foodstuff having unique
`properties.
`
`30
`
`DETAILED DESCRIPTION OF THE INVENTION
`
`35
`
`40
`
`The glucomannan used in the preparation of the composition of the present invention is the polysaccha-
`ride naturally occurring in Amorphophallus Koniac K. Koch which is the rhizome of a plane belonging to
`Colocasia antiquorum; it is composed of particles referred to as idioblasts which range from 0.5 to 1.05 mm
`in length and from 0.37 to 0.5 mm in breadth. The chemical structure of glucomannan is a chain of a 1 : 2
`mixture of glucose and mannose with acetyl and phosphate groups forming pendant ester linkages.
`Illustrative polyhydric alcohols that can be used in the present invention are polhydric alcohols in the
`narrow sense of the term such as propylene glycol and glycerin. These polyhydric alcohols are liquid and
`may be directly used; however, because of their high hygroscopicity they contain water and are in the form
`of concentrated aqueous solutions. Moreover they can be used as water solution of concentration in the
`range of 30 to 90 %. Illustrative sugar alcohols include sorbital, mannitol, maltitol, xylytol and saccharified
`products of reducing sugar. Illustrative monosaccharides include glucose, fructose, galactose and xylose.
`Illustrative disaccharides are saccharose, maltose and lactose. Starches such as sweet potato, potato and
`corn that have been decomposed with enzymes or acids are usable as oligosaccharides, and include di-,
`tri-, tetra-, penta- and hexasaccharides. The polyhydric alcohols listed above, both in the broad and narrow
`sense of the term, which are in a powder form at ordinary temperatures, are used as aqueous solutions
`50 having concentrations in the range of 30-90 wt %, preferably 50-80 wt %, more preferable 65-75wt%.
`Other natural polysaccharides that may be used in the present invention include the following:
`alginic acid which are intracellular polysaccharides in brown algae,
`sodium alginate,
`propylene glycol ester of alginic acid, and
`agar;
`carrageenan which is an intracellular polysaccharide in red algae and is hydrolyzed into D-galactose
`and D-galactose sulfate ester ;
`locust bean gum which is a polysaccharide that is present in the seeds of leguminous locust bean and
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`carob and which is chiefly composed of glucomannan;
`guar gum that is a polysaccharide present in the seed of leguminous guar and which is hydrolyzed into
`galactose and mannose ;
`tamarind seed polysaccharide which is a polysaccharide present in the seed of leguminous Tamarindus
`indica and which is hydrolyzed into glucose, xylose and galactose ;
`--pectin which is a generic term for a group of polysaccarides that are the materials of construction of the
`cell walls of plants such as fruit and vegitables and which are hydrolyzed in to galacturonic acid;
`xanthan gum is a polysaccharide produced by the microorganism Xanthomonas campestris during
`fermantation in the present of glucose and other appropriate essential elements;
`chitin which is one kind of mucopolysaccharides;
`pullulan which has a repeating unit of a -1,6 linkage derived from maltotriose ; and
`cellulose,
`cyclodextrin and
`starches.
`These natural polysaccharides are optionally used in amounts of 0.05 - 20 parts by weight, preferably
`from 0.1 to 10 parts by weight, per part by weight of glucomannan.
`In the present invention, reaction is preferably carried out in the presence of an alkali. Ordinary
`inorganic or organic alkaline substances may be employed and suitable ones inclueded: sodium hydroxide,
`potassium hydroxide, calcium hydroxide, magnesium hydroxide, barium hydroxide, sodium carbonate,
`20 potassium carbonate, calcium carbonate, ammonium carbonate, magnesium carbonate, sodium bicarbonate,
`ammonium bicarbonate, basic amino acids and amines. The addition of these alkalis is generally effective in
`providing films with improved strength and heat resistance.
`Part of the glucomannan and optionally used natural polysaccharides may be replaced by proteins to
`provide composition which generally have improved heat resistance. Solutions of these compositions in
`25 warm water have good mouth feel and can be readily eaten. Illustrative proteins are soybeen protein, wheat
`protein, milk protein, egg white, collagen, decomposed collagen and microbial proteins. Decomposition
`products of these proteins, such as polypeptides and amino acids, may also be used.
`The present invention is characterized by reacting glucomannan directly with at least one compound
`selected
`from among the polyhydric alcohols, sugar alcohols, monosaccharides, disaccharides and
`30 oligosaccharides. The component made of at least one compound selected from polyhydric alcohols, sugar
`alcohols, monosaccharides, disaccharides and oligosaccharides is used in an amount which ranges from
`0.05 to 10 parts by weight, preferably from 0.10 to 5.0 parts by weight, more preferably from 0.15 to 1.0
`part by weight, per part by weight of the powder component made of glucomannan and optionally of other
`natural polysaccharides and proteins. Generally, a higher content of the polyhydric alcohol renders it
`35 difficult for a three-dimensional network to develop.
`The reactants are mixed at a temperature ranging from 5 to 150 o C, preferably from 1 0 to 100 o C,
`more preferably from 20 to 80 ° C. Mixing at low temperatures will cause no problem because the intended
`reaction can be allowed to proceed satisfactorily by heating the mixture in a subsequent step such as
`drying. Generally, mixing at high temperatures provides a composition having a dense structure whereas a
`40 brittle composition having a coarse network results if low mixing temperatures are used.
`The composition formed by mixing the starting materials described above is a powder that is usually
`moist to some extent. A solution of this composition in water is viscous and will solidify irreversibly when
`left to stand at ordinary temperatures, frozen, refrigerated or heated. The properties, in particular the
`strength, heat resistance and the temperature for dissolution in water, of the solidified product can be
`45 altered by proper adjustment of the combination of the starting materials used. Therefore, the solidified
`product can be used as a base for semifluid or gel-like foods such as jelly and jam. Films may be formed
`from the viscous solution by shaping it into a soldified form of a suitable thickness between 1 and 1 ,000 um
`by any of the known techniques such as wet casting, freeze-drying and extrusion molding. Some of the
`films formed by these methods are heat-resistant and heat-sealable. If desired, the viscous solution may be
`coated or sprayed onto a foodstuff and dried to form an edible film on the food.
`Films having thicknesses in the range of 1-1,000 um, preferably 2- 300 um, are useful as semiper(cid:173)
`meable membranes. In a more preferable embodiment, a thin and reinforced semipermeable membrane
`can be formed by preparing a thin fibrous product from an appropriate material such as paper, nonwoven
`fabric, woven fabric or net, then filling the voids in the fibrous product with the filter film of the present
`invention. Filling of the voids in the thin fibrous product may also be achieved by coating the film with the
`viscous solution or submerging the film in the solution, followed by drying of the film.
`Filtration may be achieved by any known technique such as simple filtering under gravity, ultrafiltration
`or reverse osmosis. The filter medium may be an assembly of hollow fibers or a module of a spirally wound
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`sheet.
`In the simplest way, afoodstuff having high sodium chloride concentration is placed on top of the
`semipermeable membrane of the present invention which is in contact with an underlying water layer; in the
`absence of any applied pressure, sodium chloride and other low-molecular weight substances in the upper
`layer will permeate through the membrane to enter the underlying aqueous layer.
`Soy sauce, miso and pickled products contain a large amount of sodium chloride in order to ensure that
`they can be transported long distances or to achieve various purposes such as storage, preservation or
`good manufacturing practice. The filter film of the present invention is capable of allowing the sodium
`chloride content of these food products to be lowered without impairing their taste.
`In producing processed meat products such as hams and sausages, the meat wrapped in a semiper-
`meable membrane must be smoked. Conventionally, the semipermeable membrane is formed of regener(cid:173)
`ated cellulose, cellulose derivatives, alginates, collagen, or sheep or bovine gut. However, as already
`mentioned, these materials have problems in terms of their physical strength and heat resistance, and in
`particular, sheep and bovine guts are not uniform in size and shape and suffer from instability in supply.
`Fibrous products are usually porous and the films prepared by impregnating or coating them with the
`edible composition of the present invention serve as ideal casing materials wherein the semipermeable
`membrane formed of the edible material isreinforced with the fibrous product. Such casing materials may
`be prepared as follows: a fibrous product of a given width is shaped into a tubular base, which is
`continuously impregnated with an aqueous solution of the composition of the present invention and dried to
`form a strong fibrous casing.
`The shell of conventional soft capsules is formed from an aqueous solution of gelatin and glycerin and
`is only capable of confining oily products. The soft capsules formed from an aqueous solution of the
`composition of the present invention are capable of confining not only oily products but also water-soluble
`substances and, hence, are applicable to enlarged areas of use, for instance: (1) water-soluble vitamins
`such as vitamins B1, B2, Bs, B6, B12, niacin folic acid and vitamin C; (2) nutrients such as liquid glycides,
`proteins and minerals; (3) diets formed of soft capsules that incorporate liquid seasonings or flavors and
`which are readily edible after cooking ; and (4) cosmetics in soft capsules that are to be punctured with a
`needle to allow the contents to be used.
`Soft capsules may be prepared from the composition of the present invention as follows : the
`composition is dissolved in water and the solution is allowed to flow out of a spreader box to form a gel
`which is subsequently shaped into a film form, two sheets of the film thus obtained are passed through a
`pair of die rolls to adhere to each other ; a predetermined amount of the content (ie, fill) is forced with a
`pump to obtain a caplule form, which is subsequently dried to form a soft capsule.
`The film prepared in accordance with the present invention is also useful as an ideal wound dressing. It
`swells readily upon absorbing body fluids from a wounded site of the human body but its three-dimensional
`network will remain intact. The film increases in thickness but its area remains the same so as to allow the
`absorbed moisture to be evaporated from its furface. The film supplies the wound surface not only with
`moisture but also with the drug applied onto the outer surface of the film ; at the same time, the film allows
`the unwanted exudate to be liberated on its surface. Therefore, the film does not have to be peeled off until
`40 after the wound has healed. The thickness of the film used as a wound dressing generally ranges from 1 to
`1 ,OOOum, preferably form 5 to 200 um, more preferably from 7 to 50 um.
`When the composition of the present invention is dissolved in water, a vicous solution or slurry with a
`solids content of 2-1 0 % will form and this can be incorporated in a large amount in suitable food materials.
`The incorporated composition will solidify irreversibly be being left to stand at ordinary temperatures,
`frozen, refrigerated or heated. The properties, in particular the strength, heat resistance and the temperature
`for dissolution in water of the solidified product can be altered by properly adjusting the combination of
`starting materials used. Furthermore, the solidifed product retains the tast flavor of the food material
`present.
`The food materials that can be mixed with the viscous solution or paste of the composition of the
`50 present invention are diverse and include: seaweeds ; marine products such as shrimp, cuttlefish, fish (e.g.
`bonito, tuna and salmon) , and fish roe; vegitables such as spinach, cabbage, carrot and pumpkin; fruits
`such as orange, grape, apple and pineapple ; meats such as beef, pork, chicken, and corned beef ;
`processed foods such as cheese, jam, mayonnaise and miso ; seasonings such as soy sauce and sodium
`glutamate ; as well as spices and flavors such as peanut, almond, mustard, pepper, curry, cocoa, coffee an
`chocolate.
`These food materials may be mixed with the viscous solution or slurry of the composition of the present
`invention either directly, or after being conditioned for a given particle size or shape, or after being formed
`into a paste. The mixing ratio of these food material to the glucomannan /polyhydric alcohol composition of
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`the present invention is not limited to any particular value because it largely depends on the type of food
`material used or the specific formulation of the composition. It should however be noted that a preferable
`mixing ratio is such that the mixture can be readily formed into a film, and that the shaped food is easy to
`handle and does not reveal the mouth feel of the composition.
`The aqueous solution of the composition of the present invention is viscous and its properties, in
`particular its strength, heat resistance and temperature for dissolution in water, can be altered by allowing it
`to stand at ordinary temperatures, freezing, refrigerating or heating the same. Therefore, the aqueous
`solution, after being shaped into a gelled block of an appropriate hardness, may be mixed with a non(cid:173)
`alcoholic beverage such as juice or yogurt or foods, and the resulting mixture can be safely heated without
`10 melting to thereby provide a composite dietary product that shows a desirable combination having the sort
`of mouth feed that is possessed by dissimilar components. There is no particular limitation on the size of
`the gel block and its hardness varies with the type of base used: if the base is a liquid material such as
`juice, the moisture content of the block is preferably increased to provide a soft texture, whereas if the base
`is jelly or any other material that has a certain amount of self-retaining property, its moisture content is
`15 decreased to provide a hardness slightly lower than that of the jelly. In either case, the resulting product is
`composed to two dissimilar materials and yet displays good palatability.
`Glucomannan has a complex structure containing various side chains and reactive groups and, because
`of the presence of many hydroxyl groups at high concentrations, glucomannan enters into reaction to form
`a complex matrix even under a substantially water-free condition. The matrix forming reaction will be
`20 enhanced by the presence of an alkali and an even more complex compound will form. In the presence of
`both an alkali and water, the development of a three-dimensional network is further promoted to form an
`irreversibly solidified product, which can be processed to provide a characteristic gel-like base or a coating.
`The present invention is hereinafter described in greater detail with reference to the following examples
`to which the scope of the invention is by no means limited and wherein all parts are on a weight basis.
`
`25
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`EXAMPLE 1
`
`Eight parts of glucomannan was mixed with 2 parts of glycerin for 15 minuites an 70 ° C to form a
`sample of the composition of the present invention which was a somewhat moist powder. Two parts and a
`30 half of this composition were mixed with 97.5 parts of water to form a viscous aqueous solution. This
`solution was coated onto the peel of orange and dried at 50 ° C for 1 hour to provide orange having an
`edible film coating on its peel. This orange and uncoated orange were stored at 25 ° C for 1 0 days.
`Thereafter, the appearance of the two oranges and the mouth feel of their pulp were compared. Compared
`with the uncoated orange, the one having an edible film coat had undergone a smaller degree of water
`35 evaporation and oxidation, retained more luster and experienced less surface discoloration. The pulp of the
`coated orange was fresher and more palatable.
`
`EXAMPLE 2
`
`Three parts of the composition prepared in Example 1 was mixed with 0.04 parts of a vitamin E powder
`(70% natural vitamin E and 30 % emulsifier) and 97 parts of water to form an aqueous solution. An orange
`whose peel was coated with the resulting aqueous solution as in Example 1 was stored at 25 ° C for 15 days
`together with an uncoated orange. The results of comparison of the two oranges were the same as in
`Example 1.
`
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`EXAMPLES 3- 10
`
`The components listed in Table 1 were mixed for 10 minutes at 80 ° C in the amounts also shown in
`Table 1, so as to prepare eight additional samples of the composition of the present invention. Three parts
`50 of each of the samples was mixed with 97 parts of water and the resulting aqueous solutions were cast by
`the wet process to form translucent edible films having thicknesses ranging from 10 to 20 um. The films
`prepared in Examples 3 to 6 were water-resistant and stable in the following solutions: aqueous solutions
`with NaCI concentrations of 5% or more ; acidic aqueous solutions with pH of 2.5 - 4.5; alkaline aqueous
`sloutions with pH of 9.0 - 12.0 ; aqueous solutions with ethanol concentrations of 1 0 % or more. The films
`55 prepared in Examples 7 - 10 were not only water-resistant; they were resistant to hot water and stable in
`aqueous solutions heated to 80 - 1 00 ° C.
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`Table 1
`
`(unit in parts by weight)
`
`E X a m p
`
`I e No.
`
`glucomannan
`
`Q;
`
`()
`.--4()
`
`"0 carrageenan
`·.-i a
`.c agar
`~~ locust bean gum
`~8 xanthan gum
`calcium carbonate
`
`3
`5
`
`3
`
`4
`5
`
`2
`
`7
`
`5
`
`5
`
`5
`
`2
`
`6
`
`5
`
`2
`
`1
`
`calcium hydroxide
`
`0.05
`
`·.-!
`.--4
`Cll
`.!C
`.--4
`ro
`
`sodium
`bicarbonate
`
`glycerin
`
`8
`
`5
`4
`
`0.5
`
`9
`
`5
`
`1
`
`1 0
`
`5
`
`3
`
`1
`
`0.3
`
`0.1
`
`0.5
`
`0.3
`
`sorbitol (70%aq.sol. )
`
`1.5
`
`saccharose
`(80%aq. s 0 l.)
`
`1.5
`
`1.5
`
`1
`
`1
`
`1
`
`1.5
`
`1
`
`EXAMPLE 11
`
`An edible package film 15 urn thick was formed from a composition having the same formulation as
`used in Example 3. Stripped lobster (150g) was wrapped with this film and stored at-25 ° C for 3 months.
`The frozen lobster as wrapped in the film was thawed in a microwave oven and cooked. The cooked lobster
`had the edible film on it but one did not sense any peculiar feel as a result of the presence of the film.
`
`EXAMPLE 12
`
`An edible film 15um thick was formed from a composition having the same formulation as used in
`Example 8. Vegitable salad with dressing was sandwiched between two slices of bread. During subsequent
`storage, the dressing did not permeate into the bread at all. After the strage, the bread was eaten ; it tasted
`good and the taste of the edible film was not sensed.
`
`EXAMPLE 13
`
`Components
`
`Glucomannan
`
`Sodium bicarbonate
`
`Calcium Carbonate
`
`Glycerin
`
`7
`
`Amount ( in parts)
`
`5
`
`0. 1
`0.02
`
`1
`
`5
`
`10
`
`15
`
`20
`
`25
`
`30
`
`35
`
`40
`
`45
`
`50
`
`55
`
`Page 2273
`
`TEVA EXHIBIT 1007
`TEVA PHARMACEUTICALS USA, INC. V. MONOSOL RX, LLC
`
`

`
`EP 0 273 069 81
`
`These components were mixed at 75 ° C for 20 minutes. Three parts of the resulting composition were
`dissolved in 97 parts of water. The aqueous solution was applied continuously to form a uniform coating on
`the inner surface a fluoroethylen resin-coated cylindrical pipe having a diameter of 120 mm. The applied
`coat was dried to form a tubular casing.
`Processed meat was packed into the casing at a pressure of up to 2 kg/cm2 without causing its
`disruption. The packed meat was smoked and sterilized by heating in hot water (80 ° C) for 2 hours to
`produce a satisfactory ham.
`
`EXAMPLE 14
`
`Components
`
`Glucomannan
`
`Agar
`
`Calcium carbonate
`
`Sodium citrate
`
`Sorbitol (70% aq. sol.
`
`Amount (in parts)
`
`5
`
`0.5
`
`0.5
`
`0.3
`
`1
`
`5
`
`10
`
`15
`
`20
`
`25
`
`30
`
`These components were mixed at 80 ° C for 10 minuites. Three parts and a half of the resulting
`composition were dissolved in 96.5 parts of water to form a viscous aqueous solution. A sheet of porous
`paper having a thickness of 100 um was prepared, with wood pulp and cotton linter being used as chief
`components. The two side edges of the sheet were adhered together to form a tubular base. The wall of
`this base was impregnated with the previously prepared viscous aqueous solution and dried to form a
`casing that was formed of a sample of the film