SK281742B6 - Maltitol composition and method for preparing same - Google Patents

Abstract

The maltitol mixture has a porous honeycomb structure with high maltitol purity and low density. This mixture is suitable for the manufacture of tablets or various water-soluble powders. Also described is a process for producing a crystalline maltitol mixture

Description

The invention relates to a novel crystalline mixture of maltitol having a porous cellular structure, high purity of maltitol and low density. The invention also relates to a process for the preparation of this composition and its industrial use.

BACKGROUND OF THE INVENTION

4-O-α-D-Glucopyranosyl-D-glucitol, commonly known as maltitol, is a polyol obtained by industrial hydrogenation of maltose. Since it is chemically more stable and less caloric than sucrose and has organoleptic properties very close to sugar, it is of great interest. Moreover, maltitol has the peculiarity that it does not cause tooth decay, which opens it up and has already opened up a wide range of applications in the food and pharmaceutical industries.

For a very long time, maltitol has been known only in the form of low concentration syrups. For example, this polyol is a major component of LYCASIN 80/55 and MALTISORB 75/75 syrups, which have been administered for more than twenty years. The maltitol content of these syrups never exceeds 78% of their dry matter.

Maltitol was sold in the form of amorphous powders which were not pure. Therefore, maltitol solutions were often dried by atomization. As is known in the literature, this technique has always been considered to be a very difficult manufacture, particularly in view of the need to perform exactly both the essential degrees of adhesion in the shower tower, but also because of the very hygroscopic properties of the powders so obtained. Numerous inventions testify to important work to solve these problems. Some of these inventions are listed below:

GB 1 383 724, JP 49-87 619 and US 4,248,895 proposing to add various substances such as alginates, celluloses, modified starches, polyvinylpyrrolidones, hydrophilic polymers, proteins or protein extracts to the maltitol solutions prior to atomization, to reduce adhesion in the atomization tower.

JP 50-59 312 and JP 51-113 813 disclose methods for atomizing anhydrous dissolved maltitol mixtures. JP 49-110 620, U.S. Pat. No. 3,918,986, U.S. Pat. Nos. 3,915,736, JP 50-129,769 and JP 48-61,665, which disclose methods refer to reducing the hygroscopicity of maltitol anhydrous powders either by adding anti-noise agents or by coating the maltitol powders with carbohydrates, polyols or fatty substances, or e.g. wet granulation.

For the first time, crystals of maltitol were not prepared until around 1980. Previously, this polyol has always been considered a non-crystalline product. This erroneous conclusion, which has long been anchored in the subconscious, stems from the fact that crystallization of maltitol from a supersaturated solution from the beginning is not spontaneous, as in the case of other polyols such as mannitol, erythritol or isomalt. Some of the special properties of maltitol, in particular its viscosity and solubility, are the cause of the difficulties that have been observed.

The only crystalline form known so far for maltitol is the anhydrous form described in U.S. Pat. No. 4,408,041 to HAYASHIBARA. To recognize the properties of this crystalline form, this patent, filed in 1981, may be based on the "X-ray crystal structure of maltitol (4-O-α-D-glucopyranosyl-D-glucitol)" by SHOICHIOHNO et al., "Research on Carbohydrates, 108 (1982), 163-171. ”Several years later the first pseudocrystalline maltitol powders appeared on the market. These have been, and are, for some of them, being treated by a technique known as the "solidified" technique, which consists in solidifying an anhydrous solution of maltitol having a concentration that can reach at best 90% with the addition of seed crystal composed of carbohydrate or polyol crystals. Such a procedure is described, for example, in JP 57-47 680 and JP 58-158 145.

U.S. Pat. No. 4,408,401, mentioned earlier, it has also been proposed to prepare a crystalline powder mixture called "total sugar" by atomizing pre-crystallized solutions or solutions thickened by cooking "massescuites". These are obtained by very slow re-cooling of the supersaturated aqueous solution of maltitol, which contains a large number of polyols such as sorbitol, maltotriitol, maltotetraitol and other polyols of high degree of polymerization.

Such very slow cooling and the addition of a maltitol seed crystal will cause maltitol crystals to appear in the solution. When 20-60% of maltitol crystallizes out of this aqueous solution, it is atomized at a very low temperature, which is stated between 60 ° C and 100 ° C, in order not to lose intentionally formed crystals. As a result, the "total sugar" obtained contains 25 to 60% crystalline maltitol in the form of crystals completely identical to those obtained by crystallization in water. The disadvantages resulting from the presence of such crystals for certain specific applications are listed below.

This "whole sugar" is not sufficiently crystalline as required if it relates to the description in particular in Example 4, by drying for 40 minutes and also by allowing it to ripen for 10 hours. Obviously, this procedure was not of interest because it is time-consuming and did not represent the least progress.

A decisive step in the production of very high concentration crystalline maltitol powder was achieved due to the applicant's work, which introduces a new production method based on the use of fractionation techniques by continuous chromatography. These processes are the subject of patents EP 0 185 595 and EP 0 189 704 and make it possible to obtain, at comparable prices, powders having a purity of 99% by simple crystallization of maltitol in water present in the chromatographic fraction particularly rich in this polyol. Such a crystalline powder, for example, was marketed by the applicant several years ago, under the name crystalline MALTISORB.

Processes, which are called "solidified" techniques (massé) on the one hand, and water-based crystallization techniques on the other hand, are today almost the only industrial uses. The products thus obtained, the crystallinity of which is very diverse, are particularly suitable for certain applications, such as e.g. chewing gum or chocolate.

On the other hand, there are other uses for which these products are not quite satisfactory. This is the case, for example, if it would be desirable to use maltitol as a replacement for sucrose or lactose in the form of dry pharmaceuticals such as capsules, powders and solutions, tablets and powdered nutritional formulations for dissolution. This is also the case when it is desirable to make a substitute of the same type in sweet foods such as powdered drinks, desserts, cake preparations or chocolate and vanilla powders for breakfast.

In these particular applications, it has been observed that the pseudo-crystalline maltitol powders obtained by the solidified technique (massé) as well as the crystalline maltitol powders containing the crystals obtained by crystallizing maltitol in water exhibit one or more disadvantages, in particular that they

They are poorly marketed, cause solidification or agglomeration, dissolve slowly in water, have poor compression excipients, or do not meet the resolution and purity criteria required by different pharmacopoeias.

In the case of mannitol, it has already been proposed to improve the compression capacity by extrusion. Such a method is described, for example, in U.S. Pat. EP 0 220 103 owned by the applicant. It is not ideal as it does not make it possible to improve to a greater extent the jointly found deficiencies concerning the product's marketability.

It is an object of the present invention to improve the state of the art by providing a mixture of maltitol which does not have the aforementioned drawbacks of unsalability, agglomeration, insolubility or difficult compressibility, as has previously been known to maltitol powders. It may be considered that this requirement could be satisfied by other polyols. However, this approach is inappropriate because none of them has been found to have the necessary properties such as solubility, hygroscopicity, sweet taste and melting as close to sucrose as those of maltitol.

Contrary to all expectations, the present invention is successful and, after very thorough research in this field, solves a crystalline mixture of maltitol which does not have any of the above drawbacks. The invention demonstrates that, surprisingly and unexpectedly, such a crystalline mixture can be prepared under special conditions, starting with a syrup having a maltitol concentration of greater than 92%, using a process similar to atomization, although it has never been accepted in the past that this technique directly achieved crystallization of maltitol. Among other things, it should be noted that the atomization technique for maltitol has fallen into complete oblivion once the possibility of crystallizing this polyol from the supersaturated solution and the subsequent onset of procedures based on this principle, which are considered very effective, has been shown.

Accordingly, the invention relates first of all to a crystalline mixture of maltitol having a substantially porous and honeycomb structure of maltitol at a concentration greater than or equal to 92% and a bulk weight comprised between 100 to 700 g / l.

In the case of the present invention, the term concentration refers to the percentage of mannitol expressed in dry weight / dry weight relative to the amount of carbohydrates in the crystalline mixture of maltitol. These carbohydrates may be sugars such as, in particular, D-glucose, maltose, maltotriose, maltotetraose and polyols, which are formed by hydrogenation of these sugars. Usually this concentration is measured by high performance liquid chromatography.

SUMMARY OF THE INVENTION

A first essential feature of the maltitol composition is that it is crystalline, which gives it a high stability to moisture. As a result, it has little ability to solidify or agglomerate. This makes it easy to use and there is no need to take strict measures to avoid this risk.

The crystallinity of the composition of the invention can be evaluated by differential thermal calorimetry. It is directly proportional to the melting enthalpy which is preferably greater than 130 J / g, more preferably greater than 145 J / g and most preferably greater than 155 J / g.

Surprisingly, it has been found that the composition according to the invention still has a crystallinity substantially higher than maltitol massé or hardened maltitol, and a crystallinity generally higher than maltitol extruded at the same maltitol concentration and a crystallinity generally only slightly lower than maltitol crystallized in water at the same concentration maltitol. Naturally, the composition of the present invention has a melting enthalpy of between 160 and 164 J / g, i.e. that melting enthalpy is usually in the range of 80 and 120 J / g for maltitol massé, such as MALBIT CR powder, in the range of 130 and 145 J / g for maltitol is extruded and is between 163 and 167 J / g for maltitol crystallized in water, such as crystalline MALTISORB, manufactured and marketed by the applicant.

It has also been found that the composition of the invention has a melting point between 148 and 150 ° C, generally about 149 ° C. This temperature tends to be slightly lower than the melting point of maltitol crystallized from water at the same maltitol concentration.

According to a further feature, the crystalline maltitol composition of the invention has a maltitol content of at least 92%. However, since it can crystallize directly and much more perfectly, it preferably has a maltitol content of greater than or equal to 95%, even more preferably greater than or equal to 98%. Ideally, a concentration of about or more than 99% is achieved.

It is likewise advantageous that the composition according to the invention contains only a small amount of other polyols, such as maltitol, which polyols may in particular be sorbitol, xylitol, mannitol, iditol, arabitol, maltitotriitol or maltitotetraitol. The content of these polyols is preferably less than 5% and even more preferably less than 2% based on the dry weight of the mixture. In fact, their presence has been found to significantly impair the crystallinity of the composition of the invention. However, this is not the case or much less if the mixture contains some other substances. This explains that the crystalline mixture of maltitol may contain such substances in an entirely greater amount without being disadvantageous, depending on the use for which it is intended.

Substances capable of entering the crystalline maltitol mixture without major difficulties include, for example, intense sweeteners, colorants, perfumes, flavors, vitamins, minerals, pharmaceutical or veterinary active substances, fatty acid esters, organic acids or minerals and their salts, proteinaceous substances such as proteins, amino acids and enzymes.

A third principle is that the crystalline mixture of maltitol according to the invention usually has a density lower than that of the previously known maltitol powders. This density can be measured, for example, using an apparatus marketed by HOSOKAWA under the brand name "Powder Tester", which uses the method recommended for measuring bulk density. Under these conditions, the composition of the invention has a bulk density in the range of about 100 to about 700 g / l, more preferably in the range of 200 to 670 g / l, and most preferably in the range of 300 to 650 g / l. Typically, its bulk density is between 400 and 650 g / l.

The lower density of the composition according to the invention is due to the particular structure which clearly distinguishes it from the previously known maltitol powders. Microscopic observation revealed that its structure is essentially porous and honeycomb. In addition, the particles forming the composition of the invention are substantially spherical, free of sharp edges and formed by a plurality of crystalline microparticles joined together. This structure clearly clearly differs from the structure of maltitol crystallized in water and extruded maltitol, which is formed by cubic particles or very angular prismatic particles, or even from maltitol hardened, which has a very dense structure containing particles that are weakly birefringent in polarized light.

The composition according to the invention is almost free of particles whose shape and aspect would be similar to those observed with maltitole crystallized in water, extruded or hardened maltitole.

The composition according to the invention generally has a specific surface area of less than 0.2 m ³ / g.

In addition, it has been found that, when measuring porosity in mercury particles from 160 to 250 microns, the composition of the invention, unlike maltitol powder crystallized in water, consists of particles having an open pore size in the range of 1 to 10 microns. As a rule, the content of these pores is 0.01 to 0.03 cm ³ / g, which is less than the conventional content in "massé" or hardened maltitol powders or extruded powders.

The water content, given by drying the crystalline maltitol mixture of the invention at 130 ° C for two hours, is preferably less than 3% and even more preferably less than 1%. As a rule, this content is even less than 0.5%, but even less than 0.35%.

For the functional properties of the crystalline maltitol composition according to the invention, a measuring device sold by HOSOKAWA was used to assess its flowability, which allows to measure the flowability of the powder under standardized conditions with reproducible results, to calculate the degree of flow, called the Carr index. The composition according to the invention has an excellent degree of flowability in the range of 70 to 90. This value is preferably in the range of 75 to 90 and even more preferably in the range of 80 to 90. This value is very close to the flow rate values of the maltitol powders previously known by extrusion. crystals crystallized in water.

The flowability of the composition according to the invention is generally significantly higher than the flowability of maltitol powders obtained by simple water crystallization or by solidification techniques.

It can be concluded that the excellent flowability of the composition of the invention is explained by a combination of several of its physicochemical properties, mainly due to the absence of important electrostatic charges on the surface of the particles it consists of maltitol concentration, low hygroscopicity and finally characteristic particle shape. create. This excellent flowability is advantageous because it makes it very easy to fill and empty hoppers, tanks or containers such as bags or capsules.

A second essential functional property of the crystalline maltitol composition of the invention is its rapid dissolution in water. This dissolution rate was measured according to Test A, which involves placing exactly 5 grams of a granulometric cross-section of 200-315 microns of the test sample into 150 g of demineralized and degassed water maintained at 20 ° C in a 250 ml shallow beaker and stirred at 200 rpm. min. The dissolution time is then equal to the time it takes after the product is introduced to obtain a visibly pure formulation. Under these conditions, the composition of the invention has a dissolution time of less than 30 s, and preferably less than 26 s, and more preferably less than 20 s. These times are generally lower than those of all maltitol powders currently marketed.

Obviously, the rapid dissolution property is an undeniable advantage, for example in the manufacture of food or pharmaceutical products intended for dissolution prior to use.

The crystalline maltitol composition of the invention has further advantageous properties. Let us mention its very good compressibility for preparing tablets for chewing or cumulation and its very good miscibility with other products.

The crystalline maltitol composition of the invention may be obtained by spraying a syrup with a relatively high concentration of maltitol, relative to the amount of carbohydrate in the syrup, onto a moving bed of crystalline maltitol particles of purity at least comparable to that of the syrup. It has been shown that the concentration of maltitol in the syrup must be greater than or equal to 92% so that the crystallization of maltitol can take place in a sufficiently short time and efficiently.

This maltitol syrup is generally a perfectly clear maltitol solution, or better, a slightly opaque solution due to the possible but undesirable presence of pure maltitol crystals.

The crystalline maltitol mixture according to the invention can be obtained by a process comprising the following steps: first, a maltitol syrup having a dry matter content of at least 50% by weight is prepared. and having a maltitol concentration greater than or equal to 92%, then the syrup is finely sprayed onto a mobile powder bed of crystalline maltitol particles at a concentration at least equal to that of the syrup, the bed having a temperature in the range of 60-110 ° C; twice the mass of atomized syrup, followed by drying the powder bed and syrup to obtain a crystalline maltitol mixture, then the crystalline maltitol mixture can be aged to sufficient crystallinity, preferably up to a melting enthalpy of greater than or equal to 130 J / g, and finally a crystalline maltitol mixture partially recycled to form a new crystalline maltitol powder bed.

On the contrary, as would be expected, this method makes it possible to obtain a crystalline maltitol mixture of lower density, whose dissolution rate in water is high. These properties can be adjusted by varying the concentration of maltitol in the syrup, the dry matter content of the syrup, the fineness of spraying, the nature of the crystalline maltitol powder-forming particles, the means of moving the particles, the bed temperature, drying temperature and respective powder bed and atomized syrup masses.

For the dependency of the concentration of maltitol in the syrup, it is preferred that it is greater than or equal to 95%, preferably greater than or equal to 98%, with an ideal concentration of about 99%.

It is better to avoid the coarse atomization of the syrup that results from adhesion, insufficient crystallization of maltitol, and too much an increase in density, something that is undesirable. Likewise, in order for the maltitol composition to have these particular, described properties, it is appropriate to use a device which makes it possible to make very fine droplets or even mist from the syrup.

In assessing the nature of the powdered bed particles of maltitol, it is preferred that it also has a high maltitol concentration, at least equal to that of the syrup used. In order to obtain good results, it is also preferred that the bed has an equally low density, i. a density of less than 700 g / l and more preferably less than 650 g / l is ideally used for bedding of maltitol particles having the properties of the crystalline maltitol composition of the invention. This can be achieved by partial recycling of the composition according to the invention, which thus functions as a powder bed of crystalline maltitol. It is very advantageous to proceed in this manner, but then it is better to grind or sieve the composition of the invention so that particles of only less than 50 microns and even better, less than 90 microns are used.

The powder bed particles can be set in motion by mechanical means or by blowing air.

SK 281742-6

The latter is more advantageous since it is easier to select the air temperature, set the bed temperature to a value in the range of 60-110 ° C and adjust the properties of the crystalline maltitol mixture by controlling the air flow.

Generally, it is preferred that the temperature of the bed be maintained in the range of 65-90 ° C, ideally in the range of 70-85 ° C. It is likewise advantageous if the powder bed mass is consistently three or more times the mass of the sprayed syrup. When proceeding by partial recycling of the composition of the invention, which thus functions as a powder bed of crystalline maltitol, it is sufficient to adjust the inlet syrup flow rate to be at most 25% or preferably at most 17% of the inlet flow rate of the recycle mixture.

Drying of the powder bed to which the syrup has been atomized must be carried out so that the final water content does not exceed 2%, preferably 1% and even more preferably 0.5% of the mixture.

The invention demonstrates that it is advantageous to produce a crystalline mixture of maltitol in a continuous process, for example by using an atomization tower of the M.S.D. type from NIRO-ATOMIZER, which, by virtue of its construction, makes it possible to reproduce all essential production steps of the invention.

Finally, the invention allows a very fine spraying of syrup at a temperature in the range of 50-100 ° C by means of a nozzle which the apparatus contains and a dry matter in the range of 55-85% per bed of maltitol particles set in motion and kept in motion by the air stream. In addition, the invention makes it possible to simultaneously carry out hot air drying. Advantageously, an inlet air temperature in the range of 160 to 300 ° C and an inlet mass flow can be selected such that the air temperature exiting the tower is in the range of 60 to 130 ° C, more preferably in the range of 70 to 90 ° C. The invention also allows for an optional method of recycling a portion of the crystalline maltitol mixture and dispersing it very finely in the top of the tower around the syrup spray nozzle.

The crystalline maltitol mixture obtained by the process according to the invention can be subsequently granulated according to the particle size, if desired. The granulation may be carried out in water, steam or a syrup containing preferably maltitol.

The crystalline maltitol mixture of the invention may advantageously be used in cases such as a sweetening agent, filler or texture, excipient or carrier of various additives. Due to its specific properties, it is especially recommended for the production of tablets and powders for dissolution in the food and pharmaceutical sectors.

In any case, the barrier is not to be used for completely different purposes such as chewing gums, syrups or confectionery.

The invention will be better understood by providing examples of embodiments of the invention which are characterized by certain advantageous properties of the crystalline maltitol mixture of the invention. The examples do not have a limiting effect on the subject matter of the invention.

DETAILED DESCRIPTION OF THE INVENTION

Example 1

Preparation of a crystalline mixture of maltitol according to the invention and comparison with prior art products.

A solution of maltitol with a concentration of 75% dry matter is prepared, by dissolving the crystals of maltitol with a concentration of 99.8% maltitol. This solution is heated to 80 ° C and then kept at this temperature.

Atomization of this solution is carried out using a M.S.D. tower of NIRO ATOMIZER. For this purpose, about 100 kg of fine-grained crystalline maltitol powder is pre-metered into the tower into water. For this purpose, crystalline powder MALTISORB P 90, placed on the market by the applicant, is used. The powder serves as a powder bed of crystallized maltitol. This powder is set in motion by air flow at 40-50 ° C and recycled in the upper part of the tower after passing through a sprayer producing particles of crystalline maltitol of less than 90 microns.

The syrup is then finely sprayed onto a mobile powder bed of crystalline maltitol particles by adjusting the flow rate of the feed to the tower such that the amount of such syrup spray is no more than 25% of the amount of recycled atomized maltitol. The drying air temperature is selected at the upper inlet of the tower, which is between 165-225 ° C. The temperature of the air leaving the tower is between 70-90 ° C.

Under these conditions, it has been found that after 7 hours of tower operation, the composition of the maltitol exiting the tower is almost free of particles having shape and appearance properties similar to those found in MALTISORB P 90 powder. In fact, the mixture is substantially porous and honeycomb. and consists of particles substantially spherical without sharp edges and composed of a plurality of interconnected crystalline microparticles. This mixture formed according to the invention was named II. Its basic characteristics are shown in the table.

The procedure for atomizing a maltitol solution with a lower maltitol concentration is also carried out in the same manner as described above. This solution contains 95.8% maltitol and 2.9% other polyols. After 7 hours of tower operation, it was found that the output product was perfectly crystalline and represented all the properties of the crystalline maltitol mixture of the invention. This product is designated as 12. It should be noted that this mixture 12, although its maltitol concentration is rather low, crystallized relatively quickly, perfectly and surprisingly without requiring additional drying and maturation by air evaporation for one to twenty. hours as recommended in US Pat. no. 4,408,041.

The mixtures II and 12 according to the invention were compared with various maltitol powders known from the prior art, i.e.:

- crystalline powder containing maltitol crystals obtained by crystallization in water (MALTISORB P200),

- powder obtained according to the 'solidification' technique (AMALTY of MR TOWA CHEMICAL),

and a maltitol powder extruded according to the conditions described in EP 0 220 103.

The structure of the various products was observed with an optical microscope under polarized light and an electron microscope on granulometric sections from 0 to 100 microns. By observing samples obtained from an optical microscope corresponding to Mix II (Fig. 1), crystalline MALTISORB powder in water, solidified AMALTY MR powder (Fig. 3), and powder extruded (Fig. 4), it was shown that the single solidified AMALTY MR massé powder did not polarize the light, indicating poor crystallinity or a large crystal disorder that the composition II of the invention is essentially formed by spherical particles without sharp edges, which distinguishes very clearly the crystalline powder in water and extruded.

By comparing the obtained electron microscope images of mixture II (Fig. 5), powder crystallized in water (Fig. 6), solidified powder "massé" (Fig. 7) and powder for compressed (Fig. 8), it can be concluded that the crystalline mixture The maltitol according to the invention has a substantially porous and honeycomb structure and contains particles composed of crystalline microparticles joined together. The density of these particles appears to be significantly lower than the density of particles known to date. The prior art particles have in fact a dense and compact structure, with a smooth or rough surface, significantly different from the surface of the particles found in the composition of the invention.

In the table below, some functional properties of the mixtures 11 and 12 according to the invention are given. Compared to the prior art mixtures, the mixtures according to the invention have advantageous properties which have never existed at the same time. They are also compressible, easily flowing and rapidly soluble in water.

Moreover, they appear to be very hygroscopic, which is an undeniable advantage in their storage and use.

table

SUMMARY OF THE INVENTION Compounds of the invention 11 12 Krykalizacia ZVoáy · Print Kaoceetrtcu miHutta κ.ο * K.3K 9S.1 * ¢ 2.0 * M.0 * Obsriwdy OJ * 0.2 * 0.1 * 0.2 * Content i «ý <* polyols ikejc missed aopové moožMvo 2 · * trace nuateve 7.3 ' ο, β * EaUlpiatopoM (* and MO) 102 ^ 1 134 J / Q 133 J / fl 120 Hot frying 14 t ° C 14TC URC 144 ° C URC ŠtnktúN PotfaMtvokí New Ncporéma Additively dense neperá®e nicrduytilické Castke very dense  kooptkaé Ahus Huit • 41 «1 β »β W0 »4 so what· 703 0 » bdMpndoku CTN U.O »4 r> .o 71.0 n.o KýcUoďroqMiťtú ΓΜΙΑΙ 251 30 » 15 » 341 SthadWoO ¹ (TM 02201031) 1SH MN n unlucky Nnsoiué lačcaýsuv 140 N

Example 2

A comparison of a composition of the invention and a prior art composition of US Pat. no. 4,408,401th

'Whole sugar' according to the prior art is prepared by simple atomization of pre-crystallized solutions or calcined amounts of maltitol.

To this end, it is necessary to follow the procedures disclosed in U.S. Pat. No. 4,408,401 using crystalline suspensions having a maltitol content of 98% containing 25 to 60% maltitol crystals.

The properties of the whole sugar thus obtained are compared with the properties of the mixture II and 12 according to the invention of Example 1.

It has been observed that the total sugar representing a dense structure and bulk density, apparently always higher than 700 g / l, the other properties being also very close to the product crystallized in water. Likewise, the dissolution rate in water of these "complete sugars" is close to 70 seconds, and it is not possible to prepare tablets from these products according to the test disclosed in EP 0 220 103, although tableting strength is increasing.

It has been observed that the "total sugar" of the prior art does not represent the physical properties and advantageous functions of the II12 mixtures according to the invention.

Example 3

Prepare a sugar-free gum according to the following instructions

- base rubber 247 g

- Maltitol powder 547 g

- LYCASIN maltitol syrup ^{(R |} 80/55 198 g

- aroma of spearmint 12 g

The following are used as maltitol powder:

- particles having a cross-sectional size of 200 to 315 microns prepared from the mixture II according to the invention and listed in Example 1,

- and particles of a cross-sectional size of 200 to 315 microns obtained from maltitol powder crystallized in water

- MALTISORB P200

Compare the recipe of sugar-free chewing gum obtained under strictly the same conditions using these two maltitol powders.

It has been found by tasting that although the powders used are particularly coarse, the sample according to the invention will give the chewing gum a smoother and distinctly less sandy structure than a sample of maltitol crystallized in water.

It has also been found that the strength of the chewing gum samples containing the sample of the invention is preferably greater than the strength of the samples formed with the prior art sample. This finding is confirmed by measuring the strength by penetrometry using an INSTRON ^(r) .

This comparison confirms the improvement of the chewing gum composition according to the invention when its structure needs to be modified.

The crystalline mixture according to the invention can also be used without difficulty to produce chewing gum wrappers using a powder form or syrup.

PATENT CLAIMS

Claims (10)

A crystalline mixture of maltitol, characterized in that it is substantially porous and honeycomb with a maltitol content of greater than or equal to 92% and a bulk density of 100 to 700 g / l. The crystalline mixture of maltitol according to claim 1, characterized in that the maltitol content is greater than or equal to 95%, preferably greater than or equal to 98% and most preferably equal to or greater than 99%. The crystalline mixture of maltitol according to claim 1 or 2, characterized in that the melt enthalpy is greater than 130 J / g, preferably greater than 145 J / g and even more preferably greater than 155 J / g. The crystalline mixture of maltitol according to any one of claims 1 to 3, characterized in that it contains less than 5% by weight, preferably less than 2% by weight, of the dry matter of polyols other than maltitol. The crystalline mixture of maltitol according to any one of claims 1 to 4, characterized in that it has a bulk density in the range of 200 to 670 g / l, preferably in the range of 300 to 650 g / l and even more preferably in the range of 400 to 650 g / l. A crystalline mixture of maltitol according to any one of claims 1 to 5, characterized in that it has a Carr flow value in the range of 70 to 90, preferably in the range of 75 to 90 and even more preferably in the range of 80 to 90. The crystalline mixture of maltitol according to any one of claims 1 to 6, characterized in that it has a water content of less than 2%, preferably less than 1% and even more preferably less than 0.5%. A crystalline mixture of maltitol according to any one of claims 1 to 7, characterized in that it contains one or more additives selected from strong sweeteners, intensifiers, colorants, perfumes, flavorings, vitamins, minerals, pharmaceutical or veterinary active substances, fatty acid esters. , organic and inorganic acids and their salts, proteinaceous substances such as proteins, amino acids and enzymes. The crystalline mixture of maltitol according to any one of claims 1 to 8, characterized in that its dissolution rate in water according to Test A is less than 30 seconds, preferably less than 26 seconds and even more preferably less than 20 seconds. SK 281742-6 Process for the preparation of a crystalline mixture of maltitol, characterized in that a maltitol syrup having a dry matter content of at least 50% by weight is prepared first. and having a maltitol concentration greater than or equal to 92%, then the syrup is gently atomized into a mobile powder bed of crystalline maltitol particles at a concentration equal to that of the syrup, the bed having a temperature in the range of 60-110 ° C; of the atomized syrup, then the powder bed and syrup are dried to obtain a crystalline maltitol mixture, and then the crystalline maltitol mixture is aged until it has sufficient crystallinity and preferably until it has a melting heat of greater than or equal to 130 J / g. recycles to form a new crystalline maltitol powder bed.