Improved sugar coating process including hydrolyzed and functionalized starch

Abstract

The present invention relates to an improved sugar coating process using hydrolyzed and functionalized starch. The present invention also relates to sugar coating compositions comprising such starches.

Description

[Technical field]

[0001] The present invention relates to an improved sugar-coating method, as well as sugar-coating compositions useful in carrying out the same. The present invention also relates to solid forms sugar-coated using the method or composition. [Background technology]

[0002] Sugar coating is an operation used especially in confectionery or pharmaceuticals, which consists in creating a more or less hard or soft crystallized coating on the surface of a solid or powdery product to protect it for various reasons or to make it visually or taste-wise attractive.

[0003] The coating of solid formations (cores) is conventionally carried out in a tank called a coater, which rotates on its axis, inside which there are several cores forming a moving mass, on whose surface the constituent material of the future envelope (the "sugar coating liquid or syrup") is dispensed in liquid form. A hard and crystalline coating is obtained by applying this liquid and evaporating the water provided thereby.

[0004] Sugar coating syrups consist primarily of one or even several crystalline materials and traditionally contain binders such as gum arabic or gelatin, colorants, opacifying agents such as TiO2, mineral fillers such as talc, silica, calcium carbonate, intense sweeteners, flavors, vitamins and active ingredients.

[0005] Sugar coating is a relatively labor-intensive process involving a number of successive steps, each of which, also called a "sugar coating cycle", typically includes an application phase, generally by spraying the sugar coating syrup onto the cores, a rotation phase, also called a dwell time, to distribute the syrup on the cores, and a drying phase of each new layer of syrup produced by blowing with hot, dry air.

[0006] Sugar coating makes it possible to obtain solid shapes with a particularly attractive appearance, but it lacks flexibility as to its implementation and as to the visual effects that can be obtained.

[0007] Interestingly, in patent application WO 20020 / 128290, the applicant proposed an improved, particularly simple and flexible sugar-coating method for sugar-coating solid shapes. In addition, this method made it possible to sugar-coat solid formations containing irregular shapes such as raised depressions or ridges while preserving these irregular shapes. The crystalline materials used were sugars or sugar alcohols such as xylitol, mannitol, sucrose, erythritol, isomalt or maltitol. The formulations may include binders such as gum arabic or polyvinyl alcohol (PVA). Gum arabic, in contrast to PVA, has the advantage of being derived from renewable resources. However, it induces an unattractive yellowing of the sugar-coating layer.

[0008] There was therefore a need to improve the formulations used in the above-mentioned method of patent application WO 20020 / 128290.

[0009] the purpose The present invention therefore aims to provide a sugar coating composition, in particular for use according to the method of the aforementioned patent application WO 20020 / 128290, which is composed of renewable materials.

[0010] It is also an object of the present invention to provide a sugar coating composition that does not yellow over time and / or does not contain gum arabic.

[0011] Presentation of the invention The Applicant has found that the use of hydrolyzed and functionalized starch makes it possible to effectively replace gum arabic in these compositions. In addition to avoiding the yellowing phenomenon, sugar-coated solid formulations with hydrolyzed and functionalized starch as binder are comparable or even superior to those sugar-coated with gum arabic as binder. In particular, the Applicant has noted that the hydrolyzed and functionalized starch used according to the invention may make it possible to obtain an improved stability of sugar-coated solid formulations. Summary of the Invention

[0012] Thus, a first subject of the present invention is a sugar-coating method comprising the steps of: - step (a) of spraying a sugar coating solution containing a crystalline material onto a moving bed of cores, the cores being placed in a chamber equipped with a rotating perforated drum and the spraying being performed by at least one compressed air nozzle; - at least one step (b) subsequent to step (a) of drying the sprayed sugar-coating liquid; - (c) recovering the resulting sugar-coated solid formation, A method of sugar coating, characterized in that the sugar coating solution comprises hydrolyzed and functionalized starch.

[0013] Preferably, the crystalline material comprises xylitol.

[0014] Preferably, the hydrolyzed and functionalized starch is functionalized with an alkyl group having 1 to 5 carbon atoms.

[0015] Preferably, the hydrolyzed and functionalized starch is selected from hydroxypropylated starch, acetylated starch, hydroxyethyl starch, or mixtures thereof.

[0016] Another subject of the invention is a sugar coating liquid, comprising (a) 40-80% of components other than the solvent, (a.1) 90.0 to 99.8% xylitol, (a.2) 0.1 to 3.0% hydrolyzed and functionalized starch, (a.3) 0.1 to 3.0% of an opacifying agent; (a.4) 0.0 to 3.0% of other components; The percentages of (a.1) through (a.4) are expressed by weight relative to the total weight of the non-solvent components, the sum of which equals 100%; and (b) 60% to 20% solvent; The percentages of (a) and (b) are expressed by weight relative to the total weight of the sugar coating liquid, the sum of which equals 100% of the sugar coating liquid.

[0017] The present invention also relates to the use of such sugar coating liquids for sugar coating solid formations.

[0018] An object of the present invention is also a sugar-coated solid formulation comprising at least one sugar-coating layer obtained from such a sugar-coating liquid.

[0019] A powdered composition for sugar-coating solid objects, comprising: - 90.0-99.8% xylitol, - 0.1 to 3.0% hydrolyzed and functionalized starch, - 0.1-3.0% opacifier, - Consists of 0.0-3.0% of other ingredients These percentages are expressed by weight relative to the total weight of the powdered composition, the sum of which equals 100%.

[0020] The present invention also relates to the use of such powdery compositions for sugar-coating solid forms.

[0021] An object of the present invention is also a sugar-coated solid formulation comprising at least one sugar-coating layer obtained from such a powdery composition. [Brief description of the drawings]

[0022] [Figure 1] 1 shows the maximum solubility of various crystalline materials in water based on the temperature of the solution. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

[0023] Thus, the present invention first provides a method for sugar coating comprising the steps of: - step (a) of spraying a sugar coating solution containing a crystalline material onto a moving bed of cores, the cores being placed in a chamber equipped with a rotating perforated drum and the spraying being performed by at least one compressed air nozzle; - at least one step (b) subsequent to step (a) of drying the sprayed sugar-coating liquid; - (c) recovering the resulting sugar-coated solid formation, The present invention relates to a method of sugar coating, characterized in that the sugar coating liquid comprises hydrolyzed and functionalized starch.

[0024] The expression "solid formulation" is conventionally understood to mean any solid presentation of a sugar-coated substance ("sugar-coated solid formulation") or any solid presentation that can undergo a sugar-coating operation ("core"). Typical examples are tablets, hard capsules, soft capsules, pellets, microspheres, granules, seeds, cookies, breakfast cereals, confectionery such as chewing gum, boiled candy, chewing candy, gummies, chocolate, fruit and vegetables, or products in the form of powders and / or crystals. These solid formulations may be intended for example for food, pharmaceutical, veterinary or cosmetic use. They may be intended for human, adult or child use, or for animals. They may also be products intended for chemical or agrochemical use, but solid formulations intended to be ingested in the context of the present invention ("solid oral formulations") are preferred. Preferably, these solid formulations are selected from tablets and chewing gum.

[0025] The sugar coating fluid of the present invention comprises a crystalline material and a functionalized hydrolyzed starch.

[0026] Conventionally, the term "crystalline materials" in sugar-coating is understood to mean substances that can crystallize upon evaporation of the solvent they are dissolved in. It is these crystalline materials that form the crystalline coating targeted by the sugar-coating.

[0027] Preferably, the crystalline material of the sugar coating solution according to the present disclosure is selected from sugars and sugar alcohols, preferably comprising at least one substance selected from monomers and dimers.

[0028] Preferably, in the sugar coating liquid according to the present disclosure, sugars and sugar alcohols make up at least 50% by weight of the crystalline material, preferably at least 70% by weight, preferably at least 90% by weight. Most preferentially, the crystalline material is entirely composed of substances selected from sugars and sugar alcohols.

[0029] Preferably, these sugars and sugar alcohols are selected from xylitol, sucrose, erythritol, mannitol, dextrose, isomalt, maltitol, or any combination thereof. Preferably, these crystalline materials comprise xylitol. Preferably, the crystalline material of the sugar coating liquid consists entirely of a single substance, preferably xylitol.

[0030] In a preferred embodiment, the sugar coating method according to the present disclosure comprises: - step (a) of spraying a sugar coating solution onto a moving bed of cores, the cores being placed in a chamber equipped with a rotating perforated drum and the spraying being performed by at least one compressed air nozzle; - at least one step (b) subsequent to step (a) of drying the sprayed sugar-coating liquid; - (c) recovering the resulting sugar-coated solid formation, The sugar coating liquid is characterized in that it contains xylitol and hydrolyzed and functionalized starch.

[0031] The concentration of crystalline material in the sugar coating liquid is selected such that the crystalline material is solubilized in the sugar coating liquid. Typically, especially when the sugar coating liquid is an aqueous liquid, the sugar coating liquid according to the present disclosure has a concentration of crystalline material of 90% or less, this percentage being expressed by weight relative to the total weight of the sugar coating liquid. Preferably, this concentration is 80% or less, preferably 70% or less. This concentration is preferably 20% or more, preferably 30% or more, preferably 40% or more, preferably 50% or more. This concentration is, for example, equal to about 60%.

[0032] The maximum concentration of crystalline materials naturally depends on the nature of these crystalline materials as well as the temperature of the sugar coating liquid. For xylitol, sucrose, erythritol, mannitol, dextrose, isomalt and maltitol, one can refer, for example, to Figure 1, which shows the maximum concentrations of these crystalline materials in water based on the temperature of the solution. Thus, for example, the concentration of crystalline materials in the sugar coating liquid at 20°C is preferentially 67% or less if the composition of the crystalline materials consists of sucrose, 15% or less if mannitol, 61% or less if maltitol, 63% or less if xylitol, 25% or less if isomalt, 27% or less if erythritol and 48% or less if dextrose.

[0033] Preferably, the content of crystalline material or xylitol in the sugar coating liquid is at least 50% by weight based on the total weight of the non-solvent components of the sugar coating liquid, preferably at least 70%, preferably at least 80%, preferably at least 90%, preferably at least 95%, for example equal to about 99%.

[0034] Preferably, the sugar coating liquid according to the present disclosure has a content of crystalline material, 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 sugar 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%. This content is, for example, equal to about 59%.

[0035] The sugar coating fluid of the present invention further comprises a hydrolyzed and functionalized starch.

[0036] The expression "starch" is recalled to refer to starch isolated from any suitable plant source by any technique conventionally known to the skilled artisan. Isolated starch generally does not contain more than 3% impurities. The percentage is expressed as the dry weight of impurities relative to the total dry weight of the isolated starch. These impurities typically include proteins, colloidal materials, and fibrous residues. Suitable plant sources include, for example, legumes, cereals, and tubers. Starches according to the present disclosure may be derived, for example, from legumes (e.g., peas), cereals (e.g., corn, rice, wheat, oats), and tubers (e.g., potato, tapioca).

[0037] Preferably, the hydrolyzed and functionalized starch according to the present disclosure is derived from a legume starch and / or cereal, preferably pea or corn starch, preferably pea, preferably smooth pea. In a preferred embodiment, the hydrolyzed and functionalized starch according to the present disclosure is derived from a starch having an amylose content of 20-50%, preferably 30-45%, preferably 30-40%, for example equal to about 35%, especially when derived from pea starch, these percentages being expressed by the dry weight of amylose relative to the total dry weight of starch. This amylose content can be determined by the skilled person by potentiometric analysis of the iodine absorbed by amylose to form a complex. In another preferred embodiment, the hydrolyzed and functionalized starch according to the present disclosure is derived from a starch having an amylose content greater than 5%, preferably between 10 and 40%, preferably between 15 and 35%, preferably between 20 and 30%, for example equal to about 25%, especially when derived from corn starch.

[0038] The hydrolyzed and functionalized starches according to the present disclosure may 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 refer to hydrolyzed starches having a dextrose equivalent of 2 to 20. They are generally obtained by acid or enzymatic hydrolysis. "Pyrodextrins" conventionally are obtained from the action of high temperatures (generally at least 100°C), combined or not combined with the action of acids or bases, in the presence of small amounts of water. Such treatments conventionally result in the formation of branches and so-called "atypical" bonds, and therefore pyrodextrins are structurally different from other hydrolyzed starches, in particular maltodextrins. Preferably, the hydrolyzed starches according to the present disclosure are obtained by acid hydrolysis. Preferably, the functionalized hydrolyzed starches according to the present disclosure are not pyrodextrins.

[0039] Hydrolyzed starch must be sufficiently distinct from glucose, glucose syrup, and cyclodextrins, the rate of hydrolysis of which is too high to be called "starch" as conventionally understood by those skilled in the art. In other words, glucose, glucose syrup, and cyclodextrins are not hydrolyzed starches within the meaning of the present invention.

[0040] The functionalized starch according to the invention is hydrolyzed, which means that it has a reduced molecular weight compared to the native starch from which it is derived. Therefore, alternatively or additionally, the hydrolyzed and functionalized starch according to the present disclosure may be defined by its weight average molecular weight (Mw), which is preferably less than 10,000 kDa as determined by size exclusion chromatography (HPSEC) with refractometric detection (RI) and coupled with a light scattering detector (MALLS). Preferably, Mw is determined by the following method: A sample of the hydrolyzed and functionalized starch is diluted in a mixture of dimethyl sulfoxide and 0.1 M sodium nitrate. Two columns with porosities of 100 and 1000 Angstroms (e.g. SUPREMA columns) are used. Elution is carried out in an aqueous medium at a flow rate of 0.5 mL / min. The system is maintained at a temperature of 40°C. Preferably, the hydrolyzed and functionalized starch according to the present disclosure has a Mw of 9,000 kDa or less, preferably 7,000 kDa or less, preferably 5,000 kDa or less, preferably 4,000 kDa or less. The Mw is preferably 100 kDa or more, preferably 500 kDa or more, preferably 1,000 kDa or more, preferably 2,000 kDa or more, preferably 2,500 kDa or more, preferably 3,000 kDa or more. The Mw is, for example, equal to about 3,500 kDa.

[0041] Preferably, the hydrolyzed and functionalized starch according to the present disclosure has a viscosity in water of less than 10,000 mPa.s at 20°C and a shear rate of 100 s-1, determined on an aqueous solution containing 10% by dry weight of said starch. Preferably, the viscosity is determined with a rheometer (e.g., Physica MCR301, Anton Paar) with a cone-plate geometry of 5 cm 1° (CP50). For example, it is possible to proceed as follows: The temperature is adjusted, for example via a Peltier. A 10% dry starch solution is kept in equilibrium at 20°C. The viscosity is measured at 0.006 to 1000 s. -1A shear rate in the range of (log 1 / 2) is applied for 3 min at 20° C. Preferably, this viscosity (10% dry, 20° C., 100 s -1 The shear rate is preferably equal to or less than 5000 mPa.s, preferably equal to or less than 1,000 mPa.s, preferably equal to or less than 500 mPa.s, preferably equal to or less than 100 mPa.s, preferably equal to or less than 50 mPa.s. The shear rate is preferably equal to or greater than 1 mPa.s, preferably equal to or greater than 10 mPa.s, preferably equal to or greater than 20 mPa.s, preferably equal to or greater than 30 mPa.s, for example equal to about 40 mPa.s. For example equal to about 42 mPa.s.

[0042] The hydrolyzed starch according to the present disclosure may also be functionalized. In other words, the hydrolyzed starch comprises a functional group grafted to at least one of its hydroxyl functional groups. In other words, the term "functionalized" in the sense of the present invention excludes crosslinking. Preferably, the functionalized starch according to the present disclosure is etherified and / or esterified, preferably etherified. Preferably, the starch according to the present disclosure is functionalized with an alkyl group having 1 to 5 carbon atoms, preferably 2 to 4 carbon atoms, preferably 2 or 3 carbon atoms, preferably 3 carbon atoms. Preferably, the alkyl group is an aliphatic alkyl group, more preferably a saturated aliphatic group.

[0043] Preferably, the functionalized starch according to the present disclosure is selected from hydroxypropylated starch, acetylated starch, hydroxyethyl starch, or mixtures thereof. The functionalized starch is preferably hydroxypropylated starch, and is preferably used alone.

[0044] Hydroxypropylated starch according to the present disclosure can be obtained, for example, by etherification with propylene oxide. The hydrolyzed hydroxypropylated starch preferably has a content of hydroxypropyl groups of 0.5 to 10%, the percentage being expressed as the dry weight of hydroxypropyl groups relative to the total dry weight of the hydrolyzed hydroxypropylated starch. The content of hydroxypropyl groups can be determined by the person skilled in the art, for example by proton Nuclear Magnetic Resonance (proton NMR), preferably according to the method according to the European Pharmacopoeia as in force on 1st 2021 ("STARCH, PREGELATINIZED HYDROXYPROPYL"). The content of hydroxypropyl groups is preferably 0.5 to 9%, preferably 0.5 to 8%, preferably 0.5 to 7%, for example equal to about 7%.

[0045] The functionalized starch according to the present disclosure may be etherified or esterified, or both etherified and esterified. However, it is preferably esterified or etherified. It may be substituted (i.e. functionalized) with groups of the same or different nature. However, it is preferably substituted with groups of the same nature, for example and preferably only with hydroxypropyl groups.

[0046] Preferably, the hydrolyzed and functionalized starch according to the present disclosure has a low-temperature solubility in water of 70% or more, said percentage being expressed as the dry weight of soluble starch relative to the total weight of starch. Preferably, this low-temperature solubility in water is 80% or more, preferably 90% or more, preferably 95% or more. This low-temperature solubility in water is, for example, equal to about 98%. This solubility can be determined, for example, by placing 5 grams of said starch in 200 mL of distilled water at 20° C. The dissolved dry weight can be determined after centrifugation and dehydration of the supernatant. This solubility can be determined, for example, according to the following protocol: In a 250 mL beaker, 200 mL of distilled water is added. 5 g of starch is added and the mixture is homogenized by magnetic stirring for 15 minutes. The resulting solution / suspension is centrifuged at 4,000 rpm for 10 minutes. 25 mL of the supernatant is 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 to cool to room temperature and then weighed to calculate the solubility by dry weight.

[0047] Starches with such low temperature solubility in water can conventionally be obtained from insoluble starch by calcination and / or hydrolysis of the insoluble starch. The calcination can typically be carried out by heating a starch suspension so that the insoluble granules rupture and dissolve. The functionalized starches according to the present disclosure are hydrolyzed and, depending of course on the level of hydrolysis, may be low temperature soluble in water without the need for additional treatment.

[0048] Preferably, the hydrolyzed and functionalized starch according to the present disclosure is pregelatinized. Pregelatinization conventionally means that the starch particles no longer exhibit birefringence in polarized optical microscopy (no crystalline phases). Pregelatinization can generally be obtained from birefringent starch by heat treatment (generally between 50 and 90°C, specifically based on the plant origin of the starch) in the presence of water (said treatment is generally called "calcination" as in the preceding paragraph) and additional drying (after and / or simultaneously with calcination). Chemical substances can be used as processing aids. Pregelatinization can be carried out, for example, by drum drying. In that case, the starch can be hardened before or during the drum drying step. The starch can also be calcined and then atomized. It can also be obtained by extrusion. In the present disclosure, pregelatinization is preferentially carried out by calcination and atomization.

[0049] The hydrolyzed and functionalized starch according to the present disclosure may be subjected to other chemical and / or physical modifications than the preferred modifications mentioned above, as long as the preferred modifications are not inconsistent with the properties sought in the present invention, with respect to the quality of the resulting sugar-coated solid formulation and / or the workability of the process. However, the hydrolyzed and functionalized starch according to the present disclosure is preferably not further modified, as this does not appear to be necessary to address the problems disclosed herein.

[0050] Preferably, the hydrolyzed and functionalized starch according to the present disclosure is a product with CAS number 9049-76-7. Preferably, the hydrolyzed and functionalized starch according to the present disclosure complies with the European Pharmacopoeia ("STARCH, PREGELATINIZED HYDROXYPROPYL"), which came into force on March 1, 2021.

[0051] Particularly useful functionalized hydrolyzed starches are commercially available, for example the hydrolyzed hydroxypropylated starches LYCOAT® RS720 (CAS number 113894-92-1) or LYCOAT® RS780 (CAS number 113894-92-1) sold by the applicant.

[0052] Preferably, the functionalized hydrolyzed starch content of the sugar coating liquid is 0.1% or more, preferably 0.2% or more, preferably 0.3% or more, preferably 0.4% or more, this percentage being expressed by weight relative to the total weight of the non-solvent components of the sugar coating liquid. This content is preferably less than 5.0%, preferably 4.0% or less, preferably 3.0% or less, preferably 2.0% or less, preferably 1.0% or less. This content is, for example, from about 0.1 to about 1.0%, or from about 0.5 to about 0.9%.

[0053] Preferably, the weight ratio of crystalline material / 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 less than or equal to 170, preferably greater than or equal to 190. This weight ratio 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. This weight ratio is, for example, equal to about 200.

[0054] Preferably, the sugar coating liquid according to the present disclosure has a content of non-solvent components of less than 80%, preferably less than 70%, preferably less than 65%, this percentage expressed by weight relative to the total weight of the sugar coating liquid. This content is preferably greater than 20%, preferably greater than 30%, preferably greater than 40%, preferably greater than 50%, preferably greater than 55%. This content is, for example, equal to about 60%.

[0055] Sugar coating liquids according to the present disclosure are typically polar and contain water preferentially as the majority solvent, and most preferentially as the only solvent.

[0056] Preferably, for reasons of simplicity and where this is possible, the sugar coating method according to the invention implements a single sugar coating liquid, i.e. the sugar coating liquid has a constant composition over the duration of the sugar coating.

[0057] The sugar-coating liquid according to the present disclosure may contain substances other than those mentioned above, as long as this is not contrary to the properties required in the present invention, in particular with regard to the quality of the obtained sugar-coated solid formulation and / or the workability of the method. Such other compounds can be, for example: - Other binders such as gum arabic, polyvinyl alcohol, etc. - crystalline materials and / or sugars and / or sugar alcohols other than xylitol, - Colorants such as pigments, - Flavorings, sweeteners, - the active agent of interest, e.g. a pharmaceutical, nutritional, functional food or phytosanitary agent It is.

[0058] However, preferably, in the sugar coating liquid according to the present disclosure, the functionalized hydrolyzed starch accounts for at least 50% by weight of the binder, preferably at least 60% by weight, preferably at least 70% by weight, preferably at least 80% by weight, preferably at least 90% by weight, preferably about 100% by weight. Thus, preferably, the functionalized hydrolyzed starch according to the present disclosure is the only binder of the sugar coating liquid. In particular, the sugar coating liquid according to the present invention is preferably PVA-free or gum arabic-free, preferably PVA and gum arabic-free.

[0059] The crystalline material other than xylitol is conventionally selected from sugars and sugar alcohols, monomers and dimers, preferably mannitol, sucrose, erythritol, dextrose, isomalt, maltitol, or any combination thereof. Preferably, in the sugar coating liquid according to the present disclosure, xylitol represents at least 50% by weight of the total crystalline material and / or the total sugar and sugar alcohol. Preferably, this xylitol content is equal to or greater than 60%, preferably equal to or greater than 70%, preferably equal to or greater than 80%, preferably equal to or greater than 90%, preferably equal to about 100%. Thus, preferably, the sugar coating liquid according to the present disclosure does not comprise crystalline material other than xylitol and / or does not comprise sugar and / or does not comprise sugar alcohol other than xylitol.

[0060] Preferably, the sugar coating liquid according to the present disclosure further comprises an opacifying agent, preferably titanium dioxide. Preferably, the functionalized opacifying agent content of the sugar coating liquid is 0.1% or more, preferably 0.3% or more, preferably 0.5% or more, preferably 0.7% or more, preferably 0.9% or more, this percentage being expressed by weight relative to the total weight of the non-solvent components of the sugar coating liquid. Preferably, this opacifying agent content, in particular the titanium dioxide content, is 20.0% or less, preferably 15.0% or less, 10.0% or less, 5.0% or less. This content is, for example, equal to about 1%.

[0061] Generally, the sugar coating liquid according to the present disclosure comprises less than 5.0%, preferably not more than 4.0%, preferably not more than 3.0%, preferably not more than 2.0%, preferably not more than 1.0%, for example equal to about 0.0%, of pigments and / or colorants, these percentages being expressed by weight relative to the total weight of the non-solvent components of the sugar coating liquid.

[0062] In another preferred embodiment, the sugar coating solution according to the present disclosure comprises: (a) 40-80%, preferably 45-75%, preferably 50-70%, preferably 55-65%, for example about 60%, of components other than the solvent, (a.1) 90.0 to 99.8%, preferably 95.0% to 99.5%, preferably 96.0% to 99.0%, preferably 97.0% to 99.0%, preferably 98.0% to 99.0%, for example 98.5% xylitol; (a.2) 0.1-3.0%, preferably 0.2-2.0%, preferably 0.3-1.0%, preferably 0.4-0.8%, preferably 0.4-0.7%, preferably 0.4-0.6%, for example 0.5% of hydrolyzed and functionalized starch, (a.3) 0.1 to 3.0%, preferably 0.5 to 2.0%, for example 1.0%, of an opacifying agent; (a.4) 0.0-3.0%, preferably less than 2.0%, preferably less than 1.0%, preferably less than 0.5%, for example 0.0%, of other ingredients, preferably colorant substances; The percentages of (a.1) through (a.4) are expressed by weight relative to the total weight of the non-solvent components, the sum of which equals 100%; and (b) 60-20%, preferably 55-25%, preferably 50-30%, preferably 45-35%, for example around 40% of a solvent, which solvent is preferentially water, The percentages of (a) and (b) are expressed by weight relative to the total weight of the sugar-coating liquid, and their sum equals 100%.

[0063] The present invention also relates to the use of such sugar-coating liquid for sugar-coating a solid formulation, preferably said sugar-coating being carried out according to the method according to the present disclosure as previously described.

[0064] The sugar coating method according to the present disclosure may further comprise the step of preparing a sugar coating liquid, preferably by mixing the ready-to-use mixture with a suitable solvent, preferably water.

[0065] Preferably, this ready-to-use mixture has a composition as previously defined for the sugar coating liquid, except for the solvent, which of course is omitted.

[0066] The ready-to-use mixture according to the present disclosure is typically in the form of a powdered mixture.

[0067] In a preferred embodiment, the ready-to-use mixture according to the present disclosure comprises: - 90.0 to 99.8%, preferably 95.0% to 99.5%, preferably 96.0% to 99.0%, preferably 97.0% to 99.0%, preferably 98.0% to 99.0%, for example 98.5% xylitol, - 0.1-3.0%, preferably 0.2-2.0%, preferably 0.3-1.0%, preferably 0.4-0.8%, preferably 0.4-0.7%, preferably 0.4-0.6%, for example 0.5% of hydrolyzed and functionalized starch, - 0.1-3.0%, preferably 0.5-2.0%, for example 1.0%, of an opacifier, - a powdery composition comprising 0.0-3.0%, preferably less than 2.0%, preferably less than 1.0%, preferably less than 0.5%, for example 0.0%, of other ingredients, preferably colorant substances, These percentages are expressed by weight relative to the total weight of the powdered composition and their sum equals 100%.

[0068] The present invention also relates to the use of such a powdery composition for sugar-coating a solid formulation, preferably said sugar-coating being carried out according to the method according to the present disclosure as previously described.

[0069] The equipment used to carry out the method according to the present disclosure typically comprises a unit for storing the sugar-coating liquid, including at least one outlet for transporting the sugar-coating liquid to a device for spraying the sugar-coating liquid. This transport can be ensured, for example, by a peristaltic pump. The sugar-coating liquid is applied via a spraying device to the core bed housed in a chamber, said chamber comprising a rotating drum for the movement of said core bed. More precisely, the drum is a perforated rotating drum and the selected spraying device comprises at least one compressed air nozzle. The equipment further comprises an air inlet in the drum chamber for drying the sugar-coating liquid. Drying air is discharged, in particular by sucking air from the chamber, in particular through perforations in the rotating drum.

[0070] The elements of equipment useful in the methods according to the present disclosure are commercially available and their construction does not represent any particular difficulty for the skilled artisan.

[0071] The temperature of the sugar coating liquid is typically selected such that the crystalline material, especially xylitol, is sufficiently solubilized in the sugar coating liquid to be sprayed. This temperature is therefore also a function of the amount of crystalline material present in the liquid. Preferably, the temperature of the sugar coating liquid is less than 90°C, preferably less than 80°C, preferably less than 70°C, preferably less than 60°C, preferably less than 50°C, preferably less than 40°C, preferably less than 30°C. This temperature is preferably at least 10°C, preferably at least 15°C, or even at least 20°C. This temperature preferably corresponds to the ambient temperature, which typically varies from about 20 to about 25°C. When xylitol is used as the crystalline material, the temperature of the solvent used in the sugar coating liquid is preferably as defined above in this paragraph. However, due to the high enthalpy of dissolution of xylitol, the temperature of the sugar coating liquid is generally lower. Thus, for example, for a sugar coating solution using water at 20°C as the solvent, the sugar coating solution will generally have a temperature of 10-15°C after dissolution of the xylitol in water, and 15-20°C during sugar coating.

[0072] Preferably, the sugar coating liquid is kept under agitation during its use. Preferably, the rotation speed is selected to maintain the homogeneity of the sugar coating liquid.

[0073] In a preferred embodiment, the sugar coating liquid is stored in a single jacketed storage unit and / or the facility useful in the method according to the present disclosure does not have devices for heating the sugar coating liquid. Indeed, these devices are not mandatory in the method according to the present disclosure, since the method according to the present disclosure does not necessarily require the use of a hot sugar coating liquid.

[0074] The number of compressed air nozzles used to spray the sugar-coating liquid is conventionally selected based on the size of the sugar-coating chamber, according to the manufacturer's recommendations. This number is typically 1-2 nozzles per 40 cm diameter cross section of the sugar-coating chamber. This number can range, for example, from 1 to 10, such as from 1 to 6.

[0075] Preferably, for spraying, the method according to the present disclosure uses only compressed air nozzles.

[0076] Preferably, the nozzles used according to the present disclosure have a hole with a diameter selected from the range of 0.1 to 2.8 mm, preferably 0.1 to 2.5 mm, preferably 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.

[0077] Preferably, the spraying flow rate is selected from the range of 1-20 g / min / kg of cores, preferably 1-15 g / min / kg of cores, preferably 2-15 g / min / kg of cores, preferably 5-10 g / min / kg of cores. Preferably, the flow rate selected for spraying is increased during the sugar-coating process. In particular, the inventors have found that in the case of certain crystalline materials, the use of a low flow rate at the beginning of the sugar-coating makes it possible to promote the first crystallization phase that occurs on the surface of the cores. The flow rate can then be increased to accelerate the sugar-coating.

[0078] For spraying, the atomization pressure and the crushing pressure are adjusted based on the flow rate and the nozzle hole and are adjusted according to the manufacturer's recommendations. This flow rate and this nozzle hole typically depend on the size of the equipment used. These atomization pressures and crushing pressures are typically selected in the range of 0.5 bar to 4.0 bar, preferably 0.5 bar to 3.5 bar, for example 0.7 bar to 2.5 bar for the atomization pressure and / or 0.7 bar to 3.5 bar for the crushing pressure. This atomization pressure is, for example, equal to about 1.

[0079] In the sugar coating process of the present invention, the sugar coating liquid is sprayed onto a bed of cores moved by a rotating drum. The nature of these cores is preferably as defined above for solid forms, for example tablets or chewing gums. These cores may be completely bare or may be coated with one or more layers, for example gumming, film coating or even sugar coating layers, which are preferentially obtained in the same equipment as that used for the sugar coating process according to the present disclosure.

[0080] To set the core bed during the transfer, the rotation speed of the drum is selected based on the dimensions of the chamber and the size of the cores to be sugar coated. This rotation speed is generally selected in the range of 3 to 30 rpm, preferably in the range of 5 to 20 rpm, preferably in the range of 5 to 15 rpm. This rotation speed is, for example, equal to about 9 rpm, in particular for a perforated rotating drum with a diameter of 48.26 cm.

[0081] In an advantageous embodiment, particularly for reasons of convenience and / or space, and as the method according to the present disclosure allows it, the movement of the core bed excludes transport of said cores along the longitudinal axis, which means in particular that the sugar-coated cores are not transported from one chamber to another, i.e. that they are sugar-coated in a single chamber, and / or that the core bed is not sugar-coated in a longitudinal chamber along which it is transported.

[0082] For drying, the inlet air temperature chosen is preferably below 100° C., preferably below 80° C., preferably below 70° C., preferably below 60° C., preferably below 50° C. This temperature is generally above 20° C., preferably above 30° C. This temperature is, for example, equal to about 40° C.

[0083] For drying, the air flow rate is 50 to 8000 m 3 / h range, e.g. 100-7000m 3 / h range, e.g. 100-1000m 3 This deposition can be selected for example at 500 m 3 This deposition generally depends on the size of the turbine.

[0084] The discharge of dry air is preferably carried out by drawing air through the perforations of a perforated rotating drum.

[0085] Preferably, the area of ​​the perforated wall of a rotating drum according to the present disclosure occupies at least 50%, preferably at least 60%, preferably at least 70%, preferably at least 80%, preferably at least 90% of the surface of said wall of said drum, and preferably the wall of the drum is perforated over its entire surface.

[0086] Preferably, the temperature of the core bed being sugar-coated is below 70° C., preferably below 60° C., preferably below 50° C., preferably below 40° C. This temperature of the core bed during sugar-coating is generally at least 10° C., or even at least 20° C. This temperature of the core bed to be sugar-coated is, for example, about 25 to about 30° C. Preferably, before the start of sugar-coating, i.e. before spraying begins, the sugar-coating method according to the present disclosure comprises a step of heating the core bed to be sugar-coated. This step is in particular aimed at bringing the core bed to a target temperature corresponding to the temperature of the cores to be sugar-coated.

[0087] The sugar-coating process of the present invention is carried out concomitantly with spraying of the spray liquid and drying. However, it is conceivable to introduce a distribution step ("pause time") and a spraying step in the absence of drying, as long as this is not contrary to the properties required herein, especially with regard to the quality of the obtained sugar-coated solid formations and / or the workability of the process.

[0088] Preferably, the phase of the sugar-coating method during which spraying is not performed optionally accompanied by drying occupies less than 50% of the time of the sugar-coating method, preferably less than 40%, preferably less than 30%, preferably less than 20%, preferably less than 10%, preferably less than 5%. Most preferentially, the sugar-coating does not include a spraying phase in the absence of drying.

[0089] Preferably, possible pause times (time between two spraying phases during which there is neither spraying nor drying) occupy less than 50% of the time of the sugar-coating method, preferably less than 40%, preferably less than 30%, preferably less than 20%, preferably less than 10%, preferably less than 5%. Most preferentially, the sugar-coating does not include pause times.

[0090] Preferentially, the percentage of sugar coating (or "mass increase") is 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 increase per unit of 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. This mass increase is, for example, equal to about 0.4 or 0.5% per minute.

[0091] The method according to the present disclosure may further comprise other conventional steps than those aimed at sugar-coating the solid formation, as long as this is not contrary to the properties required herein, in particular with regard to the quality of the sugar-coated solid formation obtained and / or the workability of the method. Examples of other steps that may be mentioned are gumming, smoothing, polishing and coloring. Advantageously, if such steps are carried out, they are carried out in the same equipment as that used in the sugar-coating method according to the present disclosure. It is understood that some of these steps, such as gumming or coloring, may sometimes be integrated into the sugar-coating process, if the composition used contains such an amount of crystalline material that a layer of crystallized matter, in particular sugar and / or sugar alcohol, is effectively formed.

[0092] Preferably, the sugar-coating method according to the present disclosure comprises a smoothing step after sugar-coating. Preferably, this smoothing step uses a sugar-coating liquid according to the present disclosure for its execution. Preferably, this smoothing comprises a first step of spraying the liquid without drying, a second step of neither spraying nor drying, and a third step of drying but not spraying. These three steps constitute a smoothing cycle according to a preferential embodiment. Preferably, the smoothing comprises 1 to 5, preferably 1 to 4, preferably 1 to 3 cycles.

[0093] Coloring may be achieved directly through the addition of colorants to the sugar coating liquid, if desired.

[0094] The equipment useful for the process according to the present disclosure may contain other elements conventionally used in sugar coating processes, as long as this is not contrary to the properties required herein, in particular with regard to the quality of the obtained sugar-coated solid formations and / or the workability of the process. Preferably, however, the chamber of the drum used according to the present disclosure does not contain a lump breaker.

[0095] The present invention also relates to a sugar-coated solid formation obtained or obtainable according to the sugar-coating method according to the present disclosure. The present invention also relates to a sugar-coated solid formation using the sugar-coating liquid according to the present disclosure.

[0096] Preferably, the sugar-coated solid formulation according to the present disclosure has a sugar-coating percentage greater than 1%. This percentage of sugar-coating, also known as "mass gain", is conventionally determined as follows:

[0097]

number

[0098] In the present disclosure, the amounts of ingredients are generally expressed as percentages by weight. Unless otherwise stated, these weights are the amounts of ingredients in their original form, which is generally in powder form. These powdered ingredients generally contain a small amount of water (also called % moisture or "mass loss due to dehydration") and some impurities. In this regard, the hydrolyzed and functionalized starches according to the present disclosure generally contain 15% or less by weight of water, generally 3-12%, and sugar alcohols such as xylitol generally contain 1% or less of water. This means that, for example, when referring to a 10% by weight hydrolyzed and functionalized starch, this generally corresponds to 8.8-9.7% by dry weight (i.e., by anhydrous weight).

[0099] Conversely, in this disclosure, when dry weight is referred to, this refers to anhydrous weight.

[0100] Other characteristics and advantages of the present invention will appear clearly on reading the following examples, which are intended to illustrate but not limit the invention. EXAMPLES

[0101] A. Sugar Coating Test 1. Equipment used An equipment with the following characteristics was used: - Perforated rotating drum, 48.26cm diameter, - Blades x 6, - 1 compressed air atomizing nozzle (Schlick 970 / 7-1 S75), hole diameter 0.8 mm, - Peristaltic pump (Watson Marlow model 323), 3 roller head (313 DW), - Exacanal tubing, 4mm inner diameter, 8mm outer diameter.

[0102] 2. Core A chewing gum with the following qualitative composition was used: sorbitol (NEOSORB® P60W, ROQUETTE), base gum, maltitol syrup (LYCASIN® 85 / 55, ROQUETTE), mannitol (Mannitol 60, ROQUETTE), powdered flavor, liquid flavor, sucralose, acesulfame K.

[0103] 3. Common parameters for all tests

[0104] [Table 1]

[0105] 4. Sugar Coating with Xylitol and Gum Arabic The operating conditions were optimized to obtain the best results with gum arabic. The best results were obtained under the conditions given in this section.

[0106] The sugar coating solution had the following formulation:

[0107] [Table 2]

[0108] The percentages are expressed by weight relative to the total weight of the sugar coating liquid.

[0109] The sugar coating solution was prepared as follows: Two solutions were prepared. Solution A was prepared by mixing water with xylitol in a blade mixer. Gum arabic was then introduced in the form of a 40% solution. The whole was stirred for about 45 minutes at a speed sufficient to disperse and dissolve the xylitol. Solution B, containing titanium dioxide and water, was prepared in a high shear mixer (POLYTRON) (3-5 minutes, 11,000-30,000 rpm). Solution A was added to solution B.

[0110] The sugar coating conditions were as follows:

[0111] [Table 3]

[0112] A smoothing step was then carried out using the same solution as used for the sugar coating solution as follows.

[0113] [Table 4] Pump speed: 50 rpm

[0114] 5. Sugar Coating with Xylitol and Functionalized Hydrolyzed Starch The operating conditions were optimized to obtain the best results with the functionalized hydrolyzed starch according to the present disclosure.

[0115] Test 1 The sugar coating solution had the following formulation:

[0116] [Table 5]

[0117] The percentages are expressed by weight relative to the total weight of the sugar coating liquid.

[0118] The sugar coating solution was prepared similarly to point 4. LYCOAT® RS720 was introduced in the form of a 25% solution.

[0119] The sugar coating conditions were as follows:

[0120] [Table 6]

[0121] A smoothing step was then carried out using the same solution as used for the sugar coating solution as follows.

[0122] [Table 7] * Pump speed: 50 rpm

[0123] Test 2 The sugar coating solution had the following formulation:

[0124] [Table 8]

[0125] The percentages are expressed by weight relative to the total weight of the sugar coating liquid.

[0126] The sugar coating solution was prepared similarly to point 4. LYCOAT® RS720 was introduced in the form of a 25% solution.

[0127] The sugar coating conditions were as follows:

[0128] [Table 9]

[0129] The smoothing step was then carried out as in Test 1.

[0130] B. Stability A stability test was carried out on the sugar-coated products obtained according to section 4. and section 5., test 1. To do this, the sugar-coated chewing gums were placed without packaging at 30° C. and 70% relative humidity for 3 weeks. The water uptake was measured over time (% of mass increase due to water absorption). The test was also carried out under the following conditions: 40° C., 75% relative humidity, without packaging.

[0131] The two batches of chewing gum had the same water uptake profile.

[0132] Stability tests were also carried out in a second step on other cores, which tests, not presented here, showed that the hydrolyzed and functionalized starch according to the present disclosure makes it possible to obtain even better results than gum arabic.

[0133] Test 3 Tests were also carried out to produce a sugar coating liquid with a ready-to-use powder composition having the following composition:

[0134] [Table 10]

[0135] The percentages are expressed by weight relative to the total weight of the powdered composition.

[0136] The sugar coating solution had the following composition: 60% of this ready-to-use composition and 40% water.

[0137] By using this method, sugar coating tests were successfully carried out.

[0138] The inventors also carried out tests with larger particle size xylitol (low particle size xylitol potentially forming agglomerates during storage). Therefore, in these tests, XYLISORB® 90 (mean diameter approximately equal to 90 μm) was replaced by XYLISORB® 300 (mean diameter approximately 300 μm). Very good results were also obtained.

Claims

1. 1. A sugar coating method comprising the steps of: - step (a) of spraying a sugar coating liquid comprising a crystalline material onto a moving bed of cores, said cores being placed in a chamber comprising a rotating perforated drum and said spraying being carried out by means of at least one compressed air nozzle; - at least one step (b) concomitant to step (a) of drying said sprayed sugar-coating liquid; - step (c) of recovering the resulting sugar-coated solid formation, 13. A method of sugar coating, characterized in that the sugar coating solution comprises hydrolyzed and functionalized starch.

2. 10. The sugar coating method of claim 1, wherein the crystalline material comprises xylitol.

3. 3. The sugar coating process according to claim 1 or 2, wherein the hydrolyzed and functionalized starch is functionalized with an alkyl group having 1 to 5 carbon atoms.

4. 3. The sugar coating method according to claim 1 or 2, wherein the hydrolyzed and functionalized starch is selected from hydroxypropylated starch, acetylated starch, hydroxyethyl starch, or mixtures thereof.

5. A sugar coating solution comprising: (a) 40 to 80% of non-solvent components, (a.1) 90.0 to 99.8% xylitol; (a.2) 0.1-3.0% hydrolyzed and functionalized starch; (a.3) 0.1 to 3.0% of an opacifier; (a.4) 0.0 to 3.0% of other components; non-solvent components, the percentages of (a.1) to (a.4) being expressed by weight relative to the total weight of said non-solvent components, the sum of which equals 100%; (b) 60-20% solvent; The percentages of (a) and (b) are based on the weight of the total sugar coating liquid. The sugar coating solution is expressed as:

6. 6. Use of the sugar coating liquid according to claim 5 for sugar coating solid bodies.

7. A sugar-coated solid product comprising at least one sugar-coating layer obtained from the sugar-coating liquid according to claim 5.

8. A powdered composition for sugar-coating solid objects, comprising: - 90.0 to 99.8% xylitol, - 0.1 to 3.0% hydrolyzed and functionalized starch, - 0.1 to 3.0% of an opacifier, - 0.0-3.0% of other components, A powdered composition, wherein said percentages are expressed by weight relative to the total weight of said powdered composition, the sum of which equals 100%.

9. 10. Use of the powdery composition according to claim 8 for sugar-coating solid formulations.

10. A sugar-coated solid product comprising at least one sugar-coating layer obtained from the composition of claim 8.

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