Use of stearate for improving surface of solid form of coated sugar coating

Abstract

The present invention relates to a solid form of a coated sugar-coating composition comprising a crystallizable material and a stearate salt, such as magnesium stearate. The invention also relates to a sugar coating composition comprising a stearate salt and to a method for coating a solid core using the sugar coating composition. The invention also relates to a use for improving the surface of a sugar coating layer in a solid form of a coated sugar coating, comprising the inclusion of a stearate salt in said sugar coating layer.

Description

Technical Field

[0001] This invention relates to the field of coatings for solid forms, particularly tablets and chewing gum. Background Technology

[0002] Coating is the application of a coating material to the surface of a solid form to achieve desired properties superior to uncoated varieties, such as improving the visual aspects, odor, taste, stability, ease of swallowing, mechanical resistance of the solid form, protecting the solid form from the gastric environment, or altering the release properties of the active ingredient.

[0003] There are two main methods for tablet coating: sugar coating and film coating.

[0004] Film coating is a single-stage coating method that requires relatively short time and is therefore more favored than sugar coating in the pharmaceutical industry. Film coating involves the deposition of a polymer film (between 20 μm and 100 μm) primarily applied to tablets.

[0005] Sugar coating in solid form is visually more appealing and generally has a pleasant sweetness. However, unlike film coating, sugar coating is a more laborious, multi-step process. Sugar coating typically involves various steps, such as film coating, the sugar coating itself, smoothing, coloring, polishing, and printing, resulting in a final tablet weight increase of up to 30%–50% and a significant increase in tablet size.

[0006] Film coating consists of the following: a sealing coating is applied to the solid core to prevent water from penetrating into the tablet, avoiding subsequent sugar coating. Therefore, it provides good product stability and also strengthens the tablet core. Film-forming agents (e.g., gum arabic) are also often applied to the solid core to promote the adhesion of the sugar coating layer. The latter is often referred to as the "coating" step. Film coatings can be composed of shellac, cellulose acetate phthalate (CAP), polyvinyl acetate phthalate (PVAP), hydroxypropyl cellulose (HPC), hydroxypropyl methylcellulose (HPMC), or zein (a corn protein derivative).

[0007] Sugar coating itself is considered the first major step in the sugar coating process. It involves applying a large amount of sugar coating composition onto the solid core, thereby significantly increasing the weight of the solid core. Sugar coating provides the rapid build-up necessary to round the edges of the tablet. It also provides the basis for smoothing and coloring the coating, and any weaknesses in the final sugar coating can generally be attributed to weaknesses in the sugar coating process.

[0008] Smoothing is applied to smooth the rough surface of the sugar coating and to increase the volume of the solid core to the desired size. Smoothing syrups generally consist of a sugar coating composition having 60 wt.%–70 wt.% sugar solids. In some cases, the syrup also includes gum arabic, gelatin, pigments, starch, or opacifiers. Multiple smoothing cycles (approximately 10 cycles) are performed until the tablet is suitable for the next stage (e.g., coloring).

[0009] When desired, coloring is typically achieved by adding pigments to the coating composition or to the smoothing syrup.

[0010] Polishing produces a characteristic surface gloss and refined tablets. Polishing is performed in a polishing disc using a mixture of beeswax, carnauba wax, and candelilla wax.

[0011] There is a continuous need to improve the surface of solid forms coated with icing, both for aesthetic reasons and / or because it can facilitate certain steps in the icing process. For example, providing solid forms of icing with surfaces as regular as possible will facilitate and accelerate the smoothing step.

[0012] Technical issues

[0013] The purpose of this invention is to improve the surface of solid forms coated with sugar, particularly to improve the smoothness of the sugar coating layer.

[0014] Another objective of this invention is to shorten the sugar coating process time.

[0015] The object of this invention is to solve the above problems by providing a solution that has other properties required for such applications, such as in terms of security and ease of use.

[0016] Introduction of the present invention

[0017] The inventors have solved the above-mentioned problems by providing a coating composition that, following sugar or sugar alcohol (a crystallizable material), also contains a stearate (e.g., magnesium stearate). By doing so, the inventors are able to increase the smoothness of the coated solid form, thereby reducing the time required to smooth the coated solid form.

[0018] The smoothness achieved is even better than that obtained on coated products from the market (see...). Figure 1 (And especially by comparison with ibuprofen-coated sugar tablets), which means that even a smoothing step is not required.

[0019] Furthermore, the opacity of the sugar coating composition according to this disclosure is excellent, thus allowing the removal of titanium dioxide (TiO2), which is particularly advantageous considering that the use of TiO2 as a food additive is now banned in Europe.

[0020] The coating compositions used in this invention are particularly suitable for coating methods developed by the applicant and described in WO2018 / 234248. This sugar coating method is very fast compared to conventional sugar coating methods. Summary of the Invention

[0021] Therefore, the present invention relates first to a solid form of a coated sugar composition comprising a crystallizable material and a stearate, preferably magnesium stearate.

[0022] Preferably, the crystallizable material is selected from sugars, sugar alcohols, or any mixture thereof. More preferably, the crystallizable material is selected from xylitol, sucrose, erythritol, mannitol, dextrose, isomaltitol, maltitol, sorbitol, or any mixture thereof. More preferably, the crystallizable material is selected from xylitol, mannitol, or any mixture thereof.

[0023] Preferably, the stearate is an alkali metal salt or an alkaline earth metal salt of stearic acid, or a mixture thereof. Preferably, the stearate is selected from magnesium stearate, calcium stearate, sodium stearate, or any mixture thereof. More preferably, the stearate is selected from magnesium stearate, calcium stearate, or any mixture thereof. More preferably, the stearate is magnesium stearate.

[0024] It should be noted that the term "stearic acid" refers to stearic acid itself, but also to a mixture of stearic acid and palmitic acid in a variable proportion (Handbook of Pharmaceutical Excipients, 8th edition).

[0025] Preferably, the coating composition further includes a polymer binder.

[0026] The present invention also relates to a sugar coating composition comprising the following:

[0027] (a) A solid, said solid being composed of the following:

[0028] (a.1) 80.0% to 95.0%, preferably 85.0% to 95.0%, preferably 86.0% to 94.0%, preferably 87.0% to 93.0%, preferably 88.0% to 92.0%, preferably 89.0% to 91.0%, for example 85% to 90%, or 86% to 90%, or 90% of a crystallizable material selected from sugars, sugar alcohols or any mixture thereof;

[0029] (a.2) 4.0% to 19.0%, preferably 4.0% to 18.0%, preferably 4.0% to 17.0%, preferably 4.0% to 16.0%, preferably 4.0% to 15.0%, preferably 4.0% to 14.0%, preferably 4.0% to 13.0%, preferably 4.0% to 12.0%, preferably 4.0% to 11.0%, preferably 4.0% to 10.0%, for example 4.0%, or 6.0%, or 8.0%, or 10.0% of stearates (e.g., magnesium stearate);

[0030] (a.3) 1.0% to 10.0%, preferably 1.0% to 9.0%, preferably 1.0% to 8.0%, preferably 1.0% to 7.0%, preferably 1.0% to 6.0%, preferably 1.0% to 5.0%, preferably 1.0% to 4.0%, preferably 2.0% to 4.0%, preferably 3.0% to 4.0%, preferably 4% of a polymer binder;

[0031] (a.4) Optionally no more than 3.0%, preferably no more than 2.0%, preferably no more than 1.5%, preferably no more than 0.010%, preferably no more than 0.005% of TiO2, preferably no TiO2;

[0032] (a.5) optionally up to 1.0%, preferably up to 0.5%, preferably up to 0.10%, preferably up to 0.05%, preferably up to 0.010%, preferably up to 0.005% of pigment;

[0033] (a.6) Optionally no more than 3.0%, preferably no more than 2.0%, preferably no more than 1.0%, preferably no more than 0.5%, preferably no more than 0.10%, preferably no more than 0.005% of other components, and even more preferably no other components;

[0034] The percentages from (a.1) to (a.6) are expressed as weight relative to the total weight of the solids, and their sum equals 100%; and

[0035] (b) Optionally a solvent, preferably water.

[0036] Preferably, the crystallizable material is selected from xylitol, sucrose, erythritol, mannitol, dextrose, isomaltitol, maltitol, sorbitol, or any mixture thereof. More preferably, the crystallizable material is selected from xylitol, mannitol, or any mixture thereof.

[0037] Preferably, the stearate is an alkali metal salt or an alkaline earth metal salt of stearic acid, or a mixture thereof. Preferably, the stearate is selected from magnesium stearate, calcium stearate, sodium stearate, or any mixture thereof. More preferably, the stearate is selected from magnesium stearate, calcium stearate, or any mixture thereof. More preferably, the stearate is magnesium stearate.

[0038] The present invention also relates to a sugar coating method comprising coating a solid core with a sugar coating composition according to the present disclosure.

[0039] The present invention also relates to the use of a stearate in a solid form of a sugar coating to improve the surface of the sugar coating layer. Preferably, the use is for improving the color of the coating layer, and / or increasing its brightness, and / or increasing its opacity, and / or increasing its smoothness, and / or reducing its roughness, and / or reducing its wrinkles. More preferably, the use is for improving the smoothness of the sugar coating layer, and / or reducing its roughness, and / or reducing its wrinkles.

[0040] The present invention also relates to the use of a composition comprising a crystallizable material and a stearate for sugar coating a solid core. Attached Figure Description

[0041] Other features, details and advantages will be shown in the following detailed description and in the accompanying drawings.

[0042] Figure 1

[0043] [ Figure 1 [This is a graph showing wrinkle measurements performed on solid forms of coated sugar from the market, solid forms of coated sugar compositions according to the present disclosure, or solid forms of comparative coated sugar compositions.]

[0044] Figure 2

[0045] [ Figure 2 [A graph showing the coating thickness of a solid form of a coating composition according to the present disclosure or a comparison of the coating thickness of a solid form of a coating composition.]

[0046] Figure 3

[0047] Figure 3 It is a graph showing the viscosity of various coating formulations prepared with 60% solids at room temperature or with 70% solids at 70°C.

[0048] Figure 4

[0049] Figure 4It is a graph showing the turbidity of various coated formulations prepared with 60% solids at room temperature or with 70% solids at 70°C. Detailed Implementation

[0050] The accompanying drawings and the following detailed description essentially contain some specific elements. They can be used to improve the understanding of the invention and, if necessary, to define the invention.

[0051] It must be noted that, unless the context clearly indicates otherwise, as used in this specification and the appended claims, the singular forms “a” and “the” include a plurality of references and mean “at least one” or “one or more”. For example, mentioning a component in the singular is intended to include multiple components. Thus, “a” crystallizable material or “a” stearate means “one or more” crystallizable materials or “one or more” stearates, respectively.

[0052] The terms “comprise” and “include” are synonymous. These terms are inclusive and open-ended, and do not exclude the existence of additional, unlisted features, provided that they do not impede the implementation of the disclosed or claimed subject matter.

[0053] When the phrase "composes of" is used, there are no other features in the disclosed or claimed subject matter other than the features following the phrase.

[0054] When the term “comprising” or one of its synonyms is used herein, the subject matter disclosed or claimed by this invention may include the use of “composed of”.

[0055] 1. A solid form of a coating composition containing crystallizable material and stearate.

[0056] Therefore, this disclosure primarily relates to a solid form of a coated sugar composition comprising a crystallizable material and a stearate.

[0057] In other words, this disclosure relates to a solid form comprising a solid core and at least one coating layer, said coating layer being obtained from a coating composition comprising a crystallizable material and a stearate. Preferably, said coating layer is an outer layer.

[0058] In sugar coatings, the term "solid form" conventionally refers to any solid presentation of a substance. Typical examples include tablets, hard capsules, soft capsules, pellets, microspheres, granules, seeds, cookies, breakfast cereals, confectionery such as chewing gum, boiled candy, chewable candy, gummies, chocolate, fruits and vegetables, or products in powder and / or crystalline form. These solid forms may be intended for, for example, food, pharmaceutical, veterinary, or cosmetic use. They may be intended for human, adult, or child use, or for animal use. They may also be intended for chemical or agrochemical use, although in this disclosure, solid forms intended for ingestion (i.e., "oral solid forms") are preferred. Preferably, the solid forms according to this disclosure are selected from tablets and chewing gum.

[0059] In sugar coating methods, the solid form to be coated is conventionally referred to as a "solid core". The solid core may be uncoated or already coated with one or more layers, such as a film coating or even a sugar coating layer, which is preferably formed in the same equipment used to perform the sugar coating method according to the present disclosure.

[0060] Therefore, the solid form coating the sugar-coated composition according to this disclosure may further include one or more inner coating layers, particularly a film coating layer and / or a sugar-coated layer. Specifically, it is coated with "one" sugar-coated composition of this disclosure, meaning it is coated with "at least one" or "one or more" sugar-coated compositions of this disclosure. Preferably, the solid form coating the sugar-coated composition of this disclosure does not include any other sugar-coated layers, i.e., sugar-coated layers obtained from compositions not according to this disclosure.

[0061] As used herein, the term "solid form of coated sugar composition" is also referred to as "solid form of coated sugar composition".

[0062] The sugar coating composition disclosed herein comprises stearate and crystallizable material.

[0063] The stearate according to this disclosure is preferably an alkali metal salt or an alkaline earth metal salt of stearic acid, or a mixture thereof. Preferably, the stearate is selected from magnesium stearate, calcium stearate, sodium stearate, or any mixture thereof. It is preferably selected from magnesium stearate, calcium stearate, or any mixture thereof. It is more preferably magnesium stearate.

[0064] More preferably, in the coating composition according to the present disclosure, the stearate is composed entirely of an alkali metal salt or an alkaline earth metal salt of stearic acid, or a mixture thereof. Preferably, in the coating composition according to the present disclosure, the stearate is composed entirely of magnesium stearate, calcium stearate, sodium stearate, or a mixture thereof. Preferably, in the coating composition according to the present disclosure, the stearate is composed entirely of magnesium stearate, calcium stearate, or a mixture thereof. More preferably, in the coating composition according to the present disclosure, the stearate is composed entirely of magnesium stearate, i.e., magnesium stearate is the only stearate in the coating composition.

[0065] Preferably, the specific surface area of ​​the stearate (e.g., magnesium stearate) according to this disclosure is equal to or greater than 1 m². 2 / g, preferably equal to or greater than 2m 2 / g, preferably equal to or greater than 3m 2 / g, preferably equal to or greater than 4m 2 / g, preferably equal to or greater than 5m 2 / g, preferably equal to or greater than 6m 2 / g, preferably equal to or greater than 7m 2 / g. Preferably, it is equal to or less than 30m. 2 / g, preferably equal to or less than 25m 2 / g, preferably equal to or less than 20m 2 / g, preferably equal to or less than 15m 2 / g, preferably equal to or less than 14m 2 / g, preferably equal to or less than 13m 2 / g, preferably equal to or less than 12m 2 / g, preferably equal to or less than 11m 2 / g, preferably equal to or less than 10m 2 / g, preferably equal to or less than 9m 2 / g. For example, it equals 8m. 2 / g. This specific surface area can be determined by those skilled in the art using the BET (Brunauer, Emmett and Teller) method. It can be determined, for example, by a specific surface area analyzer (e.g., BECKMAN-COULTER, SA3100 model), based on nitrogen absorption tests performed on the surface of the analyzed product, following the techniques described in the article BET Surface Area by Nitrogen Absorption by S. BRUNAUER et al. (Journal of American Chemical Society, 60, 309, 1938). BET analysis is performed at three points.

[0066] Preferably, the amount of stearate (e.g., magnesium stearate) in the coating composition according to this disclosure is equal to or greater than 1%, the percentage being expressed by weight relative to the total solid weight of the coating composition. It is preferably equal to or greater than 2%, preferably equal to or greater than 3%, preferably equal to or greater than 4%, preferably equal to or greater than 5%, preferably equal to or greater than 6%, preferably equal to or greater than 7%, preferably equal to or greater than 8%. It is generally equal to or less than 20%, preferably equal to or less than 19%, preferably equal to or less than 18%, preferably equal to or less than 17%, preferably equal to or less than 16%, preferably equal to or less than 15%, preferably equal to or less than 14%, preferably equal to or less than 13%, preferably equal to or less than 12%, preferably equal to or less than 11%, preferably equal to or less than 10%. For example, it is equal to 4%, or equal to 6%, or equal to 8%, or equal to 10%.

[0067] In this disclosure, the term "solid" refers to a component other than a solvent.

[0068] The sugar coating composition disclosed herein comprises stearate and a crystallizable material, said crystallizable material being composed of one or more crystallizable substances.

[0069] In the sugar coating industry, the term "crystallizable material" traditionally refers to a substance or mixture of substances that can crystallize during a sugar coating process by evaporating the solvent in which the substance or mixture of substances is dissolved. This crystallizable material forms a hard, crystalline coating on the surface of a solid core. Sugar coating should not be confused with film coating. In film coating, compositions based on film-forming polymers (e.g., cellulose derivatives such as hydroxypropyl methylcellulose (HPMC) or polyvinyl alcohol (PVA)) are used, rather than compositions containing crystallizable materials (sometimes referred to as "syrup"). This film-forming composition forms a non-crystalline film on the tablet surface.

[0070] Preferably, the crystallizable material according to this disclosure is selected from sugars, sugar alcohols, or any mixture thereof, and more preferably from monomers, dimers, or any mixture thereof.

[0071] Preferably, the crystallizable material according to this disclosure is selected from xylitol, sucrose, erythritol, mannitol, dextrose, isomaltitol, maltitol, sorbitol, or any mixture thereof. More preferably, the crystallizable material according to this disclosure is selected from xylitol, mannitol, or any mixture thereof. More preferably, the crystallizable material according to this disclosure is xylitol.

[0072] More preferably, in the sugar coating composition according to the present disclosure, the crystallizable material consists entirely of sugar, sugar alcohol, or mixtures thereof. Preferably, in the sugar coating composition according to the present disclosure, the crystallizable material consists entirely of xylitol, sucrose, erythritol, mannitol, dextrose, isomaltitol, maltitol, sorbitol, or mixtures thereof. Preferably, in the sugar coating composition according to the present disclosure, the crystallizable material consists entirely of xylitol, mannitol, or mixtures thereof. More preferably, in the sugar coating composition according to the present disclosure, the crystallizable material consists entirely of xylitol, i.e., xylitol is the only crystallizable material in the sugar coating composition.

[0073] Preferably, the amount of crystallizable material in the coating composition according to this disclosure is equal to or greater than 50%, the percentage being expressed by weight relative to the total solid weight of the coating composition. It is preferably equal to or greater than 70%, preferably equal to or greater than 80%, preferably equal to or greater than 85%, preferably equal to or greater than 86%, preferably equal to or greater than 87%, preferably equal to or greater than 88%, preferably equal to or greater than 89%. It is generally equal to or less than 99%, preferably equal to or less than 95%, preferably equal to or less than 94%, preferably equal to or less than 93%, preferably equal to or less than 92%, preferably equal to or less than 91%. For example, it is 85% to 90%, or 86% to 90%, or 90%.

[0074] Preferably, the weight ratio of the crystallizable material to the stearate is selected from 2:1 to 50:1, preferably 3:1 to 45:1, preferably 4:1 to 40:1, preferably 5:1 to 35:1, preferably 5:1 to 30:1, preferably 5:1 to 25:1, preferably 6:1 to 20:1, preferably 7:1 to 15:1, preferably 7:1 to 12:1, preferably 7:1 to 10:1. For example, it is equal to 9:1, or equal to 11:1, or equal to 16:1, or equal to 24:1.

[0075] Preferably, the coating composition according to this disclosure further includes a polymer binder.

[0076] This polymer binder can be selected from any suitable starch compound, PVA, gum arabic, or any mixture thereof. It is preferably selected from starch compounds, and more preferably from hydrolyzed functionalized starches.

[0077] The term "starch compound" conventionally refers to a substance obtained from starch. It is noted that the term "starch" conventionally refers to starch isolated from any suitable plant source using any technique well known to those skilled in the art. Isolated starch typically contains no more than 3% impurities; said 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 substances, and fibrous residue. Suitable plant sources include, for example, legumes, cereals, and tubers. The starch compounds according to this disclosure can be derived from any suitable plant source, including, for example, legumes (e.g., peas), cereals (e.g., corn, rice, wheat, oats), and tubers (e.g., potatoes, cassava).

[0078] The hydrolyzed starch compounds according to this disclosure can be hydrolyzed by any suitable technique, such as by acid treatment, heat treatment, enzymatic treatment, or a combination thereof. They can be dextrins, including maltodextrin or caramelized dextrin. "Maltodextrin" conventionally refers to a hydrolyzed starch compound having a dextran equivalent of 2 to 20. They are generally obtained by acid or enzymatic hydrolysis. "Caramelized dextrin" is conventionally obtained in the presence of a small amount of water by the action of high temperature (generally at least 100°C), combined with the action of acid or base or non-acid or base ("dextrins (British gums)"). This treatment conventionally leads to rebranching and the formation of so-called "atypical boundaries," thus caramelized dextrins are structurally different from other hydrolyzed starches, particularly maltodextrins. Preferably, the hydrolyzed starch compounds according to this disclosure are obtained by acid hydrolysis. Preferably, the hydrolyzed starch compounds according to this disclosure are not caramelized dextrins.

[0079] Hydrolyzed starch compounds must be well distinguished from glucose, glucose syrup, and cyclodextrin, which are hydrolyzed to such an extent that they are still referred to as "starch," as is generally understood by those skilled in the art. In other words, glucose, glucose syrup, and cyclodextrin are not hydrolyzed starches in the sense of this disclosure.

[0080] The functionalized starch compounds according to this disclosure are hydrolyzed, resulting in a lower molecular weight compared to the natural starch from which they are derived. Therefore, alternatively or complementaryly, the hydrolyzed and functionalized starch compounds according to this disclosure can be defined by their weight-average molecular weight (Mw), preferably below 10,000 kDa, as determined by size exclusion chromatography (HPSEC) attached to a multiangle laser-light scattering (MALLS) and refractive index (RI) detector. Preferably, Mw is determined by diluting a sample of the starch compound in a mixture of dimethyl sulfoxide and 0.1 M sodium nitrate. Two columns with porosities of 100 Å and 1000 Å are used. Elution is performed 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 weight-average molecular weight (Mw) of the hydrolyzed and functionalized starch according to this disclosure is equal to or less than 9000 kDa, more preferably equal to or less than 8000 kDa, more preferably equal to or less than 7000 kDa, more preferably equal to or less than 6000 kDa, more preferably equal to or less than 5000 kDa, more preferably equal to or less than 4000 kDa, more preferably less than 4000 kDa, and more preferably equal to or less than 3500 kDa. It is preferably equal to or greater than 100 kDa, more preferably equal to or greater than 200 kDa, more preferably equal to or greater than 400 kDa, more preferably equal to or greater than 600 kDa, more preferably equal to or greater than 800 kDa, more preferably equal to or greater than 900 kDa, and more preferably equal to or greater than 1000 kDa. For example, it is equal to 3500 kDa or equal to 1000 kDa.

[0081] Preferably, the viscosity of the hydrolyzed and functionalized starch compound according to this disclosure in water at a shear rate of 100 s⁻¹ at 20°C is preferably less than 10,000 mPa·s, as measured for an aqueous solution comprising 10% dry weight of the starch compound, and the viscosity is measured on a rheometer using a 5 cm 1° cone-plate geometry. Preferably, the viscosity is equal to or less than 5,000 mPa·s, more preferably equal to or less than 1,000 mPa·s, more preferably equal to or less than 500 mPa·s, more preferably equal to or less than 100 mPa·s, and more preferably equal to or less than 50 mPa·s. It is generally greater than 1 mPa·s, preferably equal to or greater than 5 mPa·s, more preferably equal to or greater than 10 mPa·s, and more preferably equal to or greater than 15 mPa·s. For example, it is equal to 18 mPa·s or equal to 42 mPa·s.

[0082] The hydrolyzed starch compounds according to this disclosure are also functionalized. In other words, the starch compounds according to this disclosure have at least one functional group added to their hydroxyl functional groups. Preferably, the functionalized starch compounds according to this disclosure are etherified and / or esterified, and more preferably etherified. They can be selected from hydroxypropyl starch, acetyl starch, hydroxyethyl starch, octenyl succinate starch, or mixtures thereof. Preferably, they are hydroxypropyl starch.

[0083] In the case of hydrolyzed hydroxypropyl starch, the starch compound preferably has a hydroxypropyl group content of 0.5% to 10%; said percentage is expressed as the dry weight of hydroxypropyl groups relative to the total dry weight of the hydrolyzed hydroxypropyl starch. The hydroxypropyl group content can be determined by those skilled in the art, for example by proton nuclear magnetic resonance (proton NMR), preferably according to a method conforming to the European Pharmacopoeia (“STARCH, HYDROXYPROPYL PREGELATINISED”) which came into effect on June 1, 2023. It is preferably between 0.5% and 9%, more preferably between 0.5% and 8%, more preferably between 0.5% and 7%, for example equal to 7%.

[0084] Preferably, the cold water solubility of the hydrolyzed and functionalized starch compound according to this disclosure is equal to or greater than 50%, the percentage being expressed as the dry weight of soluble starch relative to the total weight of starch. Preferably, this cold water solubility is equal to or greater than 60%, more preferably equal to or greater than 70%, more preferably equal to or greater than 80%, more preferably equal to or greater than 90%, and more preferably equal to or greater than 95%. This solubility can be determined, for example, by dissolving 5 grams of the starch compound in 200 mL of distilled water at 20°C. The dry weight of the dissolved compound can be determined after centrifugation and drying of the supernatant.

[0085] Preferably, the hydrolyzed and functionalized starch compound according to this disclosure is pregelatinized. Pregelatinization conventionally refers to the starch compound particles no longer exhibiting birefringence (lack of a crystalline phase) under polarized light under an optical microscope. Pregelatinization can typically be obtained from birefringent starch or birefringent starch compounds via heat treatment in the presence of water (generally 50°C–100°C, depending particularly on the plant source of the starch) (often also referred to as “cooking”) and further drying (after and / or simultaneously with cooking).

[0086] Preferably, the hydrolyzed and functionalized starch compounds according to this disclosure are derived from legume and / or cereal starches, more preferably from pea or corn starches, more preferably from pea starches, and more preferably from smooth pea starches. Preferably, the amylose content of the pea starch is between 20% and 50%, more preferably between 30% and 45%, more preferably between 30% and 40%, for example, equal to 35%; the percentage is expressed as the dry weight of amylose relative to the total dry weight of the starch. This amylose content can be determined by those skilled in the art through potentiometric analysis of iodine absorbed by amylose to form a complex. Preferably, the amylose content of the corn starch is greater than 5%, preferably 10% to 40%, more preferably 15% to 35%, more preferably 20% to 30%, for example, equal to 25%; the percentage is expressed as the dry weight of amylose relative to the total dry weight of the starch.

[0087] The hydrolyzed and functionalized starch compounds according to this disclosure may undergo other chemical and / or physical modifications besides the previously exposed preferred chemical and / or physical modifications, provided that the starch compound does not interfere with the desired properties, particularly with respect to the safety and properties of the coating compositions obtained from the starch compound. However, and because this does not appear to be necessary in this invention, the hydrolyzed and functionalized starch compounds according to this disclosure are preferably not further modified.

[0088] Preferably, the hydrolyzed and functionalized starch compound according to this disclosure is the product of CAS No. 9049-76-7. Preferably, the hydrolyzed and functionalized starch compound according to this disclosure conforms to the European Pharmacopoeia (“STARCH, HYDROXYPROPYL PREGELATINISED”) which came into effect on June 1, 2023.

[0089] Particularly useful hydrolyzed and functionalized starch compounds are commercially available. For example, the hydrolyzed hydroxypropyl starch LYCOAT commercially available by the applicant could be mentioned. ® RS 720 (CAS No. 113894-92-1) or LYCOAT ® RS 780 (CASN°113894-92-1).

[0090] Preferably, the amount of polymer binder in the coating composition according to this disclosure is equal to or greater than 1.0%, preferably equal to or greater than 2.0%, preferably equal to or greater than 3.0%, and preferably equal to or greater than 4%; the percentage is expressed by weight relative to the total solid weight of the coating composition. It is preferably equal to or less than 10%, preferably equal to or less than 9%, preferably equal to or less than 8%, preferably equal to or less than 7%, preferably equal to or less than 6%, preferably equal to or less than 5%, and preferably equal to or less than 4%. For example, it is equal to 4%.

[0091] The coating composition according to this disclosure can be used during the coating step itself and / or during the smoothing step. It is preferably used for the coating itself, and if a smoothing step is performed, it is also used for smoothing.

[0092] The coating compositions according to this disclosure may include one or more components other than those described above, provided that such one or more components do not interfere with the desired properties, particularly with respect to the safety and properties of the coating composition obtained from such one or more components. Such other components may, for example, be selected from:

[0093] - Pigments and opacifiers (e.g., titanium dioxide, calcium carbonate, deep red pigment (lake));

[0094] - Flavoring agents, sweeteners;

[0095] - Active ingredients, such as active ingredients in pharmaceuticals, nutritional supplements, or veterinary medicines;

[0096] - Cellulose (e.g., cellulose, cellulose powder, microcrystalline cellulose (MCC));

[0097] - or any mixture thereof.

[0098] When TiO2 is included, the amount of TiO2 in the coating composition according to this disclosure is equal to or less than 5%, preferably equal to or less than 4%, preferably equal to or less than 3%, preferably equal to or less than 2%, preferably equal to or less than 1%, preferably equal to or less than 0.5%, preferably equal to or less than 0.10%, preferably equal to or less than 0.005%; the percentage is expressed by weight relative to the total solid weight of the coating composition.

[0099] However, preferably, the coating composition according to this disclosure does not include TiO2 (i.e., it is a coating composition without TiO2).

[0100] More generally, when other ingredients include opacifiers, the total amount of opacifiers is preferably equal to or less than 5%, preferably equal to or less than 4%, preferably equal to or less than 3%, preferably equal to or less than 2%, preferably equal to or less than 1%, preferably equal to or less than 0.5%, preferably equal to or less than 0.10%, preferably equal to or less than 0.005%; the percentages are expressed by weight relative to the total solid weight of the sugar coating composition.

[0101] However, preferably, the other components do not include any light-blocking agents.

[0102] When MCC is included, the amount of MCC in the coating composition according to this disclosure is preferably equal to or less than 5%, preferably equal to or less than 4%, preferably equal to or less than 3%, preferably equal to or less than 2%, preferably equal to or less than 1%, preferably equal to or less than 0.5%, preferably equal to or less than 0.10%, preferably equal to or less than 0.005%; the percentage is expressed by weight relative to the total solid weight of the coating composition.

[0103] However, preferably, the coating composition according to this disclosure does not include MCC.

[0104] When cellulose is included, the total amount of cellulose in the coating composition according to this disclosure is preferably equal to or less than 5%, preferably equal to or less than 4%, preferably equal to or less than 3%, preferably equal to or less than 2%, preferably equal to or less than 1%, preferably equal to or less than 0.5%, preferably equal to or less than 0.10%, preferably equal to or less than 0.005%; the percentage is expressed by weight relative to the total solid weight of the coating composition.

[0105] However, preferably, the coating composition according to this disclosure does not contain any cellulose.

[0106] When pigments are included, their amounts are preferably equal to or less than 2%, preferably equal to or less than 1%, preferably equal to or less than 1.0%, preferably equal to or less than 0.5%, preferably equal to or less than 0.10%, and preferably equal to or less than 0.005%; the percentages are expressed by weight relative to the total solid weight of the coating composition. When pigments are used, they are preferably introduced at the end of the coating process or during the smoothing step for cost reasons. Therefore, when referring to the percentage of pigments in the coating composition, it means herein the percentage of pigments relative to the total coating composition being sprayed, not the percentage when the pigments are added to the composition.

[0107] The sugar coating composition to be used must be in liquid form, preferably using a polar solvent, and more preferably water.

[0108] Therefore, in a preferred embodiment, the sugar coating composition according to this disclosure is a liquid composition comprising a solvent, preferably a polar solvent, and preferably water.

[0109] Choose the amount of solvent appropriate for dissolving crystallizable materials.

[0110] Generally, especially when the liquid coating composition is an aqueous coating composition, the solids content of the liquid coating composition is equal to or greater than 20%, preferably equal to or greater than 30%, preferably equal to or greater than 40%, and preferably equal to or greater than 50%; the percentage is expressed by weight relative to the total weight of the coating composition. Generally, the solids content of the liquid coating composition is equal to or less than 90%, preferably equal to or less than 80%, and preferably equal to or less than 70%. For example, it is equal to 60%.

[0111] In another preferred embodiment, the coating composition according to this disclosure is a ready-to-use powder composition. In this case, the coating composition is mixed with a solvent, preferably water, before use.

[0112] Preferably, the percentage of coating in solid form covering the sugar coating composition according to this disclosure is equal to or greater than 1%. This coating percentage (also referred to as "weight gain") is determined as follows:

[0113] [Mathematical Formula 1]

[0114]

[0115] Preferably, the coating percentage is equal to or greater than 2%, preferably equal to or greater than 5%, preferably equal to or greater than 10%, preferably equal to or greater than 15%, preferably equal to or greater than 20%, preferably equal to or greater than 25%. It is preferably equal to or less than 50%, preferably equal to or less than 45%, preferably equal to or less than 40%, preferably equal to or less than 35%. For example, it is equal to 30%.

[0116] Preferably, the thickness of the solid coating layer covering the sugar coating composition according to this disclosure is equal to or greater than 50 μm, preferably equal to or greater than 100 μm, equal to or greater than 150 μm, equal to or greater than 200 μm, equal to or greater than 250 μm, or equal to or greater than 300 μm. It is preferably equal to or less than 1000 μm, preferably equal to or less than 900 μm, preferably equal to or less than 800 μm, preferably equal to or less than 700 μm, or preferably equal to or less than 600 μm. For example, it is 300 μm to 500 μm.

[0117] It should be understood that these coating percentages and coating thicknesses refer to the coating layer obtained by coating a solid form with the sugar-coating composition according to this disclosure.

[0118] 2. A preferred coating composition comprising a crystallizable material and a stearate.

[0119] The present invention also covers sugar coating compositions that perform particularly well within the context of the present invention.

[0120] Therefore, the present invention also covers a coating composition comprising:

[0121] (a) A solid, said solid being composed of the following:

[0122] (a.1) 80.0% to 95.0%, preferably 85.0% to 95.0%, preferably 86.0% to 94.0%, preferably 87.0% to 93.0%, preferably 88.0% to 92.0%, preferably 89.0% to 91.0%, for example 90% or 86% to 90% of crystallizable material selected from sugars, sugar alcohols or any mixture thereof;

[0123] (a.2) 4.0% to 19.0%, preferably 4.0% to 18.0%, preferably 4.0% to 17.0%, preferably 4.0% to 16.0%, preferably 4.0% to 15.0%, preferably 4.0% to 14.0%, preferably 4.0% to 13.0%, preferably 4.0% to 12.0%, preferably 4.0% to 11.0%, preferably 4.0% to 10.0%, for example 4.0%, or 6.0%, or 8.0%, or 10.0% of stearates (e.g., magnesium stearate);

[0124] (a.3) 1.0% to 10.0%, preferably 1.0% to 9.0%, preferably 1.0% to 8.0%, preferably 1.0% to 7.0%, preferably 1.0% to 6.0%, preferably 1.0% to 5.0%, preferably 1.0% to 4.0%, preferably 2.0% to 4.0%, preferably 3.0% to 4.0%, preferably 4% of a polymer binder;

[0125] (a.4) Optionally no more than 3.0%, preferably no more than 2.0%, preferably no more than 1.5%, preferably no more than 0.010%, preferably no more than 0.005% of TiO2, preferably no TiO2;

[0126] (a.5) optionally up to 1.0%, preferably up to 0.5%, preferably up to 0.10%, preferably up to 0.05%, preferably up to 0.010%, preferably up to 0.005% of pigment;

[0127] (a.6) Optionally no more than 3.0%, preferably no more than 2.0%, preferably no more than 1.0%, preferably no more than 0.5%, preferably no more than 0.10%, preferably no more than 0.005% of other components, and even more preferably no other components;

[0128] The percentages from (a.1) to (a.6) are expressed as weight relative to the total weight of the solids, and their sum equals 100%; and

[0129] (b) Optionally a solvent, preferably water.

[0130] In a preferred embodiment, the coating composition is a liquid coating composition, which comprises the following:

[0131] (a) 40% to 80%, preferably 45% to 75%, preferably 50% to 70%, preferably 55% to 65%, for example 60% solids, said solids being composed of:

[0132] (a.1) 80.0% to 95.0%, preferably 85.0% to 95.0%, preferably 86.0% to 94.0%, preferably 87.0% to 93.0%, preferably 88.0% to 92.0%, preferably 89.0% to 91.0%, for example 90% or 86% to 90% of crystallizable material selected from sugars, sugar alcohols or any mixture thereof;

[0133] (a.2) 4.0% to 19.0%, preferably 4.0% to 18.0%, preferably 4.0% to 17.0%, preferably 4.0% to 16.0%, preferably 4.0% to 15.0%, preferably 4.0% to 14.0%, preferably 4.0% to 13.0%, preferably 4.0% to 12.0%, preferably 4.0% to 11.0%, preferably 4.0% to 10.0%, for example 4.0%, or 6.0%, or 8.0%, or 10.0% of stearates (e.g., magnesium stearate);

[0134] (a.3) 1.0% to 10.0%, preferably 1.0% to 9.0%, preferably 1.0% to 8.0%, preferably 1.0% to 7.0%, preferably 1.0% to 6.0%, preferably 1.0% to 5.0%, preferably 1.0% to 4.0%, preferably 2.0% to 4.0%, preferably 3.0% to 4.0%, preferably 4% of a polymer binder;

[0135] (a.4) Optionally no more than 3.0%, preferably no more than 2.0%, preferably no more than 1.5%, preferably no more than 0.010%, preferably no more than 0.005% of TiO2, preferably no TiO2;

[0136] (a.5) optionally up to 1.0%, preferably up to 0.5%, preferably up to 0.10%, preferably up to 0.05%, preferably up to 0.010%, preferably up to 0.005% of pigment;

[0137] (a.6) Optionally no more than 3.0%, preferably no more than 2.0%, preferably no more than 1.0%, preferably no more than 0.5%, preferably no more than 0.10%, preferably no more than 0.005% of other components, and even more preferably no other components;

[0138] The percentages from (a.1) to (a.6) are expressed as weight relative to the total weight of the solids, and their sum equals 100%; and

[0139] (b) 60% to 20%, preferably 55% to 25%, preferably 50% to 30%, preferably 45% to 35%, for example 40% of a solvent, said solvent being water;

[0140] The percentages in (a) and (b) are expressed relative to the total weight of the liquid coating composition, and their sum equals 100%.

[0141] Preferably, the Brookfield viscosity of the liquid coating composition is equal to or greater than 150 mPa·s and less than 400 mPa·s, which is measured, for example, using a Brookfield viscometer (e.g., a DV-I+ Brookfield viscometer) with a suitable rotor at a rotational speed of 100 rpm, according to the method given in Example Section 4. Preferably, the Brookfield viscosity is 150 mPa·s to 300 mPa·s, preferably 150 mPa·s to 300 mPa·s, preferably 200 mPa·s to 300 mPa·s, preferably 200 mPa·s to 250 mPa·s, or about 250 mPa·s.

[0142] In another preferred embodiment, the coating composition is a powdered coating composition, which comprises the following:

[0143] (a.1) 80.0% to 95.0%, preferably 85.0% to 95.0%, preferably 86.0% to 94.0%, preferably 87.0% to 93.0%, preferably 88.0% to 92.0%, preferably 89.0% to 91.0%, for example 90% or 86% to 90% of crystallizable material selected from sugars, sugar alcohols or any mixture thereof;

[0144] (a.2) 4.0% to 19.0%, preferably 4.0% to 18.0%, preferably 4.0% to 17.0%, preferably 4.0% to 16.0%, preferably 4.0% to 15.0%, preferably 4.0% to 14.0%, preferably 4.0% to 13.0%, preferably 4.0% to 12.0%, preferably 4.0% to 11.0%, preferably 4.0% to 10.0%, for example 4.0%, or 6.0%, or 8.0%, or 10.0% of stearates (e.g., magnesium stearate);

[0145] (a.3) 1.0% to 10.0%, preferably 1.0% to 9.0%, preferably 1.0% to 8.0%, preferably 1.0% to 7.0%, preferably 1.0% to 6.0%, preferably 1.0% to 5.0%, preferably 1.0% to 4.0%, preferably 2.0% to 4.0%, preferably 3.0% to 4.0%, preferably 4% of a polymer binder;

[0146] (a.4) Optionally no more than 3.0%, preferably no more than 2.0%, preferably no more than 1.5%, preferably no more than 0.010%, preferably no more than 0.005% of TiO2, preferably no TiO2;

[0147] (a.5) optionally up to 1.0%, preferably up to 0.5%, preferably up to 0.10%, preferably up to 0.05%, preferably up to 0.010%, preferably up to 0.005% of pigment;

[0148] (a.6) Optionally no more than 3.0%, preferably no more than 2.0%, preferably no more than 1.0%, preferably no more than 0.5%, preferably no more than 0.10%, preferably no more than 0.005% of other components, and even more preferably no other components;

[0149] The percentages are expressed by weight relative to the total weight of the powdered coating composition, and their sum equals 100%.

[0150] Preferably, the properties of the ingredients used are as described above.

[0151] 3. Sugar coating method and the solid form obtained therefrom

[0152] This disclosure also relates to a sugar-coated coating. method In particular, for obtaining a sugar coating in solid form that coats the sugar coating composition according to the present disclosure. method The sugar coating method This includes coating a solid core with a coating composition according to the present disclosure, namely a coating composition comprising a crystallizable material and a stearate (e.g., magnesium stearate).

[0153] Preferably, the sugar coating composition is as described in part 1 or part 2 above.

[0154] The coating composition according to this disclosure can be used during the coating step itself, and / or during the smoothing step. It is preferably used at least during the coating step itself.

[0155] Therefore, according to this disclosure method Preferably, it includes or consists of the following:

[0156] (1) An optional step of coating a solid core with a thin film.

[0157] (2) The step of coating the solid core with the sugar coating composition according to the present disclosure.

[0158] (3) Preferably, an optional step of smoothing the solid core is performed immediately after step (2).

[0159] (4) An optional polishing step performed after step (2) or after step (3) (if the former is performed).

[0160] (5) An optional printing step performed after step (2) or after step (3) (if the former is performed), or an optional printing step performed after step (4) (if the former is performed).

[0161] (6) The final step of collecting the solid form of the sugar coating thus obtained.

[0162] Coloring can be performed during the coating step (2) or during the smoothing step (3) by adding at least one pigment to the composition. When performed during the coating step (2), the pigment is preferably added during the final stage of the coating step (2) for cost reasons.

[0163] Preferably, the sugar coating step (2) includes:

[0164] - Step (2.a) of spraying the sugar coating composition onto a bed of moving solid cores, the cores being placed in a chamber equipped with a perforated rotating drum, the spraying being performed by a compressed air nozzle;

[0165] - At least one step (2.b) of the coating composition sprayed during the drying of step (2.a).

[0166] The method according to this disclosure may further include the step of preparing the sugar coating composition according to this disclosure by preferably mixing the powdered sugar coating composition according to this disclosure with any suitable solvent, preferably water.

[0167] Preferably, the solids content of the liquid coating composition thus obtained is equal to or greater than 20%, preferably equal to or greater than 30%, preferably equal to or greater than 40%, and preferably equal to or greater than 50%; the percentage is expressed by weight relative to the total weight of the coating composition. Generally, the solids content of the liquid coating composition is equal to or less than 90%, preferably equal to or less than 80%, and preferably equal to or less than 70%. For example, it is equal to 60%.

[0168] Preferably, the Brookfield viscosity of the liquid coating composition according to this disclosure is equal to or greater than 150 mPa·s and less than 400 mPa·s, said Brookfield viscosity being measured, for example, using a Brookfield viscometer (e.g., a DV-I+ Brookfield viscometer) with a suitable rotor at a rotational speed of 100 rpm, according to the method given in Example Section 4. Preferably, said Brookfield viscosity is 150 mPa·s to 300 mPa·s, preferably 150 mPa·s to 300 mPa·s, preferably 200 mPa·s to 300 mPa·s, preferably 200 mPa·s to 250 mPa·s, or about 250 mPa·s.

[0169] Preferably, the coating composition is subjected to high-speed stirring during the coating process. This speed will depend on the volume of the coating composition and the shape and size of the propeller.

[0170] In a preferred embodiment, a single coating composition is used in the coating step (2) according to this disclosure, i.e., the coating composition has a constant formulation throughout the entire duration of step (2), except that pigments may be added, particularly during the final stage of the coating step (2). In a preferred embodiment, when performing the smoothing step (3), the coating composition used for steps (2) and (3) is the same, except that pigments may be added, particularly during the final stage of the coating step (2) and / or during step (3).

[0171] The temperature of the solvent is typically chosen to allow the crystallizable material to dissolve sufficiently in the sugar coating composition to be sprayed. Therefore, this temperature depends on the nature and amount of the crystallizable substance present in the composition. In the method according to this disclosure, this temperature is typically selected from 20°C to 90°C. It is preferably below 90°C, preferably equal to or below 80°C, preferably equal to or below 70°C, preferably equal to or below 60°C, preferably equal to or below 50°C, preferably equal to or below 40°C, and preferably equal to or below 30°C. It is preferably equal to or above 10°C, preferably equal to or above 15°C, and preferably equal to or above 20°C. The solvent is preferably used at room temperature, typically between 20°C and 25°C.

[0172] Preferably, the temperature of the coating composition is typically selected from 1°C to 90°C. It is preferably below 90°C, preferably equal to or below 80°C, preferably equal to or below 70°C, preferably equal to or below 60°C, preferably equal to or below 50°C, preferably equal to or below 40°C, preferably equal to or below 30°C, and preferably equal to or below 25°C.

[0173] When xylitol is used as a crystallizable material, the temperature of the solvent used is preferably as described previously. However, due to the high enthalpy of solubility of xylitol, the temperature of the coating composition itself will generally be low. Thus, for example, for a coating composition using water at 20°C as a solvent, the temperature of the coating composition will generally be 5°C to 10°C after the xylitol dissolves, and 15°C to 20°C during the coating step (2).

[0174] To apply the coating composition, the number of compressed air nozzles used is typically selected as a function of the size of the coating chamber, based on the manufacturer's recommendations. This number of nozzles is typically 1 to 2 nozzles per 40 cm diameter cross-section of the coating chamber. The number of nozzles ranges, for example, from 1 to 10, or from 1 to 6. Preferably, no other nozzles are used in the method according to this disclosure besides the compressed air nozzles used for applying the coating composition.

[0175] Preferably, the nozzle used has an orifice with a diameter selected from 0.1 mm to 2.8 mm, preferably 0.1 mm to 2.5 mm, preferably 0.1 mm to 2.2 mm, for example 0.3 mm to 2.0 mm, or 0.5 mm to 1.8 mm, or 0.5 mm to 1.5 mm, or 0.5 mm to 1.2 mm, or 0.5 mm to 1.0 mm.

[0176] Preferably, the spraying rate is increased during the sugar coating step (2). In fact, using a lower flow rate at the beginning of the coating method is beneficial for the first stage of crystallization that occurs at the surface of the solid core. The flow rate can then be increased to shorten the coating time. Preferably, the spraying rate is selected from 1 g / min / kg solid core to 20 g / min / kg solid core, preferably 1 g / min / kg solid core to 15 g / min / kg solid core, preferably 2 g / min / kg solid core to 15 g / min / kg solid core, and preferably 2 g / min / kg solid core to 10 g / min / kg solid core.

[0177] For the drying step (2.b), the inlet temperature is preferably below 100°C, preferably equal to or below 80°C, preferably equal to or below 70°C, preferably equal to or below 60°C, and preferably equal to or below 50°C. It is preferably equal to or above 20°C, preferably equal to or above 30°C, and preferably equal to or above 40°C. For example, it is equal to 45°C.

[0178] For the drying step (2.b), the airflow rate generally depends on the size of the coating chamber. It can be selected from 50m³ per 5kg solid core. 3 / h to 8000m 3 / h, for example, 100m 3 / h to 7000m 3 / h, for example, 100m3 / h to 1000m 3 / h. For example, this equals 500m³ per 5kg solid core. 3 / h.

[0179] The discharge of dry air is preferably performed by perforating the rotating drum to draw air from the chamber.

[0180] Preferably, the temperature of the bed of solid core undergoing sugar coating step (2) is equal to or lower than 70°C, preferably equal to or lower than 60°C, preferably equal to or lower than 50°C, and preferably equal to or lower than 40°C. It is preferably equal to or higher than 10°C, preferably equal to or higher than 20°C, and preferably equal to or higher than 30°C. For example, it is between 30°C and 40°C.

[0181] Preferably, before starting the sugar coating step (2), i.e. before starting the spraying, the method according to this disclosure includes the step of heating the bed of the solid core to be sugar coated. The aim is to bring the bed temperature to a target value, which is the temperature of the solid core during sugar coating.

[0182] To keep the bed of solid cores in motion, the rotational speed of the drum is selected based on the size of the chamber and the size of the solid core to be coated. This speed is typically selected from 3 rpm to 30 rpm, preferably 5 rpm to 20 rpm, and more preferably 5 rpm to 15 rpm. When using a drum with a diameter of 48.26 cm, this speed is, for example, equal to 8 rpm.

[0183] The sugar coating step (2) is preferably carried out in conjunction with the spraying and drying of the coating composition.

[0184] However, it is possible to envision introducing dispensing (“pause time”) and spraying steps in the absence of drying, as long as this does not interfere with the desired properties, particularly with regard to the quality of the obtained solid form of the coated sugar and / or the ease of administration of the method.

[0185] Preferably, the sugar coating step (2), which is sprayed without drying, accounts for less than 50%, preferably less than 40%, preferably less than 30%, preferably less than 20%, preferably less than 10%, and preferably less than 5% of the total time of the sugar coating method. More preferably, in the absence of drying, the sugar coating step (2) does not include the spraying stage.

[0186] Preferably, the optional pause time (the time between two spraying stages during which neither spraying nor drying occurs) accounts for less than 50%, preferably less than 40%, preferably less than 30%, preferably less than 20%, preferably less than 10%, and preferably less than 5% of the sugar coating step (2). More preferably, the sugar coating step (2) does not include any pause time.

[0187] Preferably, the mass increase during the sugar coating step (2) is equal to or greater than 0.1% / min, preferably equal to or greater than 0.2% / min. It is generally equal to or less than 1.0% / min, even equal to or less than 0.9% / min, even equal to or less than 0.8% / min, even equal to or less than 0.7% / min, even equal to or less than 0.6% / min. For example, it is equal to 0.3% / min.

[0188] In addition to the sugar coating step (2), the sugar coating method according to this disclosure may also include common steps, provided that these common steps do not interfere with the desired properties, particularly with regard to the quality of the solid form of the obtained sugar coating and / or the ease of administration of the method. These common steps include, for example: film coating step (1), smoothing step (3), polishing step (4), and printing step (5).

[0189] Advantageously, if steps (1), (3) and / or (4) are performed, they are performed in the same equipment as the equipment used for the sugar coating step (2).

[0190] Preferably, especially since the equipment is not required due to the addition of stearate, the method according to this disclosure does not include a smoothing step (3).

[0191] Apparatus for performing the sugar coating method according to this disclosure typically includes a unit for storing the sugar coating composition, the unit including at least one outlet for conveying liquid sugar coating (e.g., by a peristaltic pump) to a device for spraying the liquid sugar coating. The liquid sugar coating is applied by the spraying device to a bed of solid cores contained in a chamber equipped with a rotating drum for positioning the bed of solid cores in motion. The drum is preferably a perforated rotating drum, and the spraying device is preferably a compressed air nozzle. The apparatus also includes an air inlet at the level of the chamber of the drum for drying the liquid sugar coating. The drying air is preferably exhausted by perforating the rotating drum to draw air from the chamber.

[0192] Preferably, the perforated wall region of the rotating cylinder according to this disclosure occupies at least 50%, preferably at least 60%, preferably at least 70%, preferably at least 80%, and preferably at least 90% of the curved surface of the rotating cylinder wall. Most preferably, the entire curved surface of the rotating cylinder wall is perforated.

[0193] Preferably, particularly for reasons of simplicity and / or space requirements, and because the method of the invention allows for perforation, the step of setting the bed of solid cores to be in motion does not include conveying the solid cores along the longitudinal axis. This specifically means that the solid cores that have undergone the sugar coating step (2) are not conveyed from one chamber to another, that is, they are sugar-coated in a single chamber, and / or that the bed of solid cores is not sugar-coated in the longitudinal chamber along which the solid cores are conveyed.

[0194] This disclosure also covers solid forms that are obtained or can be obtained by the sugar coating method according to this disclosure.

[0195] 4. Uses of stearates in improving the surface of solid sugar coatings.

[0196] This disclosure also relates to the use of a stearate (e.g., magnesium stearate) in a sugar coating layer in solid form for improving the surface of the sugar coating layer.

[0197] Preferably, the use includes performing the sugar coating method according to this disclosure. Preferably, the solid form of the sugar coating is as previously described. Preferably, the stearate (e.g., magnesium stearate) is as previously described.

[0198] The term "improved surface" means that a coating layer obtained by coating a sugar coating composition containing stearates has an improved surface compared to a coating layer obtained with the same sugar coating composition without said stearates. The term "improved surface" can, for example, mean improving the color of the coating layer, increasing brightness, increasing opacity, or increasing smoothness (or reducing roughness or wrinkles). Preferably, the method according to this disclosure is used to increase the smoothness (or reduce roughness or wrinkles) of the coating layer. This smoothness, roughness, or wrinkles can be determined by those skilled in the art by measuring the arithmetic mean height (Sa) (in μm), for example using a VHX-7000 microscope (KEYENCE). The Sa value is the extension of the Ra parameter (arithmetic mean height of the line) to the surface. It gives the arithmetic mean (in absolute value) of the height difference of each point relative to the average plane of the surface. 3D reconstruction is performed, and then wrinkles are measured according to the following parameters: Gaussian filter; S filter: 8 μm; L filter: 0.8 μm. Surface roughness is the average of five values.

[0199] This disclosure also relates to a method for improving the surface of a coating layer in solid form, the method comprising including a stearate (e.g., magnesium stearate) in the coating layer.

[0200] Preferably, the method includes performing a sugar coating method according to this disclosure. Preferably, the solid form of the sugar coating is as previously described. Preferably, the stearate (e.g., magnesium stearate) is as previously described.

[0201] In this disclosure, the amounts of ingredients are generally expressed as weight percentages. Unless otherwise stated, these weights are the amount of the ingredient itself, or of the ingredient in powder or oil form. Powdered ingredients may include small amounts of water (also referred to as moisture % or “loss on drying”) and / or small amounts of impurities.

[0202] Conversely, if the quantity is expressed as "dry weight," it refers to the amount of anhydrous components.

[0203] Other features and advantages of the invention will become clear when reading the embodiments given below, which illustrate the invention but are not intended to limit it.

[0204] Example

[0205] 1. The sugar coating composition to be tested

[0206] The following materials are used in the sugar coating composition:

[0207] - Xylitol (XYLISORB) ® 300, ROQUETTE)

[0208] - Polymer binder: Hydroxypropyl hydrolyzed pea starch with a cold water solubility of over 95% (LYCOAT) ® RS720, ROQUETTE

[0209] -Titanium dioxide (TiO2)

[0210] - Magnesium stearate with low specific surface area: specific surface area of ​​4.5 m² 2 / g magnesium stearate LS (ROQUETTE)

[0211] - Magnesium stearate (MgSt) with a moderate specific surface area: 8 m² 2 / g magnesium stearate STD (ROQUETTE)

[0212] - Magnesium stearate with a high specific surface area: 22 m² 2 / g magnesium stearate HS (ROQUETTE)

[0213] The formulations of the tested sugar coating compositions are presented in Table 1.

[0214] [Table 1]

[0215]

[0216] A liquid sugar coating composition was prepared with 60 wt.% solids.

[0217] 2. Sugar coating method

[0218] Based on the coating method parameters described in this article, these sugar-coated formulations are used to coat solid forms.

[0219] The equipment and parameters used for all tests are as follows:

[0220] -Cooking coating type: RAMA COTA FC19

[0221] - Pot diameter: 19''

[0222] - Solid core to be coated: 5kg solid core

[0223] -Number of spray nozzles: 1

[0224] - Spray nozzle type: Schlick 970 / 7-1 S75

[0225] - Hole diameter: 0.8mm

[0226] - Peristaltic pump: Watson Marlow model 323, head 313 DW (3 rollers)

[0227] -Number of baffles: 6

[0228] -Exacanal tube (inner diameter: 4mm, outer diameter: 8mm)

[0229] - Control air pressure: 4 bar

[0230] - Atomization pressure: 1.2 bar

[0231] - Pattern air pressure: 1.2 bar

[0232] -Dry air flow rate: 500m 3 / h

[0233] - Pressure difference in the boiler: below 0

[0234] -Pot rotation speed: 8 rpm

[0235] -Inlet air temperature: 45℃

[0236] - Coating percentage: 30%

[0237] The solid core is made of 74% mannitol. ® 200 SD (ROQUETTE), 25% microcrystalline cellulose (MICROCEL) ®Tablets composed of MC 102 (ROQUETTE) and 1% magnesium stearate (MgStD, ROQUETTE); the percentages are expressed by weight relative to the total weight of the tablets. These tablets were prepared on a FETTE P1000 press to obtain 10mm concave tablets with a weight of 400 mg and a hardness of 185 N.

[0238] The specific method parameters for each experiment are presented in Table 2.

[0239] [Table 2]

[0240]

[0241] 3. Evaluation of the solid form of the sugar coating

[0242] The smoothness of the sugar-coated formulation obtained therefrom was evaluated by measuring the arithmetic mean height (Sa) (in μm) using a VHX-7000 microscope (KEYENCE) using the method previously described in the instruction manual.

[0243] For comparison, the following commercially available solid forms of coated sugar were also evaluated: ADVIL ® (GlaxoSmithKline), Ibuprofen (CVS Health), MENTOS ® (Perfetti Van Melle).

[0244] The results are presented in Figure 1 superior.

[0245] When comparing composition 1 with compositions 2 and 3, it was observed that the addition of magnesium stearate allowed for a reduction in wrinkles in hard-coated tablets containing TiO2. The same observations were made for formulations without TiO2 when comparing formulation 4 with formulations 5-10. By comparing formulation 6 with formulations 9 and 10, it was observed that magnesium stearate with an average specific surface area performed better than magnesium stearate with low or high specific surface areas. Finally, we observed that increasing the amount of magnesium stearate increased the smoothness of the coating. Optimal results were obtained when the amount of magnesium stearate was greater than 4%, for example, 6% to 10%.

[0246] The coating thickness on samples 1, 6, and 7 was also evaluated using scanning electron microscopy (SEM) (FEI QUANTA 200F, TERMOFISHER). The results are presented in... Figure 2 superior.

[0247] The stability of coated tablets of formulation 6 was evaluated by placing them in a 45°C oven for 9 weeks. Then, color measurements were performed on 10 coated tablets using our KONICA MINOLTA CM-5 with the following settings: standard irradiation body: D65; viewing angle: 10°; orifice disk: 3mm; SCI mode (a measurement mode including specular component included for evaluating object color, independent of object surface condition); UV=100%; CIELAB color space (L... a b CIE 1976); Whiteness Index: WI (E313-96): Scale -100 to 100.

[0248] Brightness L Takes a value between 0 (black) and 100 (reference white). Parameter a This represents the value along the green to red axis. Parameter b This represents the values ​​on the blue to yellow axis.

[0249] The results are shown in Table 3.

[0250] [Table 3]

[0251]

[0252] The color difference was ΔE = 0.4, while the visible color difference should be greater than 1.5. Therefore, these results demonstrate the stability of the coated formulation according to this disclosure, which showed no discoloration or color change after being kept at 45°C for 9 weeks.

[0253] 4. Improved sugar coating formula

[0254] The inventors then discovered that, due to the lack of stability of the liquid coating formulation during the coating process, further formulation improvements were still needed. Indeed, it was observed that magnesium stearate, due to its low density, tends to rise to the surface (a phenomenon known as "creaming").

[0255] One hypothesis is that altering viscosity may have a positive impact on formulation stability. Therefore, the viscosity, processability, and turbidity of various formulations comprising different amounts of different polymer binders were tested. The tested polymer binders exhibit the characteristics shown in Table 4.

[0256] [Table 4]

[0257]

[0258] The formulations of the tested sugar coating compositions are shown in Table 5.

[0259] [Table 5] - Coated Formulations Tested

[0260]

[0261] RT: Room temperature (25℃)

[0262] The powder is manually mixed and then introduced into water (60% or 70% solids) at room temperature or 70°C. The purpose of performing the test with a higher solids content of 70% is to facilitate coating drying by reducing the amount of water to be evaporated. Therefore, the solution temperature is raised to 70°C to ensure complete dissolution of the xylitol.

[0263] The blend was then dispersed at 600 rpm using a high-speed stirrer (IKA stirrer) while at 25°C for one hour. Ease of dispersion and presence or absence of foaming were recorded. The blend was then mixed with magnetic stirring (600 rpm) while at 25°C for one hour. The evolution of the suspension and the presence of stratification were observed.

[0264] After stirring for 1 hour, the Brookfield viscosity was measured using a DV-I+ Brookfield viscometer, with rotor 2 or 3 used depending on the formulation, at a rotation speed of 100 rpm.

[0265] For all formulations, the solution after high-speed stirring has a homogeneous appearance. For all formulations, the solution after magnetic stirring has a homogeneous appearance.

[0266] Viscosity results are presented in Figure 3 middle.

[0267] A more viscous formulation (containing 6 wt.% hydroxypropylated hydrolyzed starch and prepared at 60% solids under RT) was used for coating tests, but coating was not possible due to its high viscosity.

[0268] CLEARGUM ® CO 01 vs CLEARGUM ® CO 03 performed better because the latter could not provide sufficient viscosity to the formulation; the polymer binder with the best influence on viscosity was LYCOAT. ® RS720.

[0269] Then, use TURBISCAN ™ The formulation was analyzed to observe whether a phase shift occurred.

[0270] Regardless of the polymer binder used, the suspension appears relatively easy to prepare. The one-hour mixing time is primarily determined by the initial temperature drop. No foaming occurred. Stop stirring and use TURBISCAN as recommended by the manufacturer. ™The equipment measures the layering speed. Results appear in... Figure 4 middle.

[0271] A decrease in the rate of layering and an increase in viscosity were observed.

[0272] Then, as described in Example 2, a solid was used consisting of 90 wt.% xylitol, 6 wt.% magnesium stearate (STD), and 4 wt.% lycoat. ® The coating formulation of RS720 was used to perform the coating test. A suspension was prepared using high-speed stirring (IKA) for 60 minutes, and then stirred with a magnetic stirrer throughout the coating process. As the suspension concentration in the beaker decreased, some magnesium stearate adhered to the beaker surface and formed a collar. This phenomenon did not occur when using a high-speed stirrer (IKA stirrer) at 1000 rpm. The amount of magnesium stearate on the beaker surface remained negligible. This phenomenon was more pronounced in the case of the tested octenyl succinate starch than in the case of the tested hydroxypropylated starch. Therefore, high-speed stirring is preferred during coating.

[0273] Furthermore, the resulting coated tablets are not easily broken.

[0274] The best formulation among all tested products was a 4% (by weight relative to the total solids) starch with the highest viscosity (hydroxypropylated hydrolyzed pea starch). The coating formulation obtained from it was stable under both test conditions (60% solids, RT and 70% solids, 70°C) and was easy to handle.

Claims

1. A solid form of a coated sugar composition comprising a crystallizable material and a stearate, said crystallizable material being selected from sugars, sugar alcohols, or any mixture thereof.

2. The solid form according to claim 1, wherein the stearate is an alkali metal salt or an alkaline earth metal salt of stearic acid or a mixture thereof.

3. The solid form according to any one of claims 1 or 2, wherein the stearate is selected from magnesium stearate, calcium stearate, sodium stearate or any mixture thereof, preferably selected from magnesium stearate, calcium stearate or any mixture thereof.

4. The solid form according to claim 3, wherein the stearate is magnesium stearate.

5. The solid form according to any one of claims 1 to 4, wherein the sugar coating composition further comprises a polymeric binder.

6. A sugar coating composition, said sugar coating composition comprising: (a) A solid, said solid being composed of the following: (a.1) 80.0% to 95.0%, preferably 85.0% to 95.0%, preferably 86.0% to 94.0%, preferably 87.0% to 93.0%, preferably 88.0% to 92.0%, preferably 89.0% to 91.0%, for example 85% to 90%, or 86% to 90%, or 90% of a crystallizable material selected from sugars, sugar alcohols or any mixture thereof; (a.2) 4.0% to 19.0%, preferably 4.0% to 18.0%, preferably 4.0% to 17.0%, preferably 4.0% to 16.0%, preferably 4.0% to 15.0%, preferably 4.0% to 14.0%, preferably 4.0% to 13.0%, preferably 4.0% to 12.0%, preferably 4.0% to 11.0%, preferably 4.0% to 10.0%, for example 4.0%, or 6.0%, or 8.0%, or 10.0% of stearates; (a.3) 1.0% to 10.0%, preferably 1.0% to 9.0%, preferably 1.0% to 8.0%, preferably 1.0% to 7.0%, preferably 1.0% to 6.0%, preferably 1.0% to 5.0%, preferably 1.0% to 4.0%, preferably 2.0% to 4.0%, preferably 3.0% to 4.0%, preferably 4% of a polymer binder; (a.4) Optionally no more than 3.0%, preferably no more than 2.0%, preferably no more than 1.5%, preferably no more than 0.010%, preferably no more than 0.005% of TiO2, preferably no TiO2; (a.5) optionally up to 1.0%, preferably up to 0.5%, preferably up to 0.10%, preferably up to 0.05%, preferably up to 0.010%, preferably up to 0.005% of pigment; (a.6) Optionally no more than 3.0%, preferably no more than 2.0%, preferably no more than 1.0%, preferably no more than 0.5%, preferably no more than 0.10%, preferably no more than 0.005% of other components, and even more preferably no other components; The percentages from (a.1) to (a.6) are expressed as weight relative to the total weight of the solids, and their sum equals 100%; and (b) Optionally a solvent, preferably water.

7. The sugar coating composition according to claim 6, wherein the stearate is an alkali metal salt or an alkaline earth metal salt of stearic acid or a mixture thereof.

8. The sugar coating composition according to claim 7, wherein the stearate is selected from magnesium stearate, calcium stearate, sodium stearate or any mixture thereof, preferably selected from magnesium stearate, calcium stearate or any mixture thereof.

9. The sugar coating composition according to claim 8, wherein the stearate is magnesium stearate.

10. A sugar coating method, the sugar coating method comprising coating a solid core with a sugar coating composition according to any one of claims 1 to 9.

11. Use of stearates in a sugar coating layer in solid form for improving the surface of the sugar coating layer.

12. The use according to claim 11, wherein the use is for improving the color of the sugar coating layer, and / or increasing brightness, and / or increasing opacity, and / or increasing smoothness, and / or reducing roughness, and / or reducing wrinkles.

13. The use according to any one of claims 11 or 12, wherein the use is for increasing the smoothness of the sugar coating layer and / or reducing the roughness and / or reducing the wrinkles.

14. A sugar-coated solid form obtainable by the method according to claim 10.

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