Classifications

• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K9/00—Medicinal preparations characterised by special physical form
  • A61K9/20—Pills, tablets, discs, rods
  • A61K9/28—Dragees; Coated pills or tablets, e.g. with film or compression coating
  • A61K9/2806—Coating materials
  • A61K9/2833—Organic macromolecular compounds
  • A61K9/286—Polysaccharides, e.g. gums; Cyclodextrin
• • A—HUMAN NECESSITIES
  • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
  • A23G—COCOA; COCOA PRODUCTS, e.g. CHOCOLATE; SUBSTITUTES FOR COCOA OR COCOA PRODUCTS; CONFECTIONERY; CHEWING GUM; ICE-CREAM; PREPARATION THEREOF
  • A23G3/00—Sweetmeats; Confectionery; Marzipan; Coated or filled products
  • A23G3/34—Sweetmeats, confectionery or marzipan; Processes for the preparation thereof
  • A23G3/343—Products for covering, coating, finishing, decorating
• • A—HUMAN NECESSITIES
  • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
  • A23G—COCOA; COCOA PRODUCTS, e.g. CHOCOLATE; SUBSTITUTES FOR COCOA OR COCOA PRODUCTS; CONFECTIONERY; CHEWING GUM; ICE-CREAM; PREPARATION THEREOF
  • A23G3/00—Sweetmeats; Confectionery; Marzipan; Coated or filled products
  • A23G3/34—Sweetmeats, confectionery or marzipan; Processes for the preparation thereof
  • A23G3/50—Sweetmeats, confectionery or marzipan; Processes for the preparation thereof characterised by shape, structure or physical form, e.g. products with supported structure
  • A23G3/54—Composite products, e.g. layered, coated, filled
• • 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
  • A23G4/00—Chewing gum
  • A23G4/06—Chewing gum characterised by the composition containing organic or inorganic compounds
  • A23G4/062—Products for covering, coating, finishing, decorating
• • 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
  • A23G4/00—Chewing gum
  • A23G4/18—Chewing gum characterised by shape, structure or physical form, e.g. aerated products
  • A23G4/20—Composite products, e.g. centre-filled, multi-layer, laminated
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
  • A61K47/06—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite
  • A61K47/26—Carbohydrates, e.g. sugar alcohols, amino sugars, nucleic acids, mono-, di- or oligo-saccharides; Derivatives thereof, e.g. polysorbates, sorbitan fatty acid esters or glycyrrhizin
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
  • A61K47/30—Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
  • A61K47/36—Polysaccharides; Derivatives thereof, e.g. gums, starch, alginate, dextrin, hyaluronic acid, chitosan, inulin, agar or pectin
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K9/00—Medicinal preparations characterised by special physical form
  • A61K9/0012—Galenical forms characterised by the site of application
  • A61K9/0053—Mouth and digestive tract, i.e. intraoral and peroral administration
  • A61K9/0056—Mouth soluble or dispersible forms; Suckable, eatable, chewable coherent forms; Forms rapidly disintegrating in the mouth; Lozenges; Lollipops; Bite capsules; Baked products; Baits or other oral forms for animals
  • A61K9/0058—Chewing gums
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K9/00—Medicinal preparations characterised by special physical form
  • A61K9/20—Pills, tablets, discs, rods
  • A61K9/28—Dragees; Coated pills or tablets, e.g. with film or compression coating
  • A61K9/2806—Coating materials
  • A61K9/282—Organic compounds, e.g. fats
  • A61K9/2826—Sugars or sugar alcohols, e.g. sucrose; Derivatives thereof
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K9/00—Medicinal preparations characterised by special physical form
  • A61K9/20—Pills, tablets, discs, rods
  • A61K9/28—Dragees; Coated pills or tablets, e.g. with film or compression coating
  • A61K9/2893—Tablet coating processes

Definitions

• the present invention relates to an improved coating process, as well as a coating composition useful for its implementation.
• the present invention also relates to a solid form coated using this process or this composition.
• Dragéification is an operation used in particular in confectionery or in pharmacy, which consists in creating a more or less hard crystallized coating (“hard” or “soft coating”) on the surface of solid products or pulverized, in order to protect them for various reasons or to make them visually or taste attractive.
• the coating of the solid form (core) is conventionally carried out in a tank rotating around its axis and called a dredger, inside which there is a plurality of cores forming a moving mass, on the surface of which is distributed in the liquid state the constituent material of the future envelope ("liquid or sugar-coating syrup").
• the hard and crystalline coating is obtained by applying this liquid and evaporating the water brought by it.
• the coating syrup is mainly composed of one or even several crystallizable materials, and also conventionally contains binding agents such as gum arabic or gelatin, dyes, opacifiers such as Ti02, mineral fillers such as talc , silica, calcium carbonate, intense sweeteners, aromas, vitamins, active ingredients.
• binding agents such as gum arabic or gelatin, dyes, opacifiers such as Ti02, mineral fillers such as talc , silica, calcium carbonate, intense sweeteners, aromas, vitamins, active ingredients.
• Coating is a relatively laborious process, including a large number of successive steps.
• Each of these steps also called “coating cycles”, typically includes an application phase, generally by spraying a coating syrup on the cores, a rotating phase of distribution of said syrup on the cores also called pause time, and a drying phase of each new layer of syrup carried out by blowing hot and dry air.
• Coating makes it possible to obtain solid forms having a particularly attractive appearance, but lacks flexibility as regards its implementation and as regards the visuals which it is possible to obtain.
• the present invention thus aims to provide compositions for coating, in particular for use according to the method of the aforementioned patent application WO 20020/128290 which are composed of renewable materials.
• Another object of the present invention is to provide compositions for coating which do not yellow over time and/or which are free of gum arabic.
• the present invention thus has as its first object a coating process, comprising:
• step (b) concomitant with step (a), of drying said sprayed coating liquid
• step (c) of collecting the coated solid forms thus obtained characterized in that said coating liquid comprises a hydrolyzed and functionalized starch.
• said crystallizable materials comprise xylitol.
• said hydrolyzed and functionalized starch is functionalized with alkyl groups having 1 to 5 carbon atoms.
• said hydrolyzed and functionalized starch is chosen from hydroxypropyl starch, acetylated starch, hydroxyethyl starch, or a mixture thereof.
• the present invention also relates to a coating liquid consisting of:
• the present invention also relates to the use of such a coating liquid for coating solid forms.
• the present invention also relates to a coated solid form comprising at least one coating layer obtained from such a coating liquid.
• Pulverulent composition for the coating of solid forms consisting of:
• the present invention also relates to the use of such a powdery composition for coating solid forms.
• the present invention also relates to a coated solid form comprising at least one coating layer obtained from such a powdery composition.
• FIG. 1 shows the maximum solubility of various crystallizable materials in water, as a function of solution temperature.
• the invention thus relates firstly to a coating process, comprising: - a step (a) of spraying a coating liquid comprising crystallizable materials onto a bed of moving cores, said cores being placed in a chamber equipped with a perforated rotary drum, and said spraying being carried out by means of at least one compressed air nozzle;
• step (b) concomitant with step (a), of drying said sprayed coating liquid
• step (c) of collecting the coated solid forms thus obtained characterized in that said coating liquid comprises a hydrolyzed and functionalized starch.
• solid form conventionally refers to any solid presentation of sugar-coated substances (“solid sugar-coated form”) or capable of undergoing a sugar-coating operation (“core”).
• Typical examples are tablets, hard capsules, soft capsules, pellets, microspheres, granules, seeds, biscuits, breakfast cereals, confectionery such as chewing gum, boiled sugars , chews, gummies, chocolates, fruits and vegetables, or even products in the form of powders and/or crystals.
• These solid forms can be, for example, for food, pharmaceutical, veterinary or cosmetic purposes. They can be intended for humans, adults or children, or for animals. They may also be products for chemical or agrochemical use, although solid forms intended to be ingested (“oral solid forms”) are preferred in the context of the present invention.
• these solid forms are chosen from tablets and chewing gums.
• the coating liquid of the invention comprises crystallizable materials and a functionalized hydrolyzed starch.
• crystallizable materials in coating is conventionally understood to mean substances capable of crystallizing by evaporation of the solvent in which they are dissolved. It is these crystallizable materials which form the crystalline coating targeted by the coating.
• the crystallizable materials of the coating liquid in accordance with the description comprise at least one substance chosen from sugars and sugar alcohols, preferably chosen from monomers and dimers.
• the sugars and sugar alcohols represent at least 50%, preferably at least 70%, preferably at least 90% by weight of the crystallizable materials.
• the crystallizable materials consist entirely of substances chosen from sugars and sugar alcohols.
• these sugars and sugar alcohols are chosen from xylitol, sucrose, erythritol, mannitol, dextrose, isomalt, maltitol or optionally a combination thereof.
• these crystallizable materials include xylitol.
• the crystallizable materials of the coating liquid consist entirely of a single substance, preferably xylitol.
• the coating process in accordance with the description comprises:
• step (a) of spraying a coating liquid onto a bed of moving cores said cores being placed in a chamber equipped with a perforated rotary drum, and said spraying being ensured by means of at least one nozzle compressed air;
• step (b) concomitant with step (a), of drying said sprayed coating liquid
• step (c) of collecting the coated solid forms thus obtained characterized in that said coating liquid comprises xylitol and a hydrolyzed and functionalized starch.
• the concentration of crystallizable materials in the coating liquid is chosen so that the crystallizable materials are dissolved in said coating liquid.
• the coating liquid in accordance with the description has a concentration of crystallizable materials of less than or equal to 90%, this percentage being expressed by weight relative to the total weight of said coating liquid. coating.
• this concentration is less than or equal to 80%, preferably less than or equal to 70%.
• This concentration is preferably greater than or equal to 20%, preferably greater than or equal to 30%, preferably greater than or equal to 40%, preferably greater than or equal to 50%. It is for example approximately equal to 60%.
• the maximum concentration of crystallizable materials naturally depends on the nature of these crystallizable materials, as well as the temperature of the coating liquid.
• the concentration of crystallizable materials in a coating liquid at 20° C.
• composition of crystallizable materials consists of sucrose, less than or equal to 15% when it is mannitol, less than or equal to 61% in the case of maltitol, less than or equal to 63% in the case of xylitol, less than or equal to 25% in the case of isomalt, less than or equal to 27% in the case of erythritol, less than or equal to 48% in the case of dextrose.
• the content of crystallizable materials or xylitol of the coating liquid is greater than or equal to 50% by weight relative to the total weight of ingredients other than the solvent of the coating liquid.
• This content is preferably greater than or equal to 70%, preferably greater than or equal to 80%, preferably greater than or equal to 90%, preferably greater than or equal to 95%, for example equal to approximately 99%.
• the coating liquid in accordance with the description has a content of crystallizable materials, in particular xylitol, of less than or equal to 80%, preferably less than or equal to 70%, preferably less than or equal to 60%, this percentage being expressed by weight relative to the total weight of the coating liquid.
• This content is preferably greater than or equal to 20%, preferably greater than or equal to 30%, preferably greater than or equal to 40%, preferably greater than or equal to 50%. It is for example equal to about 59%.
• the coating liquid of the invention also has a hydrolyzed and functionalized starch.
• starch conventionally denotes starch isolated from any suitable botanical source, by any technique well known to those skilled in the art. Isolated starch generally contains no more than 3% impurities; said percentage being expressed as dry weight of impurities relative to the total dry weight of isolated starch. These impurities typically include proteins, colloidal materials and fibrous residues.
• a suitable botanical source includes, for example, legumes, cereals and tubers. The starches according to the description can be derived for example from legumes (for example pea), cereals (for example corn, rice, wheat, oats) and tubers (for example potato, tapioca).
• the hydrolyzed and functionalized starch in accordance with the description is derived from a legume and/or cereal starch, preferably from peas or corn, preferably from peas, preferably from smooth peas.
• the hydrolyzed and functionalized starch in accordance with the description in particular when it is derived from a pea starch, is derived from a starch having an amylose content of 20 to 50%, from preferably from 30 to 45%, preferably from 30 to 40%, for example equal to approximately 35%; these percentages being expressed as dry weight of amylose relative to the total dry weight of starch.
• amylose content can be determined by a person skilled in the art by potentiometric analysis of the iodine absorbed by the amylose to form a complex.
• the hydrolyzed and functionalized starch in accordance with the description in particular when it is derived from a corn starch, is derived from a starch having an amylose content greater than 5%, from preferably from 10 to 40%, preferably from 15 to 35%, preferably from 20 to 30%, for example equal to about 25%.
• the hydrolyzed and functionalized starches in accordance with the description can be hydrolyzed by any suitable technique, for example by acid treatment, heat treatment, enzymatic treatment or a combination thereof. They may be dextrins, including maltodextrins or pyrodextrins. “Maltodextrins” conventionally designate hydrolyzed starches having a dextrose equivalent of 2 to 20. They are generally obtained by acid or enzymatic hydrolysis. “Pyrodextrins” are conventionally obtained from the action of high temperatures (generally at least 100°C), combined or not with the action of an acid or a base, in the presence of small quantities of water.
• hydrolyzed starches in accordance with the description are obtained by acid hydrolysis.
• functionalized hydrolyzed starches in accordance with the description are not pyrodextrins.
• Hydrolyzed starches must be clearly differentiated from glucose, glucose syrups and cyclodextrins, the hydrolysis rate of which is too high to still be referred to as “starches” as conventionally understood by a person skilled in the art.
• glucose, glucose syrups and cyclodextrins are not hydrolyzed starches within the meaning of the invention.
• the hydrolyzed and functionalized starch in accordance with the description can be defined by its weight average molecular weight (Mw) which is preferably less than 10,000 kDa as determined by steric exclusion chromatography (HPSEC) with refractometric (RI) and coupled light scattering (MALLS) detection.
• Mw weight average molecular weight
• HPSEC steric exclusion chromatography
• RI refractometric
• MALLS coupled light scattering
• the Mw is determined by the following method: samples of hydrolyzed and functionalized starch are diluted in a mixture of dimethylsulfoxide and 0.1 M sodium nitrate.
• the hydrolyzed and functionalized starch in accordance with the description has a Mw of less than or equal to 9000 kDa, preferably less than or equal to 7000 kDa, preferably less than or equal to 5000 kDa, preferably less than or equal to 4000 kDa.
• the hydrolyzed and functionalized starch in accordance with the description has a viscosity in water of less than 10,000 mPa.s at 20° C., at a shear rate of 100 s-1, determined on a solution aqueous comprising 10% dry weight of said starch.
• the viscosity is determined on a rheometer (for example Physica MCR301, Anton Paar) with a cone-plane geometry of 5 cm 1° (CP50).
• a rheometer for example Physica MCR301, Anton Paar
• CP50 cone-plane geometry of 5 cm 1°
• the temperature is regulated for example via Peltier.
• the 10% dry starch solution is maintained for one minute at equilibrium at 20°C.
• Shear rates ranging from 0.006 to 1000 s _1 (log) are applied in 3 minutes at 20°C.
• this viscosity (at 10% dry; 20°C; a shear rate of 100 s-1) is less than or equal to 5000 mPa.s, preferably less than or equal to 1000 mPa.s, preferably less or equal to 500 mPa.s, preferably less than or equal to 100 mPa.s, preferably less than or equal to 50 mPa.s. It is preferably greater than or equal to 1 mPa.s, preferably greater than or equal to 10 mPa.s, preferably greater than or equal to 20 mPa.s, preferably greater than or equal to 30 mPa.s, preferably greater than or equal to equal to 40 mPa.s. It is for example equal to about 42 mPa.s.
• the hydrolyzed starch in accordance with the description is also functionalized. In other words, it comprises functional groups grafted to at least one of its hydroxyl functions. In other words, the expression “functionalized” within the meaning of the invention excludes crosslinking.
• the functionalized starch in accordance with the description is etherified and/or esterified, preferably etherified.
• the starch in accordance with the description is functionalized with alkyl groups having 1 to 5 carbon atoms, preferably 2 to 4 carbon atoms, preferably 2 or 3 carbon atoms, preferably 3 carbon atoms.
• the alkyl group is an aliphatic alkyl group, more preferably a saturated aliphatic group.
• the functionalized starch in accordance with the description is chosen from hydroxypropyl starch, acetylated starch, hydroxyethyl starch, or a mixture thereof. It is preferably hydroxypropylated starch, preferably used alone.
• the hydroxypropyl starch in accordance with the description can be obtained, for example, by etherification with propylene oxide.
• the hydrolyzed hydroxypropyl starch in accordance with the description preferably has a content of hydroxypropyl groups of 0.5 to 10%; said percentage being expressed as dry weight of hydroxypropyl groups relative to the total dry weight of hydrolyzed hydroxypropyl starch.
• the content of hydroxypropyl groups can be determined by those skilled in the art, for example by Proton Nuclear Magnetic Resonance (proton NMR), preferably according to a method in accordance with the European Pharmacopoeia ("STARCH, HYDROXYPROPYL PREGELATINIZED”) such as in force on 1st 2021. It is preferably from 0.5 to 9%, preferably from 0.5 to 8%, preferably from 0.5 to 7%, for example equal to about 7%.
• the functionalized starch in accordance with the description can be etherified or esterified or both etherified and esterified. However, it is preferably either esterified or etherified. It can be substituted (that is to say functionalized) by groups of the same nature or of different nature. However, it is preferably substituted by groups of the same nature, for example and preferably, substituted only by hydroxypropyl groups.
• This solubility can for example be determined according to the following protocol: in a 250 ml beaker, 200 ml of distilled water are added. 5 g of starch are added and the mixture is homogenized by magnetic stirring for 15 minutes. The resulting solution/suspension is centrifuged for 10 minutes at 4000 rpm. 25 mL of the supernatant are removed and introduced into a crystallizer and placed in an oven at 60° C., until the water has evaporated. It is then placed in an oven at 103°C ⁇ 2°C for 1 hour. The residue is placed in a desiccator for cooling to room temperature and then weighed for the calculation of the solubility by dry weight.
• a starch having such cold solubility in water can be conventionally obtained from insoluble starch by cooking and/or hydrolysis of said insoluble starch. Said cooking can typically be carried out by heating a suspension of starch, so that the insoluble granules burst and dissolve. Functionalized starch conforming to the description being hydrolyzed, it is sometimes cold soluble in water without requiring additional treatment, depending of course on the level of hydrolysis.
• the hydrolyzed and functionalized starch in accordance with the description may undergo other chemical and/or physical modifications than the preferred ones set out above, provided that the latter do not contravene the properties sought here, in particular concerning the quality of the solid forms. coated sugars obtained and/or the workability of the process.
• the hydrolyzed and functionalized starch in accordance with the description is preferably not further modified.
• the hydrolyzed and functionalized starch in accordance with the description is a product of CAS No. 9049-76-7.
• the hydrolyzed and functionalized starch in accordance with the description complies with the European Pharmacopoeia (“STARCH, HYDROXYPROPYL PREGELATINIZED”) in force on March 1, 2021.
• Particularly useful functionalized hydrolyzed starches are commercially available. Mention may be made, for example, of the hydrolyzed hydroxypropylated starches LYCOAT® RS 720 (CAS No. 113894-92-1), or LYCOAT® RS 780 (CAS No. 113894-92-1) marketed by the applicant.
• the functionalized hydrolyzed starch content of the coating liquid is greater than or equal to 0.1%, preferably greater than or equal to 0.2%, preferably greater than or equal to 0.3%, preferably greater than or equal to 0.4%, this percentage being expressed by weight relative to the total weight of ingredients other than the solvent of the coating liquid.
• This content is preferably less than 5.0%, preferably less than or equal to 4.0%, preferably less than or equal to 3.0%, preferably less than or equal to 2.0%, preferably less than or equal at 1.0%. It is for example about 0.1 to about 1.0%, or about 0.5 to about 0.9%.
• the weight ratio of crystallizable materials / functionalized hydrolyzed starch is greater than or equal to 50, preferably greater than or equal to 70, preferably greater than or equal to 90, preferably greater than or equal to 100, preferably greater than or equal to 110, preferably greater than or equal to 120, preferably greater than or equal to 130, preferably greater than or equal to 140, preferably greater than or equal to 150, preferably greater than or equal to 170, preferably greater than or equal to 190. It is preferably less than or equal to 300, preferably less than or equal to 250, preferably less than or equal to 230, preferably less than or equal to 210. It is for example approximately equal to 200.
• the coating liquid in accordance with the description has a content of ingredients other than the solvent of less than or equal to 80%, preferably less than or equal to 70%, preferably less than or equal to 65%, this percentage being expressed by weight relative to the total weight of the coating liquid.
• This content is preferably greater than or equal to 20%, preferably greater than or equal to 30%, preferably greater than or equal to 40%, preferably greater than or equal to 50%, preferably greater than or equal to 55%. It is for example equal to approximately 60%.
• the coating liquid in accordance with the description is typically polar, and preferably comprises water as the majority solvent, most preferably as the only solvent.
• the coating process in accordance with the description uses a single coating liquid, that is to say that the coating liquid has a constant formulation. throughout the coating period.
• the coating liquid in accordance with the description may comprise other substances than those mentioned before, as long as this does not contravene the properties sought here, in particular concerning the quality of the solid coated forms obtained and/or the workability of the process.
• Such other compounds are for example:
• binders such as gum arabic, polyvinyl alcohol
• the functionalized hydrolyzed starch represents at least 50% by weight of the binding agents, preferably at least 60%, preferably at least 70%, preferably at least least least 80%, preferably at least 90%, preferably about 100%.
• the functionalized hydrolyzed starch in accordance with the description is the sole binder of the coating liquid.
• the coating liquid in accordance with the description is preferably free of PVA or free of gum arabic, preferably free of both PVA and gum arabic.
• the crystallizable materials other than xylitol are conventionally chosen from sugars and sugar alcohols, conventionally chosen from monomers and dimers, preferably from mannitol, sucrose, erythritol, dextrose, isomalt , maltitol or optionally a combination thereof.
• the xylitol represents at least 50% by weight of the sum of the crystallizable materials and/or of the sum of the sugars and sugar alcohols.
• this xylitol content is greater than or equal to 60%, preferably greater than or equal to 70%, preferably greater than or equal to 80%, preferably greater than or equal to 90%, preferably equal to approximately 100%.
• the coating liquid in accordance with the description is free of crystallizable materials other than xylitol and/or free of sugars, and/or free of sugar alcohols other than xylitol.
• the coating liquid in accordance with the description also comprises an opacifying agent, preferably titanium dioxide.
• an opacifying agent preferably titanium dioxide.
• the content of functionalized opacifying agents of the coating liquid is greater than or equal to 0.1%, preferably greater than or equal to 0.3%, preferably greater than or equal to 0.5%, preferably greater than or equal to 0.7%, preferably greater than or equal to 0.9%, this percentage being expressed by weight relative to the total weight of ingredients other than the solvent of the coating liquid.
• this content of opacifying agents, in particular titanium dioxide is less than or equal to 20.0%, preferably less than or equal to 15.0%, less than or equal to 10.0%, less than or equal to 5.0%. This content is for example approximately equal to 1%.
• the coating liquid in accordance with the description comprises an amount of less than 5.0% of pigments and/or dyes, preferably less than or equal to 4.0%, preferably less than or equal to 3.0% , preferably less than or equal to 2.0%, preferably less than or equal to 1.0%, for example equal to approximately 0.0%; these percentages being expressed by weight relative to the total weight of ingredients other than the solvent of the coating liquid.
• the coating liquid in accordance with the description consists of: (a) from 40 to 80%, preferably from 45 to 75%, preferably from 50 to 70%, preferably from 55 to 65%, for example about 60%, of ingredients other than the solvent consisting of:
• the present invention also relates to the use of such a coating liquid for the coating of solid forms.
• said coating is carried out according to the method in accordance with the description as described before.
• the coating process in accordance with the description may also comprise a step of preparing the coating liquid, preferably by mixing a ready-to-use liquid with a suitable solvent, preferably water.
• this ready-to-use composition as defined before for the coating liquid, with the exception of the solvent which is of course omitted.
• the ready-to-use product in accordance with the description is typically in the form of a powder mixture.
• the ready-to-use product in accordance with the present description is a powder composition consisting of:
• xylitol preferably from 95.0% to 99.5%, preferably from 96.0% to 99.0%, preferably from 97.0% to 99.0 %, preferably from 98.0% to 99.0%, for example 98.5%;
• hydrolyzed and functionalized starch preferably from 0.2 to 2.0%, preferably from 0.3 to 1.0%, preferably from 0.4 to 0, 8%, preferably 0.4 to 0.7%, preferably 0.4 to 0.6%, for example 0.5%;
• opacifying agent preferably from 0.5 to 2.0%, for example 1.0%
• the present invention also relates to the use of such a powdery composition for the coating of solid forms.
• said coating is carried out according to the method in accordance with the description as described before.
• the equipment used to implement the method in accordance with the description typically comprises a coating liquid storage unit, comprising at least one outlet for transporting the coating liquid to a device for spraying the coating liquid.
• This transport can for example be ensured by means of a peristaltic pump.
• the coating liquid is applied via the spray device to a bed of cores contained in the chamber, said chamber being provided with a rotating drum for setting said bed of cores in motion. More specifically, the drum is a perforated rotary drum, and the spray device chosen comprises at least one compressed air nozzle.
• the equipment further includes an air inlet at the drum chamber, for drying the coating liquid. The exit of the drying air takes place in particular through the perforations of the rotating drum, in particular by suction of the air from the chamber.
• the elements of the equipment useful for the method in accordance with the description are commercially available, and their arrangement does not represent any particular difficulties for the person skilled in the art.
• the temperature of the coating liquid in accordance with the description is typically chosen so that the crystallizable materials, in particular xylitol, are well dissolved in said coating liquid to be sprayed. This temperature is therefore also a function of the quantity of crystallizable materials present in the liquid.
• the temperature of the coating liquid is lower than 90°C, preferably lower than 80°C, preferably lower than 70°C, preferably lower than 60°C, preferably lower than 50°C, preferably below 40°C, preferably below 30°C.
• This temperature is preferably at least 10°C, preferably at least 15°C, or even at least 20°C. It preferably corresponds to the ambient temperature, which typically varies from about 20 to about 25°C.
• the temperature of the solvent used for the coating liquid is preferably as defined above in this paragraph.
• the temperature of the coating liquid will generally be lower, due to the high enthalpy of dissolution of xylitol.
• the coating liquid will generally have a temperature of 10 to 15°C after dissolving the xylitol in water, and 15 to 20°C C during coating.
• the coating liquid is kept under stirring during its use.
• the speed of rotation is chosen so as to maintain the homogeneity of the coating liquid.
• the coating liquid is stored in a simple envelope storage unit, and/or the equipment useful for the process in accordance with the description is free of a device for heating the coating liquid.
• the method according to the description does not necessarily require the use of high temperatures of coating liquids, these devices are not mandatory in the method according to the description.
• the number of compressed air nozzles used is conventionally chosen according to the dimensions of the coating chamber, according to the manufacturer's recommendations. This number of nozzles is typically 1 to 2 nozzle(s) per slice of 40 cm in diameter of the coating chamber. This number of nozzles varies for example from 1 to 10, for example from 1 to 6.
• the process according to the description uses only compressed air nozzles.
• the nozzles used in accordance with the description have an orifice having a diameter chosen from a range ranging from 0.1 to 2.8 mm, preferably from 0.1 to 2.5 mm, preferably from 0 ,1 to 2.2 mm, for example 0.3 to 2.0 mm, or 0.5 to 1.8 mm or 0.5 to 1.5 mm, or 0.5 to 1.2 mm, or 0.5 to 1.0 mm.
• the spray rates are chosen in a range going from 1 to 20 g/min/kg of kernels, preferably from 1 to 15 g/min/kg of kernels, preferably from 2 to 15 g/ min/kg kernels, preferably 5 to 10 g/min/kg kernels.
• the rate chosen for the spraying is increased during the coating.
• the inventors have observed that for certain crystallizable materials, the use of low flow rates at the start of coating makes it possible to promote the first phase of crystallization which takes place at the surface of the cores. The flow rate can then be increased so as to accelerate the coating.
• the atomization pressure and the crushing pressure are adjusted according to the flow rate and the nozzle orifice, and according to the manufacturer's recommendations. This flow rate and nozzle orifice typically depends on the size of the equipment used. These atomization and crushing pressures are typically chosen in a range ranging from 0.5 to 4.0 bars, preferably ranging from 0.5 to 3.5 bars, for example from 0.7 to 2.5 bars. for the atomization pressure, and/or from 0.7 to 3.5 bars for the crushing pressure.
• the atomization pressure is for example approximately equal to 1.
• the coating liquid is sprayed onto a bed of cores set in motion by means of a rotating drum.
• the nature of these nuclei is preferably as defined before for the forms solids; these are, for example, tablets or chewing gums.
• These cores can be completely bare, or be coated with one or more layers, for example of gumming, film-coating, or even coating, said layers being preferably obtained in the same equipment as that used for the coating process in accordance with the description.
• the speed of rotation of the drum is chosen according to the dimensions of the chamber and the size of the cores to be coated. It is generally chosen in a range going from 3 to 30 rpm, preferably in a range going from 5 to 20 rpm, preferably in a range going from 5 to 15 rpm. It is for example equal to approximately 9 rpm, in particular for a perforated rotary drum 48.26 cm in diameter.
• the setting in motion of the bed of cores excludes the transport of said cores according to a longitudinal axis.
• the cores being coated are not transported from one chamber to another, that is to say that they are coated in a single chamber, and/or that the bed of cores does not is not coated in a longitudinal chamber along which they are transported.
• the inlet air temperature chosen is preferably less than 100° C., preferably less than or equal to 80° C., preferably less than or equal to 70° C., preferably less than or equal to at 60°C, preferably less than or equal to 50°C.
• This temperature is generally greater than or equal to 20°C, preferably greater than or equal to 30°C. It is for example approximately equal to 40° C.
• the air flow can be chosen in a range going from 50 to 8000 m 3 /h, for example in a range going from 100 to 7000 m 3 /h, for example from 100 to 1000 m 3 /h.
• This flow rate is for example equal to about 500 m 3 /h. It usually depends on the size of the turbine.
• the exit of the drying air is preferably effected by suction of air through the perforations of the perforated rotary drum.
• the perforated wall zone of the rotary drum in accordance with the description represents at least 50% of the surface of said wall of the drum, preferably at least 60%, preferably at least 70%, preferably at least 80 %, preferably at least 90%.
• the wall of the drum is perforated over its entire surface.
• the temperature of the bed of cores during coating is less than or equal to 70° C., preferably less than or equal to 60° C., preferably less than or equal to 50° C., preferably less than or equal to at 40°C.
• This temperature of the bed of cores during coating is generally at least 10° C., or even at least 20° C.
• This temperature of the bed of cores during coating is for example about 25 to about 30°C.
• the coating process in accordance with the description comprises a step of heating the bed of core to be coated. This step aims in particular to bring the core bed to a target temperature which corresponds to that of the cores being coated.
• the coating process of the invention simultaneously carries out spraying and drying of the spray liquid. It is however conceivable to introduce steps of distribution ("pause time") and spraying in the absence of drying, as long as this does not contravene the properties sought here, in particular concerning the quality of the solid coated forms obtained and/ or the workability of the process.
• the coating process phases during which optionally the spraying is not carried out concomitantly with the drying represent less than 50% of the coating process time, preferably less than 40%, preferably less than 30%, preferably less than 20%, preferably less than 10%, preferably less than 5%.
• the coating does not include a spraying phase in the absence of drying.
• any pause times represent less than 50% of the coating process time, preferably less than 40%, of preferably less than 30%, preferably less than 20%, preferably less than 10%, preferably less than 5%.
• the coating does not include a pause time.
• the coating percentage is, per unit time, at least 0.1% per minute, preferably at least 0.2% per minute, preferably at least 0.3% per minute, preferably at least 0.4% per minute.
• This mass gain per unit time is generally less than 1.0% per minute, or even less than 0.8% per minute, or even less than 0.7% per minute. It is for example equal to approximately 0.4 or 0.5% per minute.
• the method in accordance with the description may also comprise other usual steps than those aimed at coating the solid forms, as long as this does not contravene the properties sought here, in particular concerning the quality of the coated solid forms obtained and/or the workability of the process.
• steps mention may be made, for example, of gumming, smoothing, polishing, coloring.
• steps are carried out, they are carried out in the same equipment as that used in the coating process in accordance with the description.
• the coating process in accordance with the description comprises a smoothing step, after the coating.
• this smoothing step uses the coating liquid in accordance with the description for its implementation.
• this smoothing comprises a first step of spraying the liquid without drying, a second step without spraying or drying, a third step without spraying but with drying. These three steps make up a smoothing cycle according to a preferential mode.
• the smoothing comprises 1 to 5 cycles, preferably 1 to 4, preferably 1 to 3.
• Coloring if desired, can be carried out directly by adding coloring agents to the coating liquid.
• the equipment useful for the process in accordance with the description may comprise other elements conventionally employed in coating, as long as this does not contravene the properties sought here, in particular concerning the quality of the solid coated forms obtained and/or the workability of the process.
• the drum chamber used as described is free of clod breakers.
• the present invention also relates to a coated solid form obtained or capable of being obtained according to the coating process in accordance with the description.
• the present invention also relates to a solid form coated using a coating liquid in accordance with the description.
• the coated solid forms in accordance with the description have a coating percentage greater than 1%.
• This coating percentage otherwise called “mass gain”, is conventionally determined as follows:
• Weights of Dr eified Solid Shapes Weights of Cores
• this coating percentage is greater than 3%, preferably greater than 5%, preferably greater than 10%, preferably greater than or equal to 20%, preferably greater than or equal to 25%. It is preferably less than or equal to 50%, preferably less than or equal to 40%, preferably less than or equal to 35%. It is for example approximately equal to 30%.
• the amounts of ingredients are generally expressed in percentages by weight. Unless otherwise stated, these weights are amounts of ingredients in their original form, which is usually in powder form. These powdery ingredients generally contain small amounts of water (also called % moisture or “drying mass loss”) and some impurities. As such, the hydrolyzed and functionalized starch in accordance with the description generally does not contain more than 15% by weight of water, generally 3 to 12%; sugar alcohols like xylitol do not contain usually no more than 1% water. This means that when it is for example referred to 10% by weight of hydrolyzed and functionalized starch, this generally corresponds to 8.8 to 9.7% by dry weight (i.e. by anhydrous weight) .
• Chewing gums having the following qualitative composition were used: sorbitol (NEOSORB® P60W, ROQUETTE), gum base, maltitol syrup (LYCASIN® 85/55, ROQUETTE), mannitol (Mannitol 60, ROCKET), powder flavor, liquid flavor, sucralose, acesulfame K)
• the coating liquid had the following formulation:
• the percentages are expressed by weight, relative to the total weight of the coating liquid.
• the coating liquids were prepared as follows: two solutions were prepared.
• a solution A was prepared by mixing water with xylitol in a paddle mixer. Gum arabic was then introduced as a 40% solution. The whole was left stirring for approximately 45 minutes, at a sufficient speed to disperse and dissolve the xylitol.
• a solution B comprising titanium dioxide and water was prepared in a high shear mixer (POLYTRON) (3-5 minutes, 11000-30000 rpm). Solution A was added to solution B.
• POLYTRON high shear mixer
• the coating conditions were as follows:
• the coating liquid had the following formulation:
• the percentages are expressed by weight, relative to the total weight of the coating liquid.
• the coating liquids were prepared as in point 4.
• LYCOAT® RS720 was introduced in the form of a 25% solution.
• the coating conditions were as follows:
• the coating liquid had the following formulation: [0134] [Table 8] The percentages are expressed by weight, relative to the total weight of the coating liquid.
• the coating liquids were prepared as in point 4.
• LYCOAT® RS720 was introduced in the form of a 25% solution.
• Stability tests were carried out on the coated products obtained according to section 4. and according to section 5., Test 1. To do this, the coated chewing gums were placed at 30° C. at 70% d. relative humidity without packaging for 3 weeks. The water uptakes were measured over time (in % of mass gain by water absorption). The tests were also carried out under the following conditions: 40° C., 75% relative humidity, without packaging. The two batches of chewing gum had the same water uptake profiles.
• the percentages are expressed by weight, relative to the total weight of the pulverulent composition.
• the coating liquid had the following composition: 60% of this ready-to-use mixture and 40% water.
• the inventors have also carried out tests with a xylitol of larger particle size (the small particle size xylitol can form agglomerates during its storage). In these tests, XYLISORB® 90 (average diameter approximately equal to 90 ⁇ m) was therefore replaced by XYLISORB® 300 (average diameter approximately 300 ⁇ m). Very good results have also been obtained.

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• 2021
  • 2021-07-30 FR FR2108375A patent/FR3125719A1/fr active Pending
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