WO2003001925A2

WO2003001925A2 - Method for preparing a sweetening tablet and resulting sweetening tablet

Info

Publication number: WO2003001925A2
Application number: PCT/FR2002/002179
Authority: WO
Inventors: Philippe Lefevre; Hubert Dupas
Original assignee: Roquette Freres
Priority date: 2001-06-28
Filing date: 2002-06-24
Publication date: 2003-01-09
Also published as: AU2002330535A1; FR2826549A1; WO2003001925A3

Abstract

The invention concerns a method for preparing fast-dissolving sweetening tablets characterised in that it consists in directly compressing a powder comprising granules consisting of lactose and starch jointly pulverised in a lactose/starch ratio ranging between 90/10 and 27/75, preferably between 85/15 and 50/50, and at least an intense sweetening agent. The invention also concerns a sweetening tablet having a dissolving speed in water less than 30 seconds, characterised in that it comprises granules consisting of lactose and starch jointly pulverised in a lactose/starch ratio ranging between 90/10 and 27/75, preferably between 85/15 and 50/50, and at least an intense sweetening agent.

Description

PROCESS FOR THE PREPARATION OF A SWEETENING TABLET AND SWEETENING TABLET THUS OBTAINED.

The subject of the invention is a process for the preparation of a sweetening tablet as well as a tablet comprising at least one intense sweetener.

Synthetic sweeteners, sugar substitutes, such as saccharin, cyclamate or aspartame appeared on the market at the beginning of the century, presented in the form of powder or tablets. Since their commercialization in supermarkets in 1988 in the form of the famous “sweet”, sweeteners have evolved according to the new consumption habits that have become established. Consumers are now incorporating the sweetener into their daily vocabulary, familiarizing themselves with the concept of sweet taste without calories and adopting tablets, lozenges or powders which replace the sugar which they absorbed directly. Producers are therefore striving to multiply the forms and uses of sweeteners. This is how most commercial products, such as CANDEREL ^{® in particular} , exist in the form of lollipops or powder, in various packaging: lollipop dispensers, jars, individual sachets or powder cases.

Consumers of sweeteners in these forms primarily target cold or hot beverages.

They expect the shapes placed at their disposal to be discreet and very quickly disintegrate in the drink to be sweetened without leaving any residue visible. The producers of sweetening tablets, commonly known as “sugar candies”, seek to produce a stable tablet, having the smallest possible size and sufficient hardness for their handling, disintegrating and dissolving as quickly as possible in the liquid to be sweetened, presenting a gustatory neutrality, that is to say not denaturing the flavor of the liquid to be sweetened, and are looking for the simplest formulas and processes possible that can be produced industrially. In addition, these products being similar to nutraceuticals, manufacturers are looking for "natural" ingredients.

The production of tablets by direct compression is the most advantageous technique in particular from the economic point of view since it does not require prior treatment of the powder to be compressed.

Most sweeteners are produced by compaction / compression or briquetting / compression, with lactose monohydrate as a filler-binder and a super disintegrant such as in particular crosslinked carboxymethyl cellulose. These ingredients are insufficiently compressible and therefore cannot be used in a direct compression process.

One of the known techniques for imparting compression properties to powders is wet granulation. It is an expensive process and relatively complex to implement, in which additional additives such as binders are used. Several galenical formulations with aspartame have been tested (MOLARD et al., Labo-Pharma - Problems and techniques - N ° 310 - June 1981) but none allows simple implementation by direct powder compression since granulation or prior compacting of the powder to be compressed is always necessary to obtain satisfactory tablet characteristics.

Other excipients suitable for direct compression have been tested, such as in particular sorbitol, dextrose or maltodextrins, but these excessively soluble excipients hinder the disintegration of the tablets. It is then necessary to use high quantities of super-disintegrating agents which are expensive.

There is therefore an unmet need for a sweetening formulation which is simple to produce and inexpensive. On the strength of this observation, the Applicant therefore endeavored to remedy this deficiency. And it is thus that after many research works, the Applicant has found that it was possible, surprisingly and unexpectedly, by using a particular excipient, to prepare sweetening tablets having both: - sufficient hardness a very rapid disintegration in a drink

- absence of residue after dissolution taste neutrality

- low production cost - natural ingredients The subject of the invention is therefore a process for the preparation of a fast disintegrating sweetening tablet, characterized in that a powder is directly compressed comprising granules consisting of co-dried lactose and starch and at least one intense sweetener.

For the purposes of the present invention, rapid disintegration is understood to mean a speed of dissolution of the tablet, generally less than 30 seconds in water.

Said granules used in the process according to the invention correspond to the compositions described in patent application EP 00 / 402159.8 of which the Applicant is the holder. These granules are characterized by reduced friability, a spherical structure and advantageous compressibility. In addition, the starch and lactose from which they are made are natural products quite suitable for food use. These granules are characterized by a friability generally less than or equal to 80%, preferably less than or equal to 60% according to a test A.

This test A consists in subjecting the granules to be tested to a mechanical action in a device called friabilimeter, of the ERWEKA TA type, manufactured by the company ERWEKA, rotating at a uniform rotation speed of 25 revolutions per minute, and equipped with a drum. in which 5 identical steel balls with a diameter of 17 mm and a weight of about 18.87 g have been introduced. To carry out this test A, an amount of 15 g of product with a particle size between 100 and 200 micrometers, then the apparatus is rotated for 5 minutes. At the end of the experiment, the proportion by weight represented by the residue retained on a sieve with a mesh width of 100 micrometers is determined. The value of the friability corresponds to the percentage of powder not retained by the sieve previously defined.

According to a preferred embodiment of the process according to the invention, said powder comprises 20 to 95%, preferably 50 to 80% by weight of said granules.

Preferably, these granules have a lactose / starch ratio generally between 90/10 and 25/75 and more preferably still between 85/15 and 50/50. Only these ratios make it possible to obtain granules whose compressibility and disintegration properties are optimal. Indeed, beyond 90% lactose compared to the starch contained in the granules, these have poor disintegrating properties. Below 25% lactose in the granules, they no longer compress properly and show poor flow.

These granules are also characterized by a remarkable compressibility, determined according to a test B. This test B consists in measuring the forces, expressed in Newton, which are representative of the compressibility of the composition of granules studied, given for two different density values. tablets. These forces reflect the crush resistance of cylindrical tablets with convex faces (radius of curvature of 14mm), with a diameter of 13mm, with a thickness of 6mm and apparent densities of 1.3 and 1.4 g / ml. To do this, tablets are prepared from granules according to the invention to which 0.5% by weight of magnesium stearate is added beforehand as a lubricant. Compression is carried out using a FROGERAIS AM type press. This press is equipped with round punches with concave faces, with a diameter equal to 13 mm. The penetration of the upper punch and the filling volume of the matrix are adjusted on the press so as to vary the density of the tablets, and the corresponding hardness of these tablets is determined using an ERWEKA durometer of the TBH 30 GMD type. The granules according to the invention, the lactose and starch ratio of which is between 90/10 and 50/50 have remarkable compressibility, resulting in a hardness of tablets generally greater than 70 N and preferably greater than 80 N for a density of 1.3 g / ml and / or generally greater than 170 N, preferably greater than 180 N for a density of 1.4 g / ml.

The lactose and starch granules are further characterized by a rest angle generally less than 45 °, preferably less than 40 °, which reflects their excellent flowability.

These granules can be obtained according to several variants and in particular by co-drying. Preferably, said granules are obtained by coatomization of lactose and starch, according to a process described in the aforementioned patent application. This coatomization process comprises the following stages: a starch suspension is prepared in cold water, to which lactose monohydrate is added. The mixture, having a temperature of between 15 and 25 ° C., is then atomized in a conventional apparatus known to those skilled in the art, by choosing an inlet temperature generally close to 160 ° C. and a flow rate such that the temperatures of l the air and the atomized product are generally close to 65 ° C. at the outlet. Generally, a 20% by weight starch suspension in water will be used. A corn starch will preferably be chosen, and even more preferably an "extra-white" corn starch such as that sold by the Applicant under this designation. The powder thus atomized is generally in the form of perfectly spherical granules and can be compressed directly. To proceed with the preparation of sweetening tablets in accordance with the invention, a powder is generally directly compressed comprising said granules and at least one intense sweetener, without prior granulation, which constitutes a considerable advantage compared with traditional methods. compression.

Preferably, said powder comprises 5 to 80%, preferably 20 to 50% by weight of at least one intense sweetener. By intense sweetener is meant substances with high sweetening power, greater than that of sucrose, natural or synthetic, such as for example aspartame, acesulfame K, alitame, sodium and calcium cyclamate, sucralose, neohesperidine, saccharin, stevioside,

• thaumatin, this list not being exhaustive. One or more intense sweeteners may be incorporated into the powder comprising the granules of lactose and starch by simple physical mixing, or else co-dried at the same time as lactose and starch, for example according to the process in accordance with patent application EP 00 / 402159.8.

In order to manufacture, in accordance with the invention, a quick-disintegrating sweetening tablet, use is generally made of the powder defined above, which can be intimately mixed with the necessary quantities of lubricating ingredients, flavors, colorings , of acidulants and possibly of active principles, the mixture thus obtained being generally directly subjected to compression.

It is also possible to incorporate these ingredients, like the intense sweetener, during the manufacture of starch and lactose granules.

The type of press and punches, as well as the powder compression parameters aimed at determining the size and hardness of the tablets will be adapted according to the needs and the type of product targeted.

The invention also relates, as a new industrial product, to a sweetening tablet having a dissolution rate generally less than 30 seconds in water, characterized in that it comprises granules consisting of co-dried lactose and starch and at least one intense sweetener.

According to a preferred variant, said granules generally represent 20 to 95%, preferably 50 to 80% by weight of the tablet. These advantageously have a lactose / starch ratio generally between 90/10 and 25/75, preferably between 85/15 and 50/50.

Very good results have been obtained with granules obtained by co-atomization of lactose and starch.

With regard to the intense sweetener, it is preferred that it generally represents 5 to 80%, preferably 20 to 50% by weight of the tablet. The sweetening tablet according to the invention is further characterized by a very low friability, generally less than 1%, for a tablet hardness generally less than or equal to 60N.

The friability is typically determined using a Erweka TA friability type, according to the pharmaceutical technology method 2.9.7 of the European Pharmacopoeia, ^3rd edition.

Hardness is typically measured using an ERWEKA TBH 30 GMD type durometer.

The invention further relates to a directly compressible sweetening powder characterized in that it comprises granules consisting of co-dried lactose and starch and at least one intense sweetener. This new industrial product can advantageously be packaged in the form of sachets, cases, or in boxes for sweetening all types of food or dietetic products.

The invention will be better understood on reading the examples which follow, aiming to illustrate in a nonlimiting manner advantageous embodiments and to demonstrate the superiority over the prior art of the process according to the invention and of the products obtained.

Example 1; preparation of sweetening tablets by direct compression and comparison with products of the prior art.

Sweetening lollipops of average weight 100 mg, of thickness approximately 2.5 mm, are prepared using a FROGERAIS press of the AM type equipped with concave punches of diameter 7 mm.

A powder of the following composition (% by weight) is compressed:

- lactose and starch granules (STARLAC ^® ) 78% - aspartame 20%

- DL leucine 2%

- Magnesium stearate 0.1%

The tablets obtained have a hardness of

58.4 Newtons, a friability of 0.76% and a disintegration time of 12 seconds in 100ml of water at 50 ° C with moderate stirring. No residue is observed in water after the tablet has been completely dispersed in water.

The hardness of the tablets is measured using an ERWEKA TBH 30 GMD type durometer. The friability is measured using a Erweka TA friability type, according to the pharmaceutical technology method 2.9.7 of the European Pharmacopoeia, ^3rd edition.

5 Lollipops are prepared according to the same process but with the following composition:

- STARLAC ^® : 74.9%

- Aspartame: 20%

DL leucine: 5%

10 Magnesium stearate: 0.1%

The tablets obtained have a hardness of about 36 N, a friability of 0.9%, and a disintegration time in 100 ml of water at 50 ° C of 7 seconds.

We compare the characteristics of the tablets

15 obtained with lollipops of the prior art:

The tablets according to the invention have a very low friability (less than 1%) and disintegrate in less than 10 seconds in hot water (complete dissolution in 30 seconds) like commercial lollipops. No trace of any component is detectable after complete dissolution of two tablets in tea, while the carboxymethylcelluloses (CMC) of commercial sweeteners remain visible.

During compression, a very regular flow of the powder is observed, making it possible to dispense with the addition of silicas or other agents improving the flow, and to obtain a regular weight of tablets. It is also found that the quantities of lubricant required are lower. The tablets according to the invention are quite comparable to lollipops according to the prior art in terms of dissolution and hardness and have the additional advantage of not generating any deposit in the drink. The method according to the invention makes it possible to envisage savings on the methods of the prior art

(absence of preliminary compacting / briquetting step, absence of super disintegrant) while using natural ingredients (starch and lactose).

Claims

1. Process for the preparation of fast dissolving sweetening tablets, characterized in that a powder is directly compressed comprising granules consisting of lactose and starch coatomised according to a lactose / starch ratio of between 90/10 and 25/75, preferably between 85/15 and 50/50, and at least one intense sweetener.

2. Process for the preparation of sweetening tablets according to claim 1, characterized in that said powder comprises 20 to 95%, preferably 50 to 80% by weight of granules consisting of co-atomized lactose and starch.

3. Process for the preparation of sweetening tablets according to either of Claims 1 and 2, characterized in that the said powder comprises 5 to 80%, preferably 20 to 50% by weight of at least one intense sweetener.

4. Method according to any one of claims 1 to 3, characterized in that said granules have a friability less than or equal to 80%, preferably less than or equal to 60% according to a test A.

5. Sweetening tablet having a dissolution rate in water of less than 30 seconds, characterized in that it comprises granules consisting of lactose and starch coatomised according to a lactose / starch ratio of between 90/10 and 25/75, preferably between 85/15 and 50/50, and at least one intense sweetener.

6. Tablet according to claim 5, characterized in that said granules represent 20 to 95%, preferably 50 to 80% by weight of the tablet.

7. Tablet according to either of claims 5 and 6, characterized in that said sweetener represents 5 to 80%, preferably 20 to 50% by weight of the tablet.

8. Tablet according to any one of claims 5 to 7, characterized in that the said granules have a friability less than or equal to 80%, preferably less than or equal to 60% according to a test A.

9. Tablet according to any one of claims 5 to 8, characterized in that it has a friability less than or equal to 1% for a hardness less than or equal to 60 N.

10. Directly compressible sweetening powder characterized in that it comprises granules consisting of lactose and starch coatomised according to a lactose / starch ratio between 90/10 and 25/75, preferably between 85/15 and 50/50, and at minus an intense sweetener.