US20170135371A1

US20170135371A1 - Novel sweetening composition

Info

Publication number: US20170135371A1
Application number: US15/323,551
Authority: US
Inventors: Dominique ORTIZ DE ZARATE; Sylvie Lagache; Andre Busolin; Antoine Barre
Original assignee: Roquette Freres SA
Current assignee: Roquette Freres SA
Priority date: 2014-07-01
Filing date: 2015-07-01
Publication date: 2017-05-18
Also published as: FR3023128A1; BR112016030891B1; CN106659187A; WO2016001586A1; PL3164013T3; TR201900749T4; TR201901791T4; RU2670875C2; ES2711299T3; JP2017522019A; PL3164012T3; RU2017101603A3; CN106659186A; KR102511424B1; JP2017526343A; CA2953041A1; US10420354B2; BR112016030741B1; CA2953041C; MX369524B

Abstract

A sweetening composition including from 80% to 95% by weight of crystalline pulverulent sorbitol and having an enthalpy of at most 150 J/g, a low specific surface area, a particular particle size and an excellent flow ability. Also the process for producing this novel sweetening composition, and the use of this sweetening composition in a method for preparing chewing gums and tablets.

Description

FIELD OF THE INVENTION

The present invention relates to a pulverulent sweetening composition comprising between 80% and 95% by weight of crystalline sorbitol, said composition having in particular an excellent flow ability.
The invention also relates to the process for producing this novel sweetening composition. Finally, the invention also relates to the use of this sweetening composition in a process for preparing chewing gums and tablets.

TECHNOLOGICAL BACKGROUND

Sorbitol or glucitol is a natural polyol (or sugar alcohol) with a sweetening power which is half that of sucrose. Unlike monosaccharides, its structure contains no ketone or aldehyde function. Sorbitol is mainly used as a bulk sweetener to replace sucrose. It is also used as a sequestering agent, excipient, humectant or stabilizer, in drugs, cosmetics and foods. Having in particular a large water retention capacity, it is responsible for the soft consistency of a large number of food products. The fixed water evaporates with difficulty. Sorbitol is metabolized slowly by the organism and provides few calories. In humans, sorbitol is metabolized in the same way as glucose: it provides the same energy. However, since its metabolism is non-insulin-dependent, it does not increase glycemia. This property is particularly advantageous for products intended for diabetics. In addition, it is non-fermentable by yeasts.
Pulverulent sorbitol, just like the other pulverulent polyols such as xylitol or mannitol, is more particularly used as a pharmaceutical excipient, as a sweetener and as a texturing agent in the food industry, and as an additive support in all types of industries. In powder form, sorbitol is a better excipient than xylitol and mannitol, and is widely used in tablets and chewing gums, because of its very good ability to be compressed and its refreshing effect.
Sorbitol, introduced at the industrial level at the end of the Second World War by the applicant, is currently produced by catalytic hydrogenation of pure dextrose. Dextrose, or D-glucose is itself conventionally obtained by crystallization of a glucose syrup, which constitutes the result of the hydrolysis of starch which is a glucose storage polymer and which represents the energy reservoir polysaccharide in many plants.
Generally, polyols provided in the form of pulverulent products are stored and distributed in double packagings combining an inner plastic bag with a Kraft paper bag or with a corrugated cardboard box or else in flexible containers known as “big bags”, or finally in bulk. The packaging of the sorbitol powder currently sold uses one or other of these packaging methods.
Despite these precautions, the commercial sorbitol powders can have a tendency to agglomerate in large clumps. This caking tendency will be all the greater the finer the particle size of the sorbitol powder.
In general, in order to have a crystalline sorbitol with high compressive strength, it is attempted to achieve the production of a sorbitol of gamma crystalline form (the alpha and beta forms are particularly unstable) by processing a solution that is supersaturated with sorbitol, the gamma form of which represents at least 90%. However, even when it is crystalline in its most stable gamma form, the pulverulent sorbitol conventionally obtained has a certain number of drawbacks, including that of being very hygroscopic.
This high hygroscopicity results in it being made difficult, or even impossible, for pulverulent sorbitol to flow as soon as water uptake has occurred. Its use in direct compression is then limited because of this, requiring for example serious difficulties to be overcome in terms of press filling for the production of bars or tablets.
In order to avoid this problem of the flow of pulverulent sorbitol, it has been recommended to prepare a sorbitol of low density and of coarser particle size, as described in patent FR 1 506 334.
However, it is established that the lower the apparent density of a pulverulent sorbitol, the more friable it becomes, that is to say the more sensitive it becomes to a modification of its particle size by mechanical action. In addition, the dissolution times of this pulverulent product of coarse particle size are generally too long and therefore unsuitable. Finally, while the flow ability is partially improved by using particles of such a particle size, the residual hygroscopic nature that is still too high makes, in any event, the use of this pulverulent sorbitol totally unacceptable when it is combined with ingredients or additives that are very sensitive to water.
It is also established that the capacity to fix large amounts of additives is directly dependent on the specific surface area of said particles. The absorption capacities of pulverulent sorbitol are thus all the higher, the higher its specific surface area. However, it is known that the specific surface area of dense crystals of commercial sorbitol in gamma form is very low. Thus, for a particle size of between 500 and 1000 μm, it is at most equal to 0.7 m²/g.
With the aim of preparing a pulverulent sorbitol which has a better particle size and a good flow ability and which meets the desired compressibility and friability requirements, patent application FR 2 622 190 describes a sorbitol powder containing particles with an average diameter of between 300 and 500 μm. However, the high apparent density and the relatively low specific surface area of said particles, of about 0.9 to 1.2 m²/g, are not in fact significantly modified by the production process implemented, so that the pulverulent sorbitol thus obtained retains the same moisture absorption factor and the same solubility in water as the starting sorbitol powder.
Patent EP 1 008 602 belonging to the applicant company describes a novel pulverulent sorbitol and also the process for preparing same. This novel pulverulent sorbitol simultaneously has the advantages, which are usually incompatible, of, on the one hand, low hygroscopicity and, on the other hand, high specific surface area or, on the one hand, low apparent density and, on the other hand, low friability, this being for a relatively small particle size. From the point of view of its chemical composition, the pulverulent sorbitol claimed is relatively pure, i.e. it has a high pure sorbitol richness, pure sorbitol purity or pure sorbitol content which is generally greater than 95% and more particularly greater than 98% by weight. Thus, the production of this sorbitol requires the use of high-grade raw materials, which has a considerable impact on the production costs for this product.
Thus, for some applications, it would be advantageous to have available a sorbitol composition with a low production cost.

SUMMARY OF THE INVENTION

The applicant company has managed, having carried out numerous research studies, to develop a novel pulverulent sorbitol composition which has a low production cost and has properties that are particularly advantageous for various food and pharmaceutical applications.
Thus, the present invention relates to a sweetening composition, characterized in that it comprises from 80% to 95% by dry weight of crystalline pulverulent sorbitol

- and has an enthalpy at most equal to 150 J/g,
- a volume mean diameter of between 200 and 350 μm, and
- a specific surface area, determined according to the BET method, which is less than 0.6 m²/g, preferably between 0.15 and 0.4 m²/g, and even more preferentially between 0.20 and 0.35 m²/g.

Preferably, the sweetening composition according to the invention is characterized in that it comprises from 85% to 95%, preferentially from 88% to 94.5%, and even more preferentially from 90% to 94% by dry weight of crystalline pulverulent sorbitol.
Preferably, the sweetening composition is characterized in that it has an enthalpy at most equal to 146 J/g of sample, and even more preferentially at most equal to 142 J/g of sample.
The sweetening composition is also characterized in that it has more preferentially a volume mean diameter (arithmetic mean) D4,3 of between 250 and 350 μm, and preferably between 280 and 330 μm.
The composition can be characterized in that the crystalline pulverulent sorbitol consists of at least 85% by weight, preferably of at least 90% by weight, even more preferentially at least 95% by weight of crystals of y form.
The sweetening composition can also be characterized in that its hygroscopicity value, determined by means of its weight change between 0% and 60% relative humidity, is between 2.5% and 3.4%, preferably between 2.8% and 3.2%.
This sweetening composition can have a compressibility of less than 25%, preferably of between 7% and 22% and even more preferentially between 10% and 20%.
A subject of the present invention is also the use of said sweetening composition in the production of chewing gums.
The present invention thus also relates to a chewing gum composition containing, the percentages being indicated by dry weight relative to the total dry weight of said composition:

- from 10% to 28%, preferentially from 15% to 25%, and even more preferentially 20% of at least one gum base,
- from 20% to 70%, preferentially from 30% to 60%, of the sweetening composition described above,
- from 0.1% to 5%, preferentially from 0.5% to 3%, and even more preferentially from 1% to 1.8% of at least one flavoring.

The invention relates to the use of the sweetening composition in the production of tablets for pharmaceutical or food use.

DETAILED DESCRIPTION OF THE INVENTION

The pulverulent sweetening composition in accordance with the invention is first of all characterized in that it comprises:

- from 80% to 95% by dry weight of a crystalline pulverulent sorbitol and has
- an enthalpy at most equal to 150 J/g,
- a volume mean diameter of between 200 and 350 μm, and
- a specific surface area, determined according to the BET method, which is less than 0.6 m²/g, preferably between 0.15 and 0.4 m²/g, and even more preferentially between 0.20 and 0.35 m²/g.

In the present application, the expression “comprises between 80% and 95% by dry weight of a crystalline pulverulent sorbitol” means that the pure sorbitol richness or pure sorbitol content in the sweetening composition is from 80% to 95% by dry weight, the remainder being made up of total reducing sugars such as mannitol, maltitol and also DP3s or even DP4s.
Preferably, the pulverulent sweetening composition in accordance with the invention is characterized in that it has a sorbitol content of between 85% and 95%, preferentially of between 88% and 94.5%, and even more preferentially of between 90% and 94%.
For the purposes of the invention, the sorbitol contained in the sweetening composition is in an essentially y crystalline form. For the purposes of the invention, the expression “essentially y crystalline form”, is intended to mean a content of y form sorbitol crystals of greater than 85% by weight, preferably greater than 90% by weight, even more preferentially greater than 95% by weight.
In one particularly preferred embodiment of the invention, the content of y form sorbitol crystals in the sweetening composition is greater than 98% by weight.
The sweetening composition according to the invention has an enthalpy, or more specifically an enthalpy of fusion or latent heat of fusion, at most equal to 150 J/g.
The enthalpy is determined by differential scanning calorimetry (or DSC).
Differential scanning calorimetry (DSC) operates according to a temperature gradient. It measures the energy provided in order to adhere to the increase in temperature of the sample of sorbitol powder. As long as the product is stable, its temperature changes linearly as a function of the gradient to which it is subjected.
When the product reaches its phase change temperature, it consumes further energy in order to go into liquid form. The additional energy required to adhere to the gradient is recorded by the measuring device. This is enthalpy.
It tends to be regarded that the enthalpy of fusion represents the energy that must be supplied in order to go from the crystal state to an amorphous state. Thus, a predominant crystalline form will have a higher enthalpy, and it will therefore be more difficult to go from said crystalline form to the amorphous form.
Conversely, a less pure mixture containing both a crystalline form and an amorphous form will have a lower enthalpy because it is easier to go into the amorphous state.
Thus, a sorbitol of very high purity, greater than 96% by weight on a dry basis, will therefore have a high enthalpy of fusion since it contains few, or even virtually no, impurities.
Preferably, the sweetening composition according to the invention has an enthalpy at most equal to 146 J/g of sample or even more preferentially at most equal to 142 J/g of sample.
By way of example, the sorbitol sold by the applicant company under the brand name Neosorb® has an enthalpy of fusion of about 165 J/g of sample.
The sweetening composition in accordance with the invention is also characterized by its particular particle size. Thus, the composition according to the invention has a volume mean diameter (arithmetic mean) D4,3 of between 200 and 350 μm.
In one preferential mode, the volume mean diameter (arithmetic mean) D4,3 is between 250 and 350 μm or more preferentially between 280 and 330 μm.
The choice of the particle size of the polyol powders, in particular of the sorbitol powders, is very important. The sorbitol particles have a microscopic structure that is dendritic, i.e. like an entanglement of needles. Because of this particular structure, it has generally been noted that the use of sorbitol powder having a mean particle size greater than 200 micrometers in the production of tablets, bars and/or chewing gums confers on said products a “sandy” texture, in particular on chewing gums (in particular during chewing).
The sweetening composition in accordance with the invention, although it has a larger particle size (a mean particle size greater than 200 μm), does not have this negative effect. Indeed, as demonstrated hereinafter, the chewing gums produced from this composition do not have this unpleasant sandy texture in the mouth.
These mean diameter or mean volume diameter values are determined using an LS 230-type laser diffraction particle size analyzer from the company Beckman-Coulter, equipped with its (dry process) powder dispersion module, according to the operating guide and the specifications of the manufacturer. The operating conditions of hopper screw speed and of vibration intensity of the dispersion chute are determined in such a way that the optical concentration is between 4% and 12%, ideally 8%. The measuring range of the LS 230-type laser diffraction particle size analyzer is from 0.04 μm to 2000 μm. The results are expressed in μm.
The sweetening composition in accordance with the invention is also characterized in that it has a lower specific surface area than a commercial sorbitol.
Indeed, the sweetening composition according to the invention is characterized by a specific surface area, determined according to the BET method, which is less than 0.6 m²/g, preferably between 0.15 and 0.4 m²/g, and more preferentially between 0.20 and 0.35 m²/g.
The specific surface area of the sweetening composition according to the invention is determined by means of an SA3100-type Beckman-Coulter specific surface area analyzer, based on a test for absorption of nitrogen onto the surface of the product subjected to the analysis, by following the technique described in the article BET Surface Area by Nitrogen Absorption by S. Brunauer et al. (Journal of American Chemical Society, 60, 309, 1938). The calculation of the specific surface area is based on the multilayer adsorption theory. For further details on this theory, reference may be made to the book by P. W. Atkins (Atkins and Morrow, 1986).
The BET analysis is carried out in 3 points.
By definition, the specific surface area (Ss), also called “specific surface”, represents the total surface area (As) per unit of mass (M) and it is generally expressed in m²/g.
The specific surface area denotes the actual surface area of the surface of an object, as opposed to its apparent surface area.
The specific surface area in the present invention is measured on a fraction from 250 μm to 841 μm.
The bulking agent, before being subjected to an analysis of its specific surface area, undergoes sieving on sieves of which the particle size is between 250 μm and 841 μm. This makes it possible to remove all the particles of which the diameter is less than 250 μm and also all the particles of which the diameter is greater than 841 μm.
This consequently makes it possible to concentrate on the particle size fraction relating to the major distribution of the powders of bulking agent and to dispense with the fines and the particles that are too coarse, which would distort the analysis.
In the case of a powder, the actual surface area is the sum of the surface areas of the grains. Generally, for a given mass or volume, the finer the grains, the larger the specific surface area.
Very surprisingly, the sweetening composition in accordance with the present invention has a low specific surface area of between 0.20 and 0.35 m²/g, for a volume mean diameter (arithmetic mean) D4, 3 of between 200 and 350 μm.
The opposite would have had to have been expected. With such a volume mean diameter, the specific surface area should normally have been higher, close to 1 m²/g.
To the applicant company's knowledge, there is no commercially available sweetening composition in accordance with that of the invention with similar specific surface area and particle size parameters. The sweetening composition according to the invention goes against the existing preconceptions which correlate the particle size of a powder or diameter of the particles of said powder with its specific surface area.
The sweetening composition in accordance with the invention can also be characterized by its hygroscopicity or a hygroscopicity value, determined by means of its weight change between 0% and 60% relative humidity (RH), of between 2.5% and 3.4%, preferably between 2.8% and 3.2%.
The hygroscopicity measurement test used in the present invention is the same as that described in patent EP 1 008 602. Thus, this test consists in evaluating the variation in weight of the sample of sweetening composition when it is subjected to various degrees of residual humidity (RH) between 0% and 60% at 20° C. in a piece of equipment manufactured by the company Surface Measurement Systems (London UK) and called Dynamic Vapor Sorption Series 1.
This piece of equipment consists of a differential microbalance which makes it possible to quantify the weight change of a sample relative to a reference (in this case the reference cradle of the differential balance is empty) when said sample is subjected to various degrees of humidity.
The vector gas is nitrogen, and the weight of the sample is between 10 and 12 mg. The programmed RHs are 0% RH for 24 h (dehydration), then 10%, 20%, 30%, 35%, 40%, 45%, 50%, 52%, 54%, 56%, 58% and 60% RH. The stability factor which allows the automatic passing from one RH to the next is the dm/dt ratio which is set at 0.002%/min for 20 minutes.
Finally, a table of values corresponding, for each RH, to the equation [(m-m₀)/m₀]×100 where “m” is the mass of the sample at the end of the test for the RH considered and “m_o” is the mass at the end of dehydration, is obtained.
The results are expressed as the difference between the weight change values (as described above) obtained respectively after dehydration (at 0% RH) and then at 60% RH.
Once again, it is particularly surprising that the sweetening composition in accordance with the invention can jointly have a specific surface area of less than 0.6m²/g and a hygroscopicity of between 2.5% and 3.4%. This is because it is very conventionally accepted that the hygroscopicity of a pulverulent product increases with its specific surface area, i.e. its surface area exposed to the medium containing water vapor.
As it happens, the hydrogenated sweetening composition in accordance with the invention has a low specific surface area, characteristic of a crystalline product, with however a relatively high hygroscopicity, characteristic of a granulated product.
By way of examples, the sorbitol sold by the company Merck under the name Sorbitol grade L has a hygroscopicity of 2.4% under the same measuring conditions for a specific surface area according to BET of 1.55 m²/g, and the sorbitol sold by the applicant company under the brand name Neosorb® has a hygroscopicity with a value of 1.53% for a specific surface area of less than 1m²/g.
Surprisingly and unexpectedly and contrary to what was expected, the sweetening composition in accordance with the invention has a hygroscopicity that is notably higher than what is conventionally described for the commercially available pulverulent sorbitols which also have higher specific surface areas.
Because of the higher hygroscopicity of our sweetening composition compared with that of the commercially available sorbitols, caking problems could be expected. However, against all expectations, the sweetening composition in accordance with the invention is characterized by its absence of caking, i.e. by its absence of aggregate formation during its storage for example.
Caking is a general name for the modification of the flow properties of powders, comprising both the formation of small aggregates (which are readily friable or hard) and the sticking or even the total setting to solid of the powder. The formation of links between the particles, due to the solidification of a supersaturated solution at the surface of the particles, is the mechanism responsible for the caking of powders. The caking of crystalline compounds in the pulverulent state is dependent on the particle size of the particles constituting the powder, since the crystals of small dimensions have a high specific surface area and therefore a high water adsorption, thereby leading to dissolution followed by crystallization. The formation of these small crystals serves as a cement for the setting of the powder to solid.
However, the sweetening composition in accordance with the invention does not cake and this can be partly explained by its low specific surface area.
This composition is therefore entirely suitable for being packaged in big bags and/or in bulk.
Indeed, the sweetening composition according to the invention has successfully passed the storage simulation test set up by the applicant.
This test makes it possible to simulate a storage of products in big bags. In order to carry out this test, 1200 g (=m0) of test products are introduced into a polyethylene bag 100 μm thick.
The approximate dimensions of the empty bag are 324 mm by 209 mm
When the product is in the bag, it is hermetically closed while flushing out the maximum amount of air occluded.
This bag is then placed in a metal cylinder 220 mm high and 130 mm in diameter, perforated over its entire surface area with holes 8 mm in diameter, which are arranged in staggered rows with a distance of 12 mm between the centers of the neighboring holes.
A metal disk with a diameter just smaller than that of the cylinder is placed on the bag. A 6.6 kg weight is placed on this disk, that is to say the equivalent of a pressure of approximately 600 kg/m², said pressure being identical to that to which the powder located at the bottom of a big bag is subjected.
The whole thing is then placed in a climatic chamber regulated so as to apply 15 cycles of 8 hours (3.5 hours at a temperature of 15° C. and 85% RH; 0.5 hour of transition; 3.5 hours at a temperature of 30° C. and 85% RH; 0.5 hour of transition).
At the end of these 15 cycles, the 6.6 kg weight and the disk are removed, and then the bag is carefully taken out of the cylinder and opened.
All of the powder is then carefully introduced into a 5-liter keg which is rotated, at the maximum speed, for one minute, using a Mixomat A14 tumbling mixer (Fuchs/Switzerland).
The keg is then opened and the powder therein is emptied onto a sieve, the meshes of which have square openings of approximately 8 mm by 8 mm
Some light shaking on the sieve makes it possible to eliminate all the powder of which the grains have a size below the size of the sieve meshes.
Only the cakes of product retained on this sieve are thus recovered, and these cakes are weighed. The mass ml is then determined.
The ratio (weight of cakes recovered/weight of initial product) ×100 expresses the degree of caked product.
According to the caking test described above, the sweetening composition in accordance with the invention has a caked product ratio of approximately 5%. This therefore means that, under conditions simulating storage in packaging of big bag type, only approximately 5% of the product has formed aggregates, which is extremely low.
It is particularly surprising that the sweetening composition according to the present invention, although it has a hygroscopicity value of between 2.5% and 3.4% and a sorbitol richness or content not exceeding 95%, does not exhibit a caking capacity greater than a commercially available sorbitol, which is purer and has a lower hygroscopicity. Indeed, conventionally, the sorbitol compositions that are commercially available have caked product ratios similar to those found for our composition, but for much lower hygroscopicity values and much higher sorbitol richnesses, of about 98% by weight on a dry basis.
It is in fact well known that the purer a product is, the more it is in a crystalline form and therefore the less tendency it will have to cake.
The sweetening composition in accordance with the invention can also be characterized by its very good compressibility.
The compressibility is defined as the measurement of the ability of a powder to give a tablet when a pressure is exerted. This compressibility is measured by means of the compressibility test which consists in expressing the hardness of tablets as a function of the compressive force exerted in order to obtain them.
In general, it will be said that one product is more compressible than another if this product makes it possible to obtain tablets with a higher hardness at identical compressive force.
The compressibility test is carried out on a Fette P1000 rotary press equipped with round punches (diameter 10 mm) which are concave (radius of curvature of 9 mm).
Before the compression step, the product evaluated is mixed with 0.5% of magnesium stearate which acts as a lubricant.
In order to obtain the various compressive forces, the thickness of the tablet is kept constant (5 mm), on the other hand the weight is variable (a tablet weight corresponds to each compressive force).
In order to evaluate the hardness of the tablet, the tablets formed are then placed in an Erweka 425 durometer. This device gives the value of the force in Newtons required to break/crush the tablet.
The compression profiles obtained for the sweetening composition according to the present invention in comparison with a sorbitol of Neosorb® P60W type for example, sold by the applicant, are virtually superimposable. This means that these two powders have a comparable compressibility, and that the sweetening composition of the invention is just as compressible as a sorbitol powder of the prior art which has a much higher sorbitol content, and the production cost of which is also higher.
The sweetening composition in accordance with the invention can also be characterized by its dissolution rate which is less than 15 seconds. Indeed, the sweetening composition has a high dissolution rate, also reflecting its excellent wettability.
To measure this dissolution rate, a beaker with a volume of 250 ml (short form) is used, and introduced into said beaker are 150 g of degassed demineralized water at 20° C. +/−2° C. Exactly 5 g of hydrogenated sweetening composition powder are weighed out. At t=0 h, the 5 g of sample are rapidly introduced in one go and the timer is started. The time required for the sample to completely dissolve, i.e. for there to be no more particles in suspension, is measured. The test is carried out with gentle stirring at 200 rpm using a magnetic stirrer.
Thus, under the conditions of the dissolution test described above, the sweetening composition in accordance with the invention has a dissolution rate of between 3 and 15 seconds, preferably between 5 and 14 seconds and more preferentially of between 7 and 13 seconds.
The sweetening composition can also be characterized by a bulk density of greater than 0.600, preferably of between 0.610 and 0.700, more preferentially of between 0.630 and 0.660, and a tapped density of between 0.660 and 0.850, preferably between 0.700 and 0.800.
The sweetening composition in accordance with the invention thus has a compressibility of less than 25%, preferably of between 7% and 22% and even more preferentially between 10% and 20%.
Such a compressibility value confers on the sweetening composition a better storage-stability of its pulverulent state. The compressibility values obtained for the sweetening composition according to the invention reflect the properties of a product which flows correctly.
The tapped density, bulk density and compressibility values of the hydrogenated sweetening composition according to the invention are determined using the PTE Powder Tester device sold by the company Hosokawa, according to the specifications of the manufacturer (default setting on 180 shakes for the tapped density measurement).
This device makes it possible to measure, under standardized and reproducible conditions, the flow ability of a powder by measuring in particular the bulk density and the tapped density and then calculating, from these data, the compressibility values using the following formula:
$Compressibility (%) = \frac{(tapped density - bulk density)}{Tapped density} \times 100$
Thus, the sweetening compositions according to the present invention have a particularly high caking resistance but also very good flow (compressibility) characteristics and density characteristics compared with the sorbitol powders of the prior art.
By virtue of these very numerous properties which up until now have never been combined for a sorbitol powder, the sweetening composition which is the subject of the present invention can advantageously be used in a process for producing chewing gum, and also in compression or for the production of tablets.
In the present invention, the term “chewing gum” is used without distinction to denote chewing gums and bubblegums. The difference between these two types is moreover quite indistinct. It is customary to say that chewing gums are chewed whereas bubblegums are intended for blowing bubbles, and therefore are conventionally rather consumed by a young public.
Said composition is particularly suitable for use in processes for producing chewing gums, in particular because of its good flow and its low tendency to create dust, but not only this.
The present invention therefore also relates to the use of the sweetening composition in the production of chewing gums.
The applicant company has demonstrated that the sweetening composition according to the invention is particularly advantageous in terms of reduction of formulation costs in a chewing gum recipe.
Said composition enables in particular a 60%, preferably 50%, and more preferably 40% reduction in the gum base compared with a prior art or conventional chewing gum composition, without having an impact on the final organoleptic qualities of the final product.
What is more, said composition therefore enables a not insignificant reduction in the content of flavorings used. This is because putting less gum base in the recipe has a direct impact on the amount of flavorings to be added.
The use of said composition therefore also enables a 50%, preferably 40%, and more preferably 25% reduction in the amount of flavorings compared with a prior art or conventional chewing gum composition.
Indeed, the applicant company has in particular succeeded in demonstrating that the use of the sweetening composition of the present invention, in a formulation of chewing gum type, makes it possible to confer on the chewing gum a final texture that is more flexible than that of the chewing gums obtained according to the same recipe but using a sorbitol of the prior art. Given that it is the gum base which to a large extent makes it possible to confer the texture on the chewing gum, the applicant company therefore had the idea of reducing the amount of gum base in such a way as to not modify the final texture of the chewing gum. The use of the sweetening composition of the present invention also makes it possible to reduce the amount of flavorings conventionally used. This is because a part of the flavorings remains trapped in the gum base during chewing and these flavorings are never therefore released into the saliva.
There is therefore a double advantage to using the sweetening composition, since it enables, on the one hand, the reduction of the amount of gum base, thereby consequently making it possible, on the other hand, to reduce the amount of flavorings used. Such decreases in amount of gum and of flavorings bring about a considerable reduction in the level of the production costs, and are therefore very advantageous for manufacturers.
The particular properties of the sweetening composition according to the invention, and more specifically its low specific surface area, of less than 0.6 m²/g according to the BET method, combined with a sorbitol content not exceeding 95%, and with a volume mean diameter of between 200 and 350 μm, confer on this hydrogenated sweetening composition the ability to soften the gum base and therefore in the end the chewing gum.
Moreover, although having a lower amount of flavorings in the recipe, the perception of the flavors, both in terms of intensity and in terms of persistence, in the chewing gum containing the sweetening composition according to the invention is at least identical to the chewing gum according to the prior art.
The applicant company has in particular demonstrated that, by reducing the gum base, it was entirely possible to obtain chewing gums that are entirely satisfactory in terms of texture. This was not at all obvious since the proportions between the various constituents are generally fixed and it is not possible to modify them without having a negative impact on the final quality of the products.
The present invention thus also consists of a chewing gum composition containing, the percentages being indicated by dry weight relative to the total dry weight of said composition:

The applicant recommends carrying out this mixing at a temperature of between 45° C. and 80° C., preferentially in a Z-arm mixer with a jacket or in a continuous mixer. Preferably, it is advisable to heat the gum base beforehand to a temperature of between 45° C. and 80° C., preferably between 45° C. and 55° C., by any means known to those skilled in the art. By way of example, it will be possible to heat it in a microwave oven or an oven.
The mixing of the abovementioned compounds may also employ another polyol as sweetening agent, in powder or liquid form, such as, for example, mannitol, maltitol, xylitol, erythritol, lactitol, isomalt, maltitol syrups, sorbitol syrups or hydrogenated glucose syrups.
In one advantageous embodiment of the invention, the hydrogenated sweetening composition can also be combined with a sorbitol syrup in the recipe for producing chewing gums.
Advantageously, the combination of the hydrogenated sweetening composition of the invention with a sorbitol syrup having a purity of less than 96% also makes it possible to reduce the amount of gum base in the chewing gums, and therefore the amount of flavorings.
The mixing of the abovementioned compounds may also employ, in an amount of at most 5% by weight relative to the total weight of the chewing gum, at least one constituent chosen from colorants, intense sweeteners, such as aspartame, acesulfame-K, alitame, neotame, sucralose, saccharin, neohesperidin DC, steviosides, brazzein, pharmaceutical active agents, minerals, plant extracts, antioxidants, indigestible fibers, such as, for example, oligosaccharides, such as fructooligosaccharides, indigestible fibers, such as Fibersol™, sold by the company Matsutani, or else Nutriose®, sold by the applicant, emulsifiers, such as lecithin, etc.
The gum base used may be adapted to the type of chewing gum produced. It may comprise synthetic and/or natural elastomers, such as polyisoprene, polyvinyl acetate, polyisobutylene, latexes, resins, such as terpene resins, polyvinyl esters and alcohols, fats or waxes, such as, for example, lanolin, vegetable oils that are optionally partially hydrogenated, fatty acids, glycerol partial esters, paraffin or microcrystalline waxes.
In the production of the chewing gum composition, the step of mixing the abovementioned ingredients is followed by steps of extrusion, rolling, cutting, cooling then packaging, carried out according to any technique well known to those skilled in the art. In the end, the chewing gum is present in one of the forms well known to those skilled in the art, such as sticks, balls, sweet-coated tablets, cubes or else tablets.
The present invention also relates to the use of the sweetening composition in the production of tablets for pharmaceutical or food use.
The invention also relates, in addition to the chewing gum compositions or chewing gum, a tablet produced from the sweetening composition in accordance with the invention. The sweetening composition content of the tablet will depend on the desired use of said tablet. Typically, the sweetening composition content of the tablet may be between 1% and 90% by dry weight.
The sweetening composition in accordance with the invention is capable of being obtained by:

- hydrogenation of a glucose syrup having between 40% and 50% of dry matter and comprising between 80% and 95% of glucose, between 3.5% and 12% of DP2 and between 0.5% and 8% of DP3;
- followed by a step of concentrating said hydrogenated syrup to a dry matter content greater than 50% and preferably between 70% and 80%;
- a crystallizing step, more particularly a granulating step;
- optionally followed by a maturing step, milling and finally sieving.

For the granulating step, spraying of the hydrogenated or sorbitol-rich syrup onto a sorbitol powder (primer) in a sugar-coating apparatus will most particularly preferably be carried out. Reference may be made here, for this granulating step, to document FR 2 202 867.
A better understanding of the invention will be obtained on reading the following examples, which cannot in any way limit the present invention.

EXAMPLE 1

Process for Producing the Sweetening Composition According to the Invention:
A glucose syrup containing 45% of dry matter and comprising 95% by dry weight of glucose, 4% of DP2 and 1% of DP3 is hydrogenated under a hydrogen pressure of 60 bar. During the hydrogenation, the pH slowly decreases to a low value of approximately 4.5. The pH is then raised back up to 8, by adding sodium hydroxide, in the form of an aqueous sodium hydroxide solution, in order to end the hydrogenation up to a reducing sugar concentration of less than or equal to 2% on a dry basis.
The hydrogenation step is followed by:

- a step of concentrating to a dry matter content of greater than 50%, preferably between 70% and 80% of dry matter;
- a crystallizing step under the conditions described in patent FR 2 202 862;
- and, finally, milling.

EXAMPLE 2

Characteristics of the Pulverulent Sweetening Composition According to the Invention
The composition obtained according to the implementation of the production process described in example 1 is analyzed so as to determine all its physicochemical characteristics, and is compared with a commercial sorbitol powder sold by the applicant company under the brand name Neosorb®.


	Sweetening composition	Neosorb ® P60W
	according to the invention	Sorbitol

Sorbitol (%/on a dry basis)	93.2	98.5
Maltitol (%/on a dry basis)	1.8	0.2
Mannitol (%/on a dry basis)	0.8	0.6
Enthalpy (J/g)	141	163
Volume mean diameter (μm)	320	290
Specific surface area (m²/g)	0.3	0.85
Hygroscopicity (%)	2.9	1.6
Bulk density	0.650	0.680
Tapped density	0.710	0.710

This is the first time that such a sweetening composition having the characteristics combined above is described. This composition is therefore novel.

EXAMPLE 3

Use of the sweetening composition according to the invention in the production of chewing gums
The control was carried out with a sorbitol powder sold by the applicant company under the brand name Neosorb®.
All the percentages expressed are done so relative to the total dry weight of the chewing gum composition used.

I. Preparation of the Chewing Gum Compositions

Ingredients used in the Chewing Gum Compositions:


	Control composition	Compositions according
Ingredients	(%)	to the invention (%)

Solsona T gum base	30	20
Mannitol 60	5	5
Xylitol 90	7	7
Lycasin ® 85/55 maltitol	4	8
syrup
Glycerol	4	4
Liquid flavoring	1.50	1.10
Powder flavoring	0.50	0.50
Neosorb ® P60W Sorbitol	48	0
Sweetening composition	0	54.4
according to the invention
TOTAL	100	100

The Solsona T gum base is sold by the company Cafosa.
The Neosorb® P60W sorbitol is a crystalline sorbitol powder sold by the applicant. The mannitol 60, the xylitol 90 and the Lycasin® 85/55 maltitol syrup are also sold by the applicant.
Procedure for Preparing the Control Chewing Gum Compositions and the Chewing Gum Compositions According to the Invention

- Mixing: procedure in minutes—Carried out in a Z-arm mixer at 45° C.—Production of a batch of 50 kg of center

0 min: Introduce the molten gum base (stoved overnight at 50° C.) and the mannitol and xylitol.
3 min: Add the Lycasin® 85/55.
5 min: Add either the Neosorb sorbitol, or the hydrogenated sweetening composition according to the invention.
9 min: Add the glycerol.
10 min: Add the powdered flavoring.
12 min: Add the liquid mint/vanilla flavoring.
15 min: Unload the mixer (the dough is at approximately 50° C.). Form blocks of approximately 2 kg and store for 1 hour at 50% RH and at 20° C. The blocks must be at approximately 48° C. for the extrusion.

- Extrusion (Togum TO-E82 apparatus).
- Body setpoint temperature =36° C.
- Head setpoint temperature =39° C.
- Rolling 4 stations-Pre-cutting 2 stations (Togum TO-W191 apparatus).
- Sprinkling of the strip of chewing gum with a 90/10 mannitol/talc mixture.
- Maturation.
- Store the precut sheets of tabs at approximately 15° C-50% RH for approximately 24 h.

2. Evaluation of the Organoleptic Qualities of the Chewing Gums

The chewing gums previously obtained were tasted by a panel of 15 individuals trained in the tasting and grading of chewing gums.
The panel was asked to grade from 0 to 4 the flexibility of the chewing gums during the first seconds of chewing, but also after three minutes of chewing,
4 being the maximum flexibility and 0 corresponding to a very hard or even brittle chewing gum.
The panel was also asked to grade the perception of the flavor during chewing. This test was also carried out during the first seconds of chewing and after three minutes of chewing in order to evaluate the persistence of the flavor,
4 being the grade given for a very strong flavor and 0 corresponding to a chewing gum no longer having any flavor at all.
The products were presented in a random order, and coded with a 3-figure number so that the panellists are not influenced either by knowledge of the products or by their codes. The tastings were carried out in a sensory analysis laboratory.
At T+0, the chewing gum is placed in the oral cavity and at the same time the timer is started. Chewing then begins.
The data were processed by means of statistical processing (ANOVA and mean comparison tests are performed on the means obtained at each time interval).


	Evaluation	Evaluation
	of flexibility	of flavor persistence

	T =		T =
	10 seconds	T = 3 min	10 seconds	T = 3 min

Control CG	4	3	4	2
CG according	4	3	4	3
to the invention

It emerges that:

- the flexibility of the two chewing gums changes in an identical manner Although containing 10% less gum base than the control chewing gum, no difference in terms of texture and more particularly in terms of flexibility between the two samples was noticed by the panel of tasters.
- In terms of the perception and persistence of the flavour, here again there is no difference at t=10 seconds between the control chewing gum and the chewing gum according to the invention. Although having a lower amount of flavorings in the recipe, the perception of said flavorings in the chewing gum containing the sweetening composition according to the invention is identical to the control chewing gum. It would even appear that the flavor persistence is improved over time since the chewing gum obtained from the sweetening composition according to the invention, containing less gum base and less flavoring, is nevertheless graded as being slightly better than the control chewing gum after three minutes of chewing.
- Thus, the chewing gum produced with the sweetening composition according to the invention and containing 10% less of gum base relative to weight, that is to say a reduction in said gum base of 33%, and containing 0.4% less of flavoring relative to weight, that is to say a reduction of 20% in the amount of flavoring, is identical in terms of texture and is slightly better in terms of flavor persistence.

The advantage of the present invention is perfectly demonstrated by this example.

EXAMPLE 4

4 other tests were carried out in order to test the advantage of the sweetening composition according to the invention in the reduction of the gum base content in a chewing gum recipe and in order to compare said composition according to the invention with other polyols. The 4 new tests were carried out with a gum base content reduced to 20% (by weight).
Test 1 relates to a chewing gum recipe carried out with Neosorb® P60W.
Test 2 relates to a chewing gum recipe using the sweetening composition according to the invention.
Test 3 relates to a chewing gum recipe carried out with maltitol sold by the applicant company under the brand name SweetPearl®, and having a mean particle size of 150 μm.
Test 4 relates to a chewing gum recipe carried out with maltitol sold by the applicant company under the brand name SweetPearl®, and having a particle size of 90 μm.
All the percentages expressed are done so relative to the total dry weight of the chewing gum composition used.
Preparation of the Chewing Gum Compositions
Ingredients used in the Chewing Gum Compositions:


	Control
	Composition
INGREDIENTS	(Example 3)	TEST 1	TEST 2	TEST 3	TEST 4

NEOSORB ®	48.00	54.38
P60W sorbitol
Sweetening			54.38
composition
according to
the invention
SweetPearl ® 150				54.38
SweetPearl ® 90					54.38
Solsona T gum base	30.00	20.00	20.00	20.00	20.00
Mannitol 60	5.00	5.00	5.00	5.00	5.00
Xylitol 90	7.00	7.00	7.00	7.00	7.00
Glycerol	4.00	4.00	4.00	4.00	4.00
Lycasin ® 85/55 maltitol	4.00	8.00	8.00	8.00	8.00
syrup
Liquid flavoring	1.50	1.13	1.13	1.13	1.13
Powder flavoring	0.50	0.50	0.50	0.50	0.50
TOTAL	100	100	100	100	100

The procedure for preparing the control chewing gum compositions and chewing gum compositions according to the invention is exactly the same as the one described in example 3 above.
Evaluation of the Behavior of the Chewing Gums during Batchwise Preparation thereof
The control (control composition of example 3) behaves very well during chewing gum preparation. The gum is nicely elastic and not too hard. There is no disappointing tacky phenomenon.
Test 1 (Neosorb® P60W and 20% gum base) provides an extremely hard gum base which increasingly hardens over time. The gum is very compact with no elasticity. Furthermore, this test is very dry.
Test 2 (composition according to the invention and 20% gum base) exhibits a behavior identical to that of the control, namely: a gum base which is nicely elastic and not too hard. There is no disappointing tacky phenomenon.
Test 3 (SweetPearl® 150 and 20% gum base) has a gum with an extremely soft base. It has good elasticity, but is very tacky and difficult to put into form.
Test 4 is identical to test 3.
Evaluation of the Organoleptic Qualities of the Chewing Gums
The chewing gums previously obtained were tasted by a panel of 15 individuals trained in the tasting and grading of chewing gums.
The panel was asked to grade from 0 to 4 the flexibility of the chewing gums after three minutes of chewing, 4 being the maximum flexibility and 0 corresponding to a chewing gum having become very hard or even brittle.
The hardness was also graded as being the resistance of the chewing gum when setting about chewing, 4 being the grade for a chewing gum exhibiting resistance to chewing and 0 being for a chewing gum that is extremely soft immediately upon setting about chewing.
The panel was also asked to grade the perception of the flavor during chewing. It was asked to time the moment when the flavor was the strongest. This is what is referred to as the aromatic peak. This peak is noted in seconds. An early aromatic peak signifies an earlier release of the flavor during chewing, and therefore a depletion of aromatic notes that is also earlier.
The intensity of the aromatic peak was also graded on a scale of 1 to 3,
3 being the grade given for a high aromatic peak and 0 corresponding to an aromatic peak of low intensity.
In addition, the final criterion evaluated is that of the volume occupied by the chewing gum at the end of chewing. The larger the chewing gum, the higher the grade, 4 being the maximum.
The products were presented in a random order, and coded with a 3-figure number so that the panellists are not influenced either by knowledge of the products or by their codes. The tastings were carried out in a sensory analysis laboratory.
At T+0, the chewing gum is placed in the oral cavity and at the same time the timer is started. Chewing then begins.
The data were processed by means of statistical processing (ANOVA and mean comparison tests are performed on the means obtained at each time interval).
It emerges that:


			Tps for the	Intensity of
Hardness	Volume	Flexibility	peak (s)	the peak

Control	3.68	3.16	2.95	31.94	2.04
Test 1	3.48	2.44	2.77	22.59	2.03
Test 2	3.49	2.58	2.93	30.07	2.40
(invention)
Test 3	0.98	1.78	2.98	24.05	2.72
Test 4	0.70	1.78	3.73	24.59	2.72

The control chewing gum is relatively hard, has a large volume at the end of chewing and has a later aromatic peak. This means that the flavor persistence will also be longer during chewing.
The two tests carried out with maltitol of two different particle sizes gives chewing gums which are not at all satisfactory. They were judged to be much too soft and to have no hardness and resistance when setting about chewing. Furthermore, the volume at the end of chewing is very small, thereby signifying that there was no expansion during chewing. The occurrence of the aromatic peak is earlier. The aromatic intensity perceived is greater. Necessarily in these two tests, since the chewing gum is much too soft, it is easy to imagine that access to the aromatic molecules present in the gum base is easier.
Test 1 is satisfactory in terms of the characteristics of hardness and of volume at the end of chewing. The aromatic peak occurs relatively early and thus the flavor persistence is less over time. What is more, the intensity of the aromatic peak is relatively low.
Test 2 containing the sweetening composition according to the invention is the test which gives the most satisfaction. Although containing only 20% of gum base, it has a late aromatic peak reflecting good flavor perception during chewing. Furthermore, the intensity of the peak is also high and attests to an excellent flavor perception. This all being the case for a chewing gum which exhibits good hardness when setting about chewing. Finally, the volume obtained at the end of chewing also attests to the fact that the chewing gum has indeed expanded during chewing thereof.
Thus, the chewing gum produced with the sweetening composition according to the invention and containing 10% less of gum base relative to weight, that is to say a reduction in said gum base of 33%, and containing 0.37% less of flavoring relative to weight, that is to say a reduction of 18.5% in the amount of flavoring, is identical in terms of texture and is slightly better in terms of aromatic perception than a chewing gum produced according to the prior art. The advantage of the present invention is perfectly demonstrated by this example.

EXAMPLE 5

Use of the sweetening composition according to the invention in the production of chewing gums in combination with a sorbitol syrup
Preparation of the Chewing Gum Compositions
Ingredients used in the Chewing Gum Compositions:


Recipe	Control	Test 1	Test 2

Neosorb ® P60W sorbitol	38.40	44.40	0.00
Sweetening composition according	0.00	0.00	44.40
to the invention
Liquid sorbitol at 95% purity	89.60	103.60	103.60
Solsona T gum base	60.00	40.00	40.00
Glycerol	8.00	8.00	8.00
Liquid flavoring	3.00	3.00	3.00
Powder flavoring	1.00	1.00	1.00
TOTAL	200	200	200

All the percentages expressed are done so relative to the total dry weight of the chewing gum composition used.
The chewing gums were prepared according to the same process as that described in the previous examples.
The chewing gums were also tasted by a trained jury according to the criteria indicated in example 3 below.
It emerges that:
The flexibility of the three chewing gums changes in an identical manner Although containing 10% less gum base than the control chewing gum, no difference in terms of texture and more particularly in terms of flexibility between the three samples was noticed by the panel of tasters.
In terms of the aromatic perception, the chewing gum of test 1 was noted as being that which had the greatest aromatic note and a persistence in terms of duration that was also longer.
Thus, the chewing gum produced with the sweetening composition according to the invention and containing 10% less of gum base relative to weight, that is to say a reduction in said gum base of 33%, is identical in terms of texture and is slightly better in terms of flavor persistence. The advantage of the present invention is once again perfectly demonstrated by this example.

EXAMPLE 6

Measurement of the Specific Surface Areas According to the Invention
As indicated above, the specific surface area according to the invention is measured on a sample of powder obtained on a fraction of from 250 μm to 841 μm.
Preparation of the Sample
To prepare the sample, a sufficient amount of sample is sieved on sieves of 841 μm and 250 μm in order to recover approximately 3 grams of a particle size fraction of between 841 and 250 microns.
A sample is then introduced into a measuring cell of the apparatus, dried beforehand and tared to within 0.001 g, the sample being sufficient to ¾ fill the reservoir of the cell.
Degassing
The cell containing the sample is placed in the degassing station.
The degassing is carried out by referring to the instructions for use of the apparatus.
Analysis of the Powder
Once the degassing has been carried out, the cell is again weighed to within 0.001 g and is placed in the measuring station. The analysis is then carried out by referring to the instructions for use of the apparatus.
The apparatus automatically processes the results collected. The result is expressed in m²/g.

Claims

1. A sweetening composition, characterized in that it has:

from 80% to 95% by dry weight of crystalline pulverulent sorbitol,

an enthalpy at most equal to 150 J/g,

a volume mean diameter of between 200 and 350 μm,

a specific surface area, determined according to the BET method, which is less than 0.6 m²/g, preferably between 0.15 and 0.4 m²/g, and even more preferentially between 0.20 and 0.35 m²/g.

2. The sweetening composition as claimed in claim 1, characterized in that it has between 88% and 94.5%, and more preferentially between 90% and 94%, of crystalline pulverulent sorbitol.

3. The sweetening composition as claimed in claim 1, characterized in that the enthalpy is at most equal to 146 J/g of sample, and even more preferentially at most equal to 142 J/g of sample.

4. The hydrogenated sweetening composition as claimed in claim 1, characterized in that its volume mean diameter (arithmetic mean) D4,3 is between 250 and 350 μm, and preferably between 280 and 330 μm.

5. The sweetening composition as claimed in claim 1, characterized in that the sorbitol consists of at least 85% of crystals of γ form, preferably of at least 90% by weight, or more preferentially of at least 95% by weight of crystals of γ form.

6. The sweetening composition according to claim 1, characterized in that it has a hygroscopicity value, determined by means of its weight change between 0% and 60% relative humidity, of between 2.5% and 3.4%, preferably between 2.8% and 3.2%.

7. The sweetening composition as claimed in claim 1, characterized in that its compressibility is less than 25%, preferably between 7% and 22% and even more preferentially between 10% and 20%.

8. A method of producing chewing gums comprising mixing the sweetening composition as claimed in claim 1 with a chewing gum base and at least one flavoring.

9. A chewing gum composition containing, with the percentages being given by dry weight relative to the total dry weight of said composition:

from 10% to 28%, preferentially from 15% to 25%, and even more preferentially 20% of at least one gum base,

from 20% to 70%, preferentially from 30% to 60%, of the sweetening composition as claimed in claim 1,

from 0.1% to 5%, preferentially from 0.5% to 3%, and even more preferentially from 1% to 1.8% of at least one flavoring.

10. A method for producing tablets for pharmaceutical or food use comprising adding the sweetening composition as claimed in claim 1 to a tablet composition for pharmaceutical or food use.