EP3641570A1

EP3641570A1 - Sugar coating method and sugar coated solid forms with irregular shapes

Info

Publication number: EP3641570A1
Application number: EP18730375.5A
Authority: EP
Inventors: Philippe Lefevre; Grégory Le Bihan; Sébastien CROQUET
Original assignee: Roquette Freres SA
Current assignee: Roquette Freres SA
Priority date: 2017-06-19
Filing date: 2018-06-18
Publication date: 2020-04-29
Also published as: CN116746693A; FR3067567B1; RU2021137304A; CN110913707B; JP2023093686A; FR3067567A1; RU2020101488A; RU2020101488A3; US20200214315A1; WO2018234248A1; CN110913707A; JP2020524003A; CA3067114A1

Abstract

The present invention relates to new sugar-coated solid forms with irregular shapes, and to a sugar coating method which is particularly useful for the preparation of same.

Description

NEW DRAGEIFICATION PROCESS AND DRAGED SOLID FORMS HAVING IRREGULAR SHAPES

The present invention relates to new sugar-coated solid forms having irregular shapes, as well as a coating process particularly useful for their preparation.

BACKGROUND OF THE INVENTION Sugar coating is an operation used in particular in confectionery or in pharmacy, which consists in creating a more or less hard crystallized coating ("hard" or "soft coating") on the surface of products. solid or powdery, to protect them for various reasons or to make them attractive visually or tastefully. The coating of the solid form (core) is carried out in a vat rotating about its axis and called a dredger, inside which there is a plurality of nuclei forming a mass in motion, on the surface of which is distributed to the liquid state the constitutive material of the future envelope ("liquid or syrup coating"). The hard and crystalline coating is obtained by applying this liquid and evaporation of the water brought by it.

The coating syrup is mainly composed of one or more crystallizable materials, and also conventionally contains binding agents such as gum arabic or gelatin, dyes, opacifiers such as TiO ₂ , mineral fillers such as talc, silica, calcium carbonate, intense sweeteners, flavors, vitamins, active ingredients.

The coating is a relatively laborious process, including a large number of successive steps. Each of these steps, also called "coating cycles", typically includes an application phase, generally by spraying a coating syrup on the cores, a rotary phase of distribution of said syrup on the cores also called pause time, and a drying phase of each new layer of syrup made by blowing hot and dry air.

The drageification makes it possible to obtain solid forms having a particularly attractive appearance, but lacks flexibility as to its implementation and as to the visuals that can be obtained. In particular, and this is the subject of the present invention, it is not possible in drageification to obtain solid shapes having complex irregular shapes, for example relief impressions or ridges. sugar-coated

FIRE I LLE OF REM PLACEM ENT (RULE 26) solid forms having such irregularities, the latter are masked after coating: the coating liquid fills the grooves and cavities formed by the printing in relief ("logo in-filling"), and enlarges the edges which then round off. It is also not possible to maintain the asymmetry that the nuclei eventually present, as for example when these nuclei are seeds. The solid forms obtained by coating thus conventionally have a generally coarse and rounded shape, not very faithful to that of the starting nuclei.

Therefore, for example in pharmacy, it is generally preferred the film lamination of tablets ("film coati ng"). In this process, not a syrup, but a film-forming composition, generally based on cellulose derivatives such as hydroxypropylmethylcellulose (HPMC), or more recently, modified starches. This film-forming composition forms a thin film on the surface of the tablets and advantageously makes it possible to preserve the impressions in relief present on the surface of the tablets, such as logos, active molecule names or active dosages.

Although this method allows the preservation of precise forms, it nevertheless leads to tablets having a much less attractive appearance than the coated forms. In addition, the film coating produces an amorphous coating, which is much less stable than the crystallized coating resulting from the coating.

Thus, there is currently no method for producing solid forms coated with original shapes. Also, when the manufacturer wishes to reveal logos or other patterns on the surface of the solid forms coated, it does so through the application of a colored composition on the surface of the coated forms.

An approach to this problem is described in US 2008/0026131 A1. This document discloses a coating process for preserving the irregular shape of chocolates. However, this method only allows to keep coarse and round general shapes, and not complex irregular shapes. The teaching of US 2008/0026131 A1 does not allow the preparation of solid forms coated with complex irregular shapes such as ridges or relief printing. This process, particularly long and laborious, comprises multiple cycles of coating (syrup application / distribution / drying).

FIRE I LLE OF REM PLACEM ENT (RULE 26) Objectives of the invention

The object of the present invention is thus to provide solid, sugar-coated shapes having complex irregular shapes, as well as a process making it possible to achieve this.

The invention also aims to provide a particularly simple and flexible method for the coating of solid forms.

Presentation of the invention

The Applicant has been able to produce solid, sugar-coated shapes in which irregular shapes such as relief impressions, ridges, and asymmetrical shapes are preserved after coating.

The Applicant has achieved this through the implementation of at least one new coating process, characterized in that it comprises:

^■ a step (a) spraying a coating liquid comprising a composition of crystallizable material on a bed of moving cores, said cores being placed in a room equipped with a perforated rotating drum, and said spraying being achieved by means at least one compressed air nozzle;

At least one step (b) concomitant with step (a), of drying said pulverized coating liquid;

^■ a step (c) collecting the sugar-coated solid forms thus obtained.

The process of the invention applies to various solid forms (tablets, chewing gums, etc.) and offers a multitude of possibilities for manufacturers, and in particular that of being able to now offer the consumer new visuals of solid, sugar-coated forms. .

In this process, drying and spraying are performed concomitantly. Surprisingly, despite the continuous wetting of the nuclei, the nuclei do not erode, and the irregular shapes are preserved.

This is particularly surprising since it was previously accepted that the spraying must necessarily be stopped for a significant time during the process: otherwise, the cores are perpetually moistened, so that the substance used for the coating can not crystallize, that the solid form is eroded and degraded, and that the nuclei adhere to each other (phenomenon of collage). However, this phenomenon is not observed with the method of the invention, even on very hygroscopic nuclei, that is to say eager for water.

FIRE I LLE OF REM PLACEM ENT (RULE 26) Also, and contrary to conventional coating, the method of the invention does not require that the coating liquid has a high content of dry materials (at least 70% for a conventional coating with maltitol). This also goes against the general knowledge of the trade, for the same reasons as those mentioned in the previous paragraph (significant humidification of the cores).

The fact that low levels of solids can be used has a number of advantages. Firstly, it gives the possibility of using coating liquids at low temperatures, and thus introducing thermolabile ingredients in these liquids or in the cores compositions to be coated. Indeed, if high temperatures are conventionally used in coating, it is to allow the coating solution to have a high content of crystallizable materials in solution. This high dry matter is not necessary in the process of the invention, the temperature of the coating liquid can be lowered.

Secondly, it also allows for drageification with crystallizable materials having low solubility in water. A good illustration of this advantage is presented in the Examples in point 1. (Tests "Man-IN1 to -IN5"), where mannitol was used for the coating. This coating does not require the addition of large amounts of binders, unlike the processes of the prior art. In other words, a coating properly speaking is operated here, since the crystallizable materials can be largely in the majority. Thus, for the first time, the process of the invention has made it possible to obtain solid, sugar-coated forms whose coating layer has high levels of mannitol, without this requiring the addition of excessive amounts of binders. such as gum arabic or polyvinyl alcohol. The Man-IN5 test even shows that it is possible to do without binders.

The process developed by the Applicant has further advantages that make it also useful for the coating of solid forms that do not have particularly complex irregular shapes. In particular, the method of the invention is much more flexible than conventional methods of coating, and can be particularly simple in its implementation.

FIRE I LLE OF REM PLACEM ENT (RULE 26) In addition, this process is applicable to different crystallizable materials, as demonstrated in point 1. hereinafter in the Examples. Sucrose, xylitol, erythritol and mannitol in particular give very satisfactory results. Finally, the method of the invention does not necessarily require large modifications of its parameters during its execution (drying temperature, formulation of the coating liquid, etc.), and can be implemented in a relatively simple and compact equipment. None of the documents of the prior art discloses or suggests such a method. For example the document US 2008/0026131 A1 mentioned above never simultaneously performs drying and spraying.

Summary of the invention

The subject of the present invention is a solid coated form having at least one raised impression, and / or at least one edge, and / or in that it is asymmetrical, the coating layer of said asymmetrical sugar-coated solid form. faithfully marrying the shape of the nucleus from which it comes. The present invention also relates to a process which is particularly useful for the preparation of sugar-coated solid forms having complex irregular shapes, comprising:

^■ at least one step (b) concurrent with step (a), drying said sprayed coating liquid;

^■ a step (c) collecting the sugar-coated solid forms thus obtained.

The present invention also relates to a coated solid form comprising at least one coating layer comprising:

crystallizable materials consisting of at least 50% by dry weight of mannitol; and, optionally, binders, the ratio by dry weight crystallizable materials / binders being greater than 15.

FIRE I LLE OF REM PLACEM ENT (RULE 26) Detailed description of the invention

The present invention thus has for its first object solid forms coated with at least one embossed impression, and / or at least one edge, and / or in that it is asymmetrical, the coating layer of said asymmetrical sugar-coated solid form marrying faithfully the shape of the nucleus from which it comes.

The solid forms of the invention have particular irregular shapes, i.e., relief prints, edges, or asymmetries. Examples of relief printing include patterns (such as logos) or inscriptions (brand names, molecule names, assays, etc.). Relief impressions are present on the surface of solid forms, while edges are more involved in defining the general shape of the sugar-coated solid shape. These solid forms coated with sugar are particularly characterized in that the nuclei to be coated from which they are derived themselves have these irregular shapes. It is understood that these irregular shapes of the initial nuclei are preserved after coating. This means in particular that the inscriptions are legible, and the reasons identifiable. These irregular shapes also cover asymmetrical shapes, that is to say not having an axis of symmetry. It is understood here that the coating layer of asymmetrical sugar-coated solid forms closely follows the shape of the cores from which they are derived.

Preferably, this solid form of the invention has at least one raised impression and / or at least one edge, more preferably at least one raised impression.

The subject of the present invention is also a solid coated form, having the irregular shapes as described above or not, characterized in that it comprises at least one coating layer comprising:

Preferably, the crystallizable materials of the coating layer of this coated solid form consist of at least 60% by dry weight of mannitol, preferably at least 70%, preferably at least 80%, preferably at least 90%, or even only mannitol.

FIRE I LLE OF REM PLACEM ENT (RULE 26) More preferably, in the coating layer of these coated sugar-coated solid forms, the ratio by dry weight crystallizable materials / binders is greater than 20, or even greater than 30, or even greater than 40. The coating layer may also advantageously be free of binders .

In drageification, the term "solid form" conventionally means any solid presentation of sugar-coated substances ("solid coated form") or capable of undergoing a coating operation ("core"). Typical examples are tablets, hard capsules, soft capsules, pellets, microspheres, granules, seeds, biscuits, breakfast cereals, confectionery such as chewing gums, cooked sugars. , chewables, jelly candies, chocolates, fruits and vegetables, or products in the form of powders and / or crystals. These solid forms can be for example food, pharmaceutical, veterinary, cosmetic. They can be intended for the human, adult or child, or the animal. They may also be products with a chemical or agrochemical purpose, although solid forms intended to be ingested in the context of the present invention are preferred. Preferably, these solid forms are chosen from tablets and chewing gums.

Preferably, the solid coated forms of the invention comprise at least one coating layer whose composition is identical to that of the coating liquid used in the coating process of the invention; it being understood that only what constitutes the dry matter of the coating liquid is considered here.

Preferably, the solid coated forms of the invention have a percentage of coating greater than 1%. This percentage of coating, otherwise known as "mass gain", is conventionally determined as follows:

(Weight of coated solid forms - Weight of cores) / Weight of cores x 100.

This percentage of coating is preferably greater than 3%, preferably greater than 5%, preferably greater than 7%, preferably greater than 10%, for example at least 15%, and even at least 20%. %.

The subject of the invention is also a coating method which is particularly useful for the preparation of coated solid forms according to the invention, comprising:

A step (a) of spraying a coating liquid comprising a composition of crystallizable materials on a bed of moving cores, said cores being placed in a chamber equipped with a perforated rotary drum, and said spraying being ensured by means of at least one compressed air nozzle;

FIRE I LLE OF REM PLACEM ENT (RULE 26) ^■ at least one step (b) concurrent with step (a), drying said sprayed coating liquid;

^■ a step (c) collecting the sugar-coated solid forms thus obtained. The equipment used to implement the process of the invention typically comprises a storage unit for the coating liquid, comprising at least one outlet for transporting the coating liquid to a device for spraying the coating liquid. The coating liquid is applied through the spraying device on a bed of cores contained in the chamber, said chamber being provided with a rotating drum for moving said bed of cores. More specifically, the drum is a perforated rotary drum, and the selected spray device comprises at least one compressed air nozzle. The equipment further comprises an air inlet at the drum chamber for drying the coating liquid. The exit of the drying air is effected in particular through the perforations of the rotary drum, in particular by suction of the air from the chamber.

The elements of the equipment useful to the invention are commercially available, and their arrangement does not represent any particular difficulties for a person skilled in the art. The coating liquid useful in the invention comprises a composition of crystallizable materials.

The term "composition of crystallizable materials" conventionally means a composition consisting of substances capable of crystallizing by evaporation of the solvent in which they are dissolved.

Preferably, the composition of crystallizable materials of the coating liquid useful in the invention comprises at least one substance chosen from sugars and polyols, preferably chosen from monomers and dimers.

Advantageously, the sugars and polyols represent at least 50%, preferably at least 70%, and even more preferably at least 90% by dry weight of the composition of crystallizable materials of the coating liquid. Most preferably, the composition of crystallizable materials of the coating liquid consists entirely of substances selected from sugars and polyols.

In the present invention, it is understood that when referring to a dry mass of compounds, this mass includes any impurities.

FIRE I LLE OF REM PLACEM ENT (RULE 26) Preferably, these sugars and polyols are selected from xylitol, sucrose, erythritol, mannitol, dextrose, isomalt, maltitol or possibly a combination thereof. Most preferably, these sugars and polyols are selected from sucrose, mannitol, xylitol, erythritol, or possibly a combination thereof, more preferably from sucrose, mannitol, xylitol, or possibly a combination of them.

Preferably, the composition of crystallizable materials of the coating liquid consists entirely of a single substance. Thus, for example and advantageously, the crystallizable material composition useful for the invention is xylitol, or sucrose, or erythritol, or mannitol, or dextrose, or isomalt, or maltitol.

The concentration of crystallizable materials of the coating liquid is chosen so that the crystallizable materials are solubilized in said coating liquid.

Typically, especially when the coating liquid is an aqueous liquid, the coating liquid of the invention has a concentration of crystallizable materials of less than 90%, this percentage corresponding to the dry weight of crystallizable materials of the coating liquid relative to the weight total of said coating liquid. Preferably, this concentration is less than or equal to 70%, preferably less than or equal to 60%, preferably less than 60%, even less than or equal to 55%, even less than or equal to 50%, or even less than or equal to 45%, even less than or equal to 40%, even less than or equal to 35%, even less than or equal to 30%, even less than or equal to 25%, or even equal to 20%. This concentration is generally greater than 10%, or even at least 15%, or even at least 20%.

The maximum concentration of crystallizable material naturally depends on the nature of these crystallizable materials, as well as the temperature of the coating liquid. For xylitol, sucrose, erythritol, mannitol, dextrose, isomalt and maltitol, reference may be made, for example, to FIG. 6 which shows the maximum concentrations of these crystallizable materials in water according to the temperature of the liquid. For example, the concentration of crystallizable materials of a 20 * Ό coating liquid is preferably less than or equal to 67% when the composition of crystallizable materials is sucrose, less than or equal to 15% when mannitol, less than or equal to 61% in the case of maltitol, less than or equal to 63% in the case of xylitol, less than or equal to 25% in the case of isomalt, less than or equal to 27% in the case of erythritol, less than or equal to 48% in the case of dextrose.

FIRE I LLE OF REM PLACEM ENT (RULE 26) Generally, the coating liquid of the invention comprises other substances than crystallizable materials, as long as it does not contravene the properties sought in the present invention, in particular as regards the quality of the obtained sugar-coated solid forms and / or the workability of the process . Such other compounds are for example:

binders, such as gum arabic, polyvinyl alcohol;

coloring substances such as pigments, opacifying agents such as, for example, titanium dioxide;

flavors, sweeteners;

- assets, of interest for example pharmaceutical, nutritive, nutraceutical, or phytosanitary.

Preferably, the coating liquid of the invention has a solids content by weight of less than 90%, preferably less than 85%, preferably less than 80%, preferably less than 75%, preferably less than or equal to at 70%, preferably less than or equal to 60%, preferably less than 60%, even less than or equal to 55%, even less than or equal to 50%, even less than or equal to 45%, even less than or equal to 40% %, even less than or equal to 35%, even less than or equal to 30%, even less than or equal to 25%, or even equal to 20%. This dry matter is generally greater than 10%, preferably at least 15%, more preferably at least 20%.

Preferably, the dry matter of the coating liquid of the invention thus consists of:

50.0 to 100.0% by dry weight of crystallizable materials, especially as defined above;

from 0.0 to 50.0% by dry weight of other ingredients, especially as defined above; the sum of these percentages being equal to 100.0%.

Preferably, the dry matter of the coating liquid of the invention comprises an amount of at least 60.0% by dry weight of crystallizable materials, preferably at least 70.0%, preferably at least 80% by weight. , 0%, preferably at least 90.0%, or even at least 94.0%, or even at least 95.0%, or even at least 96.0%.

Generally, the dry matter of the coating liquid of the invention comprises less than 5.0% by dry weight of pigments and / or dyes, preferably less than 4.0%, preferably less than 3.0%.

FIRE I LLE OF REM PLACEM ENT (RULE 26) Generally, the dry matter of the coating liquid of the invention comprises an amount of less than 5.0% by dry weight of opacifying agents, preferably less than 4.0%, preferably less than 3.0%, preferably less than 3.0%, preferably less than 2.0%.

Generally, the dry matter of the coating liquid of the invention comprises an amount of less than 15.0% by dry weight of binder, preferably less than 10.0%, or even less than 8.0%, or even less than 5, 0%. The coating liquid used in accordance with the invention is typically polar, and preferably comprises water as the majority solvent, most preferably as sole solvent.

In an advantageous embodiment, for reasons of simplicity and since this is possible, the coating process according to the invention uses a single coating liquid, that is to say that the coating liquid has a formulation constant throughout the duration of the coating.

The temperature of the coating liquid is typically chosen so that the crystallizable materials are well solubilized in said coating liquid to be sprayed. This temperature is also a function of the amount of crystallizable materials present in the liquid. In the process of the invention, this temperature is typically selected in a range of from 20 to 90 * Ό. Preferably, this temperature is less than 85 ° C., preferably less than δΟΌ, preferably less than 75 ° C., preferably less than 70 ° C., or even lower than 65 ° C., or even lower than 60 ° C., or even lower. at 55 ° C., or even below 50 ° C., or even below 45 ° C., or even below 40 ° C., or even below 35 ° C., or even below 30 ° C. This temperature is usually at least 15 * Ό, or even at least 20 * Ό. It corresponds for example to the ambient temperature, which typically varies from 20 to 25 ^<0 .

In an advantageous embodiment, the coating liquid is stored in a single envelope storage unit, and / or the equipment that is useful for the process of the invention is free of a device for heating the coating liquid. Indeed, the method of the invention does not necessarily require the use of high temperatures of coating liquids, these devices are not mandatory in the method of the invention.

For the spraying of the coating liquid, the number of compressed air nozzles used is conventionally chosen according to the dimensions of the chamber of

FIRE I LLE OF REM PLACEM ENT (RULE 26) sugar coating, according to the manufacturer's recommendations. This number of nozzles is typically 1 to 2 nozzle (s) for each 40 cm diameter portion of the coating chamber. This number of nozzles varies, for example, from 1 to 10, for example from 1 to 6. Preferably, for spraying, the method of the invention uses only compressed air nozzles.

Preferably, the nozzles used in accordance with the invention have an orifice having a diameter selected in a range from 0.1 to 2.8 mm, preferably from 0.1 to 2.5 mm, preferably from 0.1 to 2.5 mm. at 2.2 mm, for example from 0.3 to 2.0 mm, or from 0.5 to 1.8 mm or from 0.5 to 1.5 mm, or from 0.5 to 1.2 mm, or from 0.5 to 1.0 mm.

Preferably, the spray rates are selected in a range of from 0.5 to 20.0, preferably from 1.0 to 20.0, preferably from 2.0 to 20.0, for example 2.0. at 15.0, or even 2.0 at 10.0 g / min / kg of nuclei.

In an advantageous embodiment, the flow rate chosen for the spraying is increased during the coating. In particular, the inventors have found that for certain crystallizable materials, the use of low flow rates at the beginning of coating makes it possible to favor the first phase of crystallization which takes place on the surface of the cores. The flow can then be increased to accelerate the coating.

For spraying, the atomizing and crushing pressure is adjusted according to the flow rate and orifice of the nozzle, and according to the manufacturer's recommendations. These atomization and crushing pressures are typically chosen in a range from 0.5 to 4.0 bar, preferably from 0.5 to 3.5 bar, for example from 0.7 to 2.5 bar. for the atomization pressure, and / or 0.7 to 3.5 bar for the crushing pressure.

In the present invention, the coating liquid is sprayed onto a moving bed of cores by means of a rotating drum.

The nature of these nuclei is preferably as defined before for solid forms; it is for example tablets or chewing gums. These cores can be completely bare, or be coated with one or more layers, for example scrubbing, film-coating or even coating, said layers being preferably obtained in the same equipment as that used for the coating process of the invention.

FIRE I LLE OF REM PLACEM ENT (RULE 26) For the setting in motion of the bed of cores, the speed of rotation of the drum is chosen according to the dimensions of the chamber and the size of the cores to be coated. It is generally chosen in a range from 3 to 30 rpm, for example in a range from 10 to 20 rpm.

In an advantageous embodiment, in particular for the sake of simplicity and / or bulk, and because the method of the invention allows it, the movement of the bed of cores excludes the transport of said cores along a longitudinal axis. . This means in particular that the cores being coated are not transported from one chamber to another, that is to say they are coated in a single chamber, and / or that the bed of cores is not coated in a longitudinal chamber along which they are transported.

For drying, the temperature chosen for the drying air is preferably less than 10ΟΌ, preferably less than or equal to 80%, preferably less than or equal to 75%, preferably less than or equal to 70%, or even less than or equal to 65 * Ό, or even less than or equal to 60 * Ό, or even less than or equal to 55 * Ό, or even less than or equal to 50 ^, or even less than or equal to 45 * Ό, or even less than or equal to 40 * Ό, or even less than or equal to 35 ° C, or even less than or equal to 30 ^, or even less than or equal to 25 * Ό. This drying temperature is generally at least 15%, preferably at least 20%.

For drying, the flow rate can be chosen in a range from 50 to 8000 m ³ / h, for example in a range from 100 to 7000 m ³ / h, for example from 100 to 1000 m ³ / h. The exit of the drying air is advantageously effected by suction of air by means of the perforations of the perforated rotary drum.

Preferably, the perforated wall area of the rotary drum useful for the invention preferably represents at least 50% of the surface of said drum wall, preferably at least 60%, preferably at least 70%, preferably at least 80% preferably at least 90%. Most preferably the wall of the drum is perforated over its entire surface.

Preferably, the temperature of the bed of nuclei being coated is at most 70%, preferably at most 60%, preferably at most 55%, preferably at most 50%, preferably at most more than 45 * Ό, not more than 40 * Ό, not more than 35 ° C or more than 30 * Ό or more than 25 * Ό. This temperature of the bed of cores being coated is generally at least 10 * Ό, or even at least 15 * Ό.

FIRE I LLE OF REM PLACEM ENT (RULE 26) Preferably, before the beginning of the coating, that is to say before the spraying starts, the method of the invention comprises a step of heating the core bed to be coated. This step aims in particular to bring the core bed to a target temperature. The coating process of the invention concomitantly performs spraying and drying of the spraying liquid.

However, it is conceivable to introduce steps of distribution ("pause time") and spraying in the absence of drying, as long as it does not contravene the properties sought in the present invention, particularly concerning the quality of the sugar-coated solid forms. obtained and / or the maneuverability of the process.

Preferably, the coating process phases during which the spraying is not carried out concomitantly with the drying process represent less than 50% of the coating process time, preferably less than 40%, preferably less than 30%, preferably less than 20%, preferably less than 10%, preferably less than 5%. Most preferably, the coating does not include a spray phase in the absence of drying. Preferably, the possible pause times (time between two spraying phases during which there is neither spraying nor drying) represent less than 50% of the coating process time, preferably less than 40%, preferably less 30%, preferably less than 20%, preferably less than 10%, preferably less than 5%. Most preferably, the coating does not include pause time.

The coated solid forms obtained by the process of the invention preferably have a percentage of coating greater than 1%, preferably greater than 3%, preferably greater than 5%, preferably greater than 7%, preferably greater than 10%, for example at least 15%, or even at least 20%.

Preferably, this percentage of coating is, per unit of time, at least 0.05% per minute, preferably at least 0.10% per minute, preferably at least 0.13% per minute. or at least 0.15% per minute, or even at least 0.20% per minute, or even at least 0.30% per minute.

The method of the invention may further comprise other usual steps than those aimed at coating the solid forms, as long as it does not contravene the properties sought in the present invention, especially as regards the quality of the sugar-coated solid forms.

FIRE I LLE OF REM PLACEM ENT (RULE 26) obtained and / or the maneuverability of the process. Examples of other steps include, for example, guming, smoothing, polishing, and coloring. Advantageously, if such steps are performed, they are performed in the same equipment as that used in the coating process of the invention. It is understood that some of these steps, such as scrubbing or staining for example, can sometimes be likened to steps of coating, if the composition used comprises such a quantity of crystallizable materials that there is actually forming a layer crystallized substances, in particular sugars and / or polyols. Regarding these other usual steps, it is interesting to note that the coating made according to the method of the invention already provides a good level of smoothing of solid forms. The coloration may also be carried out directly by adding coloring agents in the coating liquid. The method of the invention may also comprise a priming step. This priming step consists in applying, one or more times, a pulverulent composition to the bed of cores to be coated, or being coated, preferably during coating. This powdery composition typically comprises crystalline materials. These crystalline materials are typically of the same nature as the crystallizable materials of the coating liquid, but may be different. The amount of powder composition applied is typically less than 10% by weight based on the weight of tablets, preferably less than 5%.

Preferably, when dextrose, isomalt, maltitol or a combination thereof are used, the method comprises an additional priming step. Preferably, when sucrose, xylitol, mannitol, erythritol or a combination thereof are used, the method excludes this priming step.

The equipment useful to the invention may comprise other elements conventionally used in coating, as long as this does not contravene the properties sought in the present invention, in particular as regards the quality of the obtained sugar-coated solid forms and / or the workability of the process.

In this respect, it is interesting to note that the prior art sometimes mentions the use of breakwaters, which are intended to avoid the appearance of collages during coating. Such breakwaters are not necessary in the process of the invention. Thus preferably, and because it is advantageously possible in the context of the method of the invention, the chamber of the drum used in accordance with the invention is free of breaker clods.

FIRE I LLE OF REM PLACEM ENT (RULE 26) The invention will be better understood with the aid of the examples which follow, which are intended to be illustrative and not limiting. Examples

1. Draying tests according to the invention

1 .1. Equipment used

Equipment with the following characteristics has been used:

- perforated rotary drum: diameter 30.48 cm, volume 2L;

Anti-slip bars x6;

1 compressed air atomization nozzle (Schlick 970 / 7-1 S75); orifice diameter 0.8 mm; Peristaltic pump (Watson Marlow model 323); head 3 rollers (313 DW);

Tube: internal diameter 2 mm: outer diameter 6 mm.

1 .2. Draqification liquids

The coating liquids tested had the following formulations (%:

All these coating liquids were contained in a single envelope storage tank, and at room temperature (20-25 * Ό). 1 .3. stones

The following lots of cores were used as a substrate for coating:

FIRE I LLE OF REM PLACEM ENT (RULE 26) 1 .4. Processes and Results

The conditions common to all the tests were as follows: Operating pressure 4 bars; Atomization and crushing pressure of 1, 0 or 1, 3 bars (chosen depending on the viscosity of the solution, as recommended by the manufacturer); Differential pressure -0.25 mbar; Drum rotation speed 18 rpm; Airflow drying 100 m ³ / h.

Before the start of spraying, the tablet bed was heated for 2 minutes in order to reach the desired temperature for the bed of cores. Spraying and drying were then carried out concomitantly throughout the process (no break time). At the end of coating, the spraying was stopped, and the solid forms dried for another 2 minutes.

The following tables show the results obtained as well as the process characteristics specific to each test.

SUBSTITUTE SHEET (RULE 26) Essay Essay Essay Essay Essay

Xyl-IN1 Xyl-IN2 Xyl-IN3 Xyl-IN4 Xyl-IN5

Liquid coating

contents

Xylitol Xylitol Xylitol Xylitol Xylitol crystallizable

Formulation

GA PVA BF N N

ref.

% materials

60% 60% 60% 60% 60% dry

Coating process

Comp- Comp- Comp- Comp-

Cores ref. CG

SORB SORB SORB SORB

Temperature

inlet air 60 ° C 60 ° C 60 ° C 60 ° C 60 ° C

(drying)

Flow rates 3.5 - 7.5 - 7.5 - 7.5 - 7.5 - 7.5 - 7.5 - 7.5 g / min g / min / min g / min g / min

Observation

gluing step step step during gluing gluing gluing gluing process

Temperature

measured from bed 40 ° C 40 ° C 40 ° C

of cores

Duration of

60 minutes 60 minutes 60 minutes 60 minutes 60 minutes process

Solid, sugar-coated shapes

Gain

mass 20.0% 20.0% 20.0% 20.0% 20.0%

(Gain of (0.33% / (0.33% / (0.33% / (0.33% / (0.33% / mass / minute) minute) minute) minute) minute) minute)

Figures 1. a) 1. b) 1. C) 1. d) 1. e)

Surface area

smooth smooth smooth smooth smooth touch

Homogeneous homogeneous color homogeneous homogeneous homogeneous

Form Form Form Form Form General general general general good, clean, clean, clean, clean, clean,

shapes

impressions impressions impressions irregular impressions

relief embossed relief embossed well well well well identifiable identifiable identifiable identifiable

FIRE I LLE OF REM PLACEM ENT (RULE 26) Essay Essay Essay Essay Essay

Man-IN1 Man-IN2 Man-IN3 Man-IN4 Man-IN5

Liquid coating

contents

Mannitol Mannitol Mannitol Mannitol Mannitol crystallizable

Formulation ref. GA GA PVA PVA2 BF

% materials

20% 20% 20% 20% 20% dry

Coating process

Comp- Comp- Comp- Comp- Comp-

Cores ref.

MANN ^* SORB SORB SORB SORB

Temperature

inlet air 25 ° C 55 ° C 55 ° C 55 ° C 55 ° C

(drying)

Flow rates of 2.2 8.5 3.5 - 7.5 3.5 - 7.5 7.5 - 7.5 7.5 - 7.5 g / min spray g / min g / min g / min g / min

Observation of

no step steps no sticking during

collage collage collage collage collage the process

Temperature

measured from bed 21 -26 ^< Ό 35 ° C 35 ° C 35 ° C 35 ° C of stones

Duration 144 1 50 150 150 1 50 process minutes minutes minutes minutes minutes

Solid, sugar-coated shapes

Mass Gain 1 8.9% 20.0% 20.0% 20.0% 20.0%

(Mass gain (0.13% / (0.13% / (0.13% / (0.13% / (0.13% /

minute) minute) minute) minute) minute) minute)

Figures 2.a) 2.b) 2.c) 2.d) 2.e)

Surface area

smooth smooth smooth smooth smooth touch

Homogeneous homogeneous color homogeneous homogeneous homogeneous

Form Shape Shape General General General

Shape very clear, very clear, very clear, very clear,

shapes

general impressions impressions impressions irregular impressions

well sharp relief embossed relief well well well identifiable well identifiable identifiable

^* these cores did not include raised impressions

FIRE I LLE OF REM PLACEM ENT (RULE 26) Test Bag-IN1 Test Ery-IN1

Liquid coating

Crystalline material Sucrose Erythritol

Formulation ref. GA GA

% dry matter 50% 25%

Coating process

Cores ref. Comp-SORB Comp-SORB

Inlet air temperature 70 ° C

70 ° C

(drying)

Spray rates 3,5 -> 6 g / min 3,5 - 7,5 g / min

Light collage at the beginning

Observation of collage during

which fades as and when no gluing process

measured

Measured bed temperature 44-45 ° C

44-45 ° C

stones

Process time 70 minutes 120 minutes

Solid, sugar-coated shapes

Mass gain 20.0% 20.0%

(Mass gain / minute) (0.29% / minute) (0.17% / minute)

Figures 3.a) 4.a)

Smooth surface +/- smooth smooth

Homogeneous homogeneous color

General form well General form well

Irregular shapes sharp, impressions in sharp, embossed prints well identifiable relief well identifiable

FIRE I LLE OF REM PLACEM ENT (RULE 26) Lso-IN1 test Mal-IN1 test

Liquid coating

Crystalline material Isomalt Maltitol

Formulation ref. GA GA

% dry matter 25% 33%

Coating process

Cores ref. Comp-MANN ^* Comp-MANN ^*

40 g of isomalt after 20 g 50 g of maltitol after liquid of 35 g of liquid of

Priming sprayed sugar coating sprayed then 30 g 40 g isomalt

sprayed solution

Inlet air temperature

60 ° C 55 ° C

(drying)

Spray rates 1, 8 -> 10.0 g / min 1, 7 -> 13.3 g / min

Collage at the beginning who

Observation of collage during

no gluing fades as the process progresses

measured

Measured temperature of the bed

35-40 ° C 30-36 ^< Ό cores

Process time 138 minutes 76 minutes

Solid, sugar-coated shapes

Mass gain 19.5% 15.0%

(Mass gain / minute) (0.14% / minute) (0.20% / minute)

Rough rough touch surface

Homogeneous homogeneous color

General form well General form well

Irregular shapes

net net

^* these cores did not include raised impressions

1 .5. Discussion

The method of the invention advantageously allows all types of solid forms to be coated in a very simple process, and makes it possible to successfully retain complex irregular shapes, such as relief impressions, ridges, and asymmetrical shapes. The inventors have thus succeeded, for example, in coating tablets and chewing gums, whether they are hygroscopic ("Comp-SORB" and "CG") or not ("Comp-MANN") while preserving the raised impressions. present on their surface.

Surprisingly, in spite of the continuous wetting of the nuclei, the stones have not eroded and the complex irregular shapes have been preserved (absence of "logo in- filing", that is to say of filling the grooves and cavities formed by the relief prints). For example, in the tests "Man-IN1 to -IN5", a coating liquid of 20% of

SUBSTITUTE SHEET (RULE 26) dry matter only was used. However, the coated tablets obtained have clearly visible irregular shapes (FIG. 2a), in particular perfectly recognizable relief impressions (FIGS. 2.b) to 2.e)). The method of the invention has in addition to other significant advantages, which make it also useful for coating solid forms having conventional shapes.

The coating liquids used can contain all kinds of crystallizable materials and can be very simple formulating. Tests "Xyl-IN3" and "Man-IN5", for example, show that a binder-free coating liquid ("BF") is also suitable for the process of the invention. The method of the invention also makes it possible to successfully rubberize solid forms with so-called "natural" coating liquids, which in particular are free of titanium dioxide (Test "Xyl-IN4", using the "N" coating liquid ).

The method of the invention also allows the use of very low solids, which is also new in coating. All the tests presented here use coating liquids whose dry matter does not exceed 60%. The method of the invention thus makes it possible to use carbohydrates which are poorly soluble in water (for example mannitol) for coating.

The process of the invention also allows the use of relatively low drying temperatures. The main objective of the "Man-IN1" test is to illustrate this effect and shows that a mannitol coating with a temperature of 25 ° C. is possible. The resulting sugar-coated solid forms have a very clear shape, faithful to that of the starting nuclei (Figure 2. a). The possible use of particularly low drying temperatures makes it possible in particular to obtain a core bed temperature which is also low, thus making it possible to obtain the coating of core compositions having thermolabile ingredients, as is the case with certain active agents. especially pharmaceutical. Thus, in the "Man-IN1" test, the temperature of the tablet bed does not exceed 26 ° C.

The temperature of the coating liquid can also be very low, since the process of the invention does not necessarily require that the latter contain a large amount of crystallizable materials in solution. In these tests, the coating liquids used were indeed at ambient temperature (20-25 ° C.). In addition to facilitating the implementation of the method, this allows the use of thermolabile ingredients in these liquids.

Finally, the solid forms obtained by the process of the invention are satisfactory also with regard to their color and their surface to the touch.

FIRE ILLUSTRATED (RULE 91) ISA / EP 2. Comparative draqification tests

In this part, the inventors have attempted to sugar coat 1 kg of Comp-SORB tablets exhibiting relief printing according to the document US 2008/0026131 A1 mentioned above.

2.1. Equipment used

Equipment with the following characteristics has been used:

rotating drum: diameter 30 cm;

Anti-slip bars x8;

1 compressed air atomization nozzle (BINKS 460); orifice diameter 0.8 mm;

- Peristaltic pump (Watson Marlow model 323); head 3 rollers (313 DW);

Tube: internal diameter 2 mm: outer diameter 6 mm.

2.2. Liquids for coating

According to US 2008/0026131 A1, Example 1, the coating liquids employed were as follows:

"Gum syrup": Formulation (% dry): 96.0% sucrose; 4.0% gum arabic (introduced as a 40% solution by weight of solids); Dry matter content: 72%.

"Smoothing syrup": Formulation (% dry): 97.0% sucrose; 2.0% glucose syrup; 1.0% titanium dioxide; Dry matter content: 70%.

"Color syrup": Formulation (% dry): 98.0% sucrose; 2.0% Blue Pigment (Blue No. 1

Lake); Dry matter content: 69%.

The temperature of these liquids was adjusted if necessary so as to solubilize the compounds. 2.3. Processes and Results

In the following tests, the conditions of Example 1 of US 2008/0026131 A1 have been observed (drying temperatures, dry materials, etc.). The parameters such as the spraying rate or the speed of rotation of the drum have been adapted to the size of the coating chamber available to the inventors.

Test Bag-CP1:

A first test was carried out according to the following table by carrying out several cycles each consisting of a spraying phase, then a pause time (distribution), then a drying step:

SUBSTITUTE SHEET (RULE 26) Speed of

Spray pause drying

Phases cycles rotation of the

(flow, duration) (duration) (° C, duration)

drum

Gumming (gum

1 -9 20 g / min, 1 min 1 min 27 ° C, 7 min 19 rpm syrup)

This test was not successful and was stopped because of too much sticking, despite a drying capacity of the equipment higher than that described in document US 2008/0026131 A1 (50 m ³ / h against 15.3 m ³ / h).

A second test was therefore performed in order to avoid this sticking phenomenon and to reproduce Example 1 of US 2008/0026131 A1 in its entirety. Test Bag-CP2:

Following the failure of the Sac-CP1 test, the first cycle of the first phase was modified: the operator intervened to take off the nuclei, and the operating conditions were modified. This test was carried out according to the following table:

The results obtained are shown in Figure 5. a). The tablets thus coated are very rough, and have a generally coarse and rounded shape. The logos and impressions that were present on the cores are covered and are no longer identifiable. The inventors have found that the surface of the tablet was damaged from the first cycles of coating. The tablets solubilized from the first two minutes, despite the high solids content of the coating liquids used and the crystallization was also very difficult.

Test Sac-CP3: A third test was carried out in which only the "Smoothing" Porphyry Phase of the Sac-CP2 Assay was implemented. Results similar to those of the Sac-CP2 Assay were obtained (Figure 5.b)): the coated tablets had a generally coarse and rounded shape, and the raised prints were covered.

FIRE I LLE OF REM PLACEM ENT (RULE 26)

Claims

Claims A solid coated form, characterized in that it has at least one embossed impression and / or at least one edge and / or in that it is asymmetrical, the coating layer of said asymmetrical sugar-coated solid form conforming faithfully to the shape of the nucleus from which it comes.

A solid coated form according to claim 1, characterized in that it is chosen from tablets, hard capsules, soft capsules, pellets, microspheres, granules, seeds, biscuits, breakfast cereals, confectionery, products in the form of powders and / or crystals.

A method of coating, comprising:

^■ a step (c) collecting the sugar-coated solid forms thus obtained.

A coating process according to claim 3, characterized in that said composition of crystallizable materials comprises at least one substance selected from sugars and polyols.

A coating process according to claim 4, characterized in that the sugars and polyols represent at least 50%, preferably at least 70%, and more preferably at least 90% by dry weight of the crystallizable material composition of the coating liquid .

A coating process according to one of claims 4 and 5, characterized in that said sugars and polyols are chosen from xylitol, sucrose, erythritol, mannitol, dextrose, isomalt, maltitol or a combination of them.

A coating process according to claim 6, characterized in that said sugars and polyols are selected from xylitol, sucrose, erythritol, mannitol, or a combination thereof.

FIRE I LLE OF REM PLACEM ENT (RULE 26)

8. A coating process according to any one of claims 3 to 7, characterized in that said coating liquid has a concentration of crystallizable materials of less than 90%, this percentage corresponding to the weight of crystallizable materials of the coating liquid relative to total weight of said coating liquid

9. A coating method according to any one of claims 3 to 8, characterized in that the compressed air nozzles have an orifice having a diameter selected in a range from 0.1 to 2.8 mm. 10. Sugar-coated solid form, characterized in that it comprises at least one coating layer comprising:

FIRE I LLE OF REM PLACEM ENT (RULE 26)