FR3037799A1 - HYDRODISPERSIBLE SOLID PARTICLES BASED ON PROPOLIS - Google Patents

Abstract

Solid propolis-based hydrodispersible particle, characterized in that it contains a carrier comprising water-soluble dietary fibers.

Description

The present invention relates to solid particles, preferably of the granular type, based on propolis which are water-dispersible in water. It also relates to a process for preparing said particles. Propolis is a natural substance made by bees from their secretions and resinous substances collected on certain plants, including conifers and buds of several plant species. This substance is used by bees as a mortar to seal cracks in the hive and ensure its sealing and as an anti-infectious substance to clean the hive, prevent the growth of mold and other pathogens. Propolis contains more than 300 different components including many flavonoids, trace elements and many vitamins. Because of its anti-infectious (antifungal, antiseptic, and antibiotic), healing and anti-inflammatory properties, propolis is widely used in pharmacy, especially for the production of antitussive pharmaceutical compositions or for the ENT or dermatological sphere. It is also used for producing prophylactic compositions, food supplements, or mixed with plants in infusions. It is also an ingredient used for the realization of cosmetics or hygiene products such as soaps, shampoos, creams, skin lotions, toothpastes, etc ...

Because of the current consumer appeal for natural products, it can find many other applications in many areas. After being harvested and purified, propolis is generally supplied in the form of a substantially hydrophobic solid bread, which is therefore very difficult to solubilize in water. This very sparingly soluble form makes its use intact particularly difficult. In order to be integrated into the above-mentioned preparations, the purified propolis bread must be crushed and then dissolved in alcohol at 70 or 90 °. The use of alcohol for producing propolis preparations has many disadvantages.

First of all, the components of the purified starting propolis which are not soluble in alcohol, are not found in the extract obtained and are therefore not present either in the final compositions obtained from this extract. We can not guarantee that all the properties of propolis are preserved. Moreover and above all, the presence of alcohol in propolis preparations is particularly problematic when these preparations are intended for children, pregnant women, or people intolerant to alcohol. It therefore limits its application by excluding a certain number of people who could benefit from it. Finally, the presence of alcohol in these preparations when they are intended for food sometimes imposes the payment of a tax called "alcohol" related to the presence of alcohol in these preparations.

In order to make propolis more easily soluble in water, several solutions have been proposed in the prior art. Thus, for example, patent application CN 112641301 discloses a solid dispersion of propolis with urea and polyethylene glycol.

Also known is CN 102499338 which discloses capsules containing propolis made with cyclodextrin and a fatty acid and polyglycerol ester.

Japanese Patent JP 245,159/90 is also known which teaches the addition of a surfactant in the form of a polyol and fatty acid ester in order to improve the solubilization of propolis. While some of these solutions proposed in the prior art improve the dispersibility in water of the propolis components, they have many disadvantages. Indeed, the process for manufacturing these propolis-based compounds is very complex and difficult to implement. In addition, the finished products obtained most often have an unpleasant taste due to the presence of one or more added emulsifiers or surfactants to solubilize in water.

There is therefore an important demand to provide a purified propolis-based solid product which would be readily water-soluble and which would not have the disadvantages of the products presented in the prior art. Another problem to be solved by the invention is that of developing a product based on propolis incorporating the 5 standards of products from organic farming. Such a product should advantageously have a pleasant taste and be easy to manufacture, handle and transport.

The invention advantageously makes it possible to overcome the drawbacks of the solutions of the prior art and proposes for this purpose a new solid hydrodispersible product based on propolis which is preferentially purified. In order to solve this technical problem, the invention provides a propolis-based propolis-based solid particle, which is characterized by containing a carrier comprising water-soluble dietary fiber. In the specification and in the claims, "soluble dietary fiber" means any fully water-soluble plant cell compound resistant to the different enzymatic hydrolyses involved in the physiological process of digestion. Specifically, the enzymes of the body abundantly present in the small intestine, of the sucrase-maltase type, have no hydrolysis action on the bonds of the units forming the fibers, thus causing no increase in blood sugar, and insulin levels in the blood. These fibers are composed of cellulose, hemicellulose, oligosaccharides, pectin, gums, waxes, these various compounds are those taken into account in dietary fiber analyzes. The soluble fibers are distinguished from sugars or derivatives of sugars, such as for example sucrose, glucose, lactose, maltodextrin, which are easily assimilated sugars fast or slow.

According to the invention, the dietary fibers consist of a polymer that is entirely soluble in water, chosen in particular from the group comprising inulin, oligo-fructoses (also called fructo-oligosaccharides (FOS)), gum d acacia, used alone or as a mixture.

In an advantageous embodiment, the dietary fibers are inulin.

In another embodiment, the support consists exclusively of soluble dietary fibers, in particular inulin. According to a preferred embodiment, propolis is purified propolis.

According to one embodiment variant, the support of the particle according to the invention also contains maltodextrin. According to one embodiment of the invention, the particle is in the form of granules. According to another embodiment of the invention, the particle of the invention contains between 5 and 30%, preferably between 10 and 15% by weight of propolis, the complement to 100% by weight being constituted by the support. The carrier may be exclusively composed of soluble dietary fiber or may further contain maltodextrin. In this case, the maltodextrin represents between 5 and 15% by weight of the support. The invention also teaches the use of a solid particle of this type for producing a pharmaceutical composition, a food supplement, a food preparation, a beverage or a cosmetic product. The invention also teaches the use of a solid particle for producing a syrup, a mono-oral dose, a spray, a ampoule, a tablet, a tablet to suck , a dry orodispersible single dose, a capsule, a capsule, a preparation for dilution, an infusion preparation. The invention finally teaches a process for the manufacture of solid propolis-based hydrodispersible particles, characterized in that, in the absence of a hydrophilic solvent, the propolis and the support comprising food fibers are mixed until a mixture is obtained. softened, the softened mixture is extruded through a die, the filaments resulting from the extrusion are broken up to obtain particles.

According to one embodiment of the process according to the invention, the propolis supplied is purified propolis. According to another embodiment of the process according to the invention, the soluble food fibers and / or the propolis are supplied in pulverulent or ground form. According to another embodiment, the method according to the invention further comprises at least one of the following steps: a heating step, a cooling step, a step of grinding the obtained solid particles, or a sieving calibration step . Other features and advantages of the invention will appear on reading the detailed description which follows, description made with reference to the accompanying drawings, in which: FIG. 1 is a photograph of non-calibrated propolis-based granules according to an exemplary embodiment of the invention; FIG. 2 is a photograph obtained by scanning electron microscopy of the surface of one of the granules visible in FIG.

The photograph of FIG. 1 illustrates an exemplary embodiment of propolis solid particles according to the invention. In an advantageous embodiment, soluble dietary fiber is represented by inulin.

In known manner, inulin is a mixture of oligomers and fructose polymers, which is naturally produced by many types of plants, such as chicory, artichoke, dandelion or Jerusalem artichoke, and which is used by these as a means of storing energy. Inulin is particularly abundant in the chicory root from which it is extracted industrially. The structure of inulin can be represented by the formula GFn, where G is a unit of glycosyl, F is a unit of fructosyl and n is the number of fructosyl units bound.

The degree of polymerization of inulin is variable. Inulin frequently consists of about 60 fructose units, but may also have a much lower molecular weight. When it contains less than 10 units of fructose, it is also called fructo-oligosaccharides (F.O.S.) or oligo-fructose.

Inulin or, more generally, soluble dietary fibers constitute an ideal support for the manufacture of propolis particles, which are water-dispersible and intended to be ingested. They make it possible to include propolis inside a matrix of dietary fibers and thus encapsulate the non-water-soluble propolis. The matrix of 10 dietary fibers perfectly soluble in water, thus confers on the solid particles obtained a satisfactory overall water dispersibility. This principle is illustrated in the photograph of Figure 2 which allows to see the internal structure of the particle through the cracks present on the surface of the granule 15 photographed. There is the presence of substantially spherical microcavities which allow the inclusion of propolis within the matrix of soluble dietary fiber. Propolis is thus fragmented and surrounded by soluble fibers that lead to its dispersion in the presence of water.

The propolis-based particles according to the invention thus lead to a stable suspension by simple dispersion in an aqueous medium of the particles, in the absence of alcohol. The dispersion is obtained at ambient temperature by simple agitation of the medium. Dietary fiber is dissolved in water and propolis is dispersed in water. All the active compounds of the starting propolis is thus restored after dissolution, which preserves all the characteristics and properties of the initial propolis.

In addition, in the solid particles according to the invention, the active compounds of propolis are optimally protected by the dietary fiber and their stability is guaranteed. The organoleptic characteristics and the aromatic profile of propolis are perfectly and completely restored after dispersion.

In an alternative embodiment, the particle according to the invention may contain other components in addition to soluble dietary fiber and propolis, especially maltodextrin, preferably in a lower proportion than the soluble fibers. The added maltodextrin, which is an assimilable sugar by the body, is also soluble in water. It is a carrier material cheaper than certain dietary fibers, in particular inulin and thus, by reducing the amount of inulin required, to reduce the cost, while retaining the essential properties of the invention.

The solid particles according to the invention can be directly consumed in this form after dispersion in an aqueous medium or be incorporated in many galenic forms imaginable by those skilled in the art. In particular, oral forms such as syrups, or drinkable single doses, which can therefore be administered without contraindications to children, pregnant women and persons intolerant to alcohol, can easily be carried out because of the no alcohol. Due to the hydrodispersible nature of the solid particles according to the invention, the propolis they contain is immediately available after ingestion in the presence of saliva. The particles according to the invention are therefore particularly suitable for the production of dry forms such as tablets to be sucked or orodispersible compositions, or for the production of locally applied sprays.

The particles according to the invention are also particularly suitable for producing preparations to be reconstituted by adding water, especially for the reconstitution of hot or cold beverages. There may also be mentioned an application of the invention for the production of products intended to be infused such as herbal teas or tea. In this case, the propolis-based particles according to the invention may be mixed with one or more plants intended to be infused. The particles are preferably provided with a particle size adapted to the size of the plant pieces used. Thanks to the invention, an optimal dispersion of propolis is obtained in the hot water of the infusion and an optimum organoleptic rendering thereof in the mouth.

Many other galenic forms can be envisaged, in particular for example sachets, tablets, capsules, powders, inclusion in pasty forms. The invention also teaches a propolis-based particle manufacturing process above. described. This process essentially consists of extruding a mixture comprising a support based on soluble dietary fibers and propolis in a die without the addition of a hydrophilic solvent.

The process according to the invention is advantageously carried out in the absence of a hydrophilic solvent to prevent the solubilization of the dietary fibers. Hydrophilic solvent is any solvent miscible in water capable of dissolving dietary fiber and especially water.

The first step of the process is to mix the dietary fiber and solid propolis, in the absence of a solvent or other additive, until a softened mass is obtained. It has been observed that this change of state occurs from a relatively low temperature, for example of the order of 60 ° C. Such a temperature makes it possible to preserve all the active principles of propolis without heat-related degradation. The softening temperature being relatively low, it is not necessarily necessary to heat to obtain it, the heating caused spontaneously by the mixing operation may be sufficient.

Likewise, by its operation, the extruder, in or near which this mixture is made, can generate enough heat to cause softening of the mixture. Depending on the equipment used, a temperature of between 30 ° and 130 ° C. can be obtained, it being understood that those skilled in the art will adapt the operating parameters of the extruder so as not to reach a temperature which can distort the properties of the extruder. propolis. An operating temperature of the order of 70 ° C may be preferentially retained. Nevertheless, additional heating can be provided when needed to achieve softening of the mixture.

To achieve mixing, the food fiber can advantageously be provided in a powder form. The pulverulent form can indifferently correspond to an atomized or micronized form from natural fibers. Indeed, the state of the specific surface of the fibers is of little importance insofar as the material undergoes a change of state 5 causing the particles to lose their basic structure during softening. Propolis, preferably purified propolis, is also preferably previously reduced to powder or ground to facilitate mixing. Propolis and soluble fiber can be mixed before the temperature rise. In another embodiment, the propolis may be incorporated into the soluble fiber by adding in proportion as the temperature rise to the softened state. Due to the change of softening state which occurs with a low temperature rise, it is possible to overcome the presence of water or other hydrophilic solvents to achieve mixing and extrusion. In the next step of the process, the mixture of propolis and soluble dietary fiber is extruded through a die, while the mixture is still in the softened state. The size of the die is of course chosen according to the desired size of the particles that one wishes to obtain. As the die exits, the filaments cool in contact with the ambient air. The resulting filaments are then appropriately fragmented to obtain the desired size solid particles. This division step may be performed by different methods, such as, for example, grinding or crushing. A sieving step closes the process. The particles obtained after extrusion and cooling have a high cohesion and a high hardness, much higher than that of natural soluble fibers.

This important hardness advantageously makes it possible to fractionate and calibrate them, in a wide range and on demand, without any problem of friability. The particles can then be directly used or calibrated and packaged without excessive loss of material.

According to one embodiment of the invention, the particles are in the form of granules and have a size of between 0.1 and 3 millimeters, advantageously between 0.3 and 2 millimeters. Of course, the sizes mentioned above correspond to an average size over all the granules obtained.

The invention and the advantages thereof will become more apparent from the following exemplary embodiments. EXAMPLE 1: PRODUCTION OF A PROPOLIS CHILD SYRUP WITHOUT ALCOHOL Preparation of propolis granules: In an extruder, 88% by weight of inulin in powder form and 12% by weight of propolis resin were introduced and mixed. purified ground. Mixing the two products generated a rise in temperature to about 70 ° C which caused the mixture to soften. The softened mixture was extruded through a 2 mm die and the resulting filaments were fractionated by rotary knives placed at the die exit, to form granules. The granules were then cooled. Preparation of the syrup: In a tank equipped with a stirring system, the following solution was prepared: Water: 40 Kg Propolis granules (prepared above): 10 Kg After complete dissolution, it was added successively with stirring the following compounds: Aqueous extract of pollen: 2.00 Kg 30 Dry extract of acerola titrated with 25% vitamin C: 1.00 Kg Honey: 45.00 Kg Liquid fructose: 4.50 Kg Natural flavor red fruits: 0.10 Kg Water in sufficient quantity to 100,00 Liters.

The pH was adjusted to 5 with citric acid. The mixture was then pasteurized and filtered, and then packaged in glass vials. EXAMPLE 2 Manufacture of a PROPOLIS 5 ALCOHOL-FREE COLLUTORY SPRAY Preparation of the propolis granules: The propolis granules were prepared as in Example 1.

Preparation of the spray: In a first tank, the following solution No. 1 was prepared with stirring: Honey: 28.00 kg Glycerine: 28.00 kg Hydroglycerine extract of blackcurrant buds: 2.50 kg Hydroglycerine extract of calendula: 2.50 Kg In a second vat, the following solution No. 2 was prepared with stirring: Water: 30.00 liters Potassium sorbate 0.10 Kg 20 Sodium benzoate 0.10 Kg Propolis granules (prepared below) above): 10.00 Kg Solutions No. 1 and No. 2 were mixed in a final preparation vat and water was added in sufficient quantity per 100.00 Liters.

The pH was adjusted to 5 with citric acid. The mixture was then pasteurized and filtered, and then packaged in 30 ml glass bottles with metering pump and spray tip. EXAMPLE 3: MANUFACTURE OF PROPOLIS ORODISPERSIBLE TABLETS FOR LOCAL SPHERE ENTRIES Preparation of propolis granules: In an extruder, 88% by weight of inulin in pulverulent form and 12% by weight of resin were introduced and mixed. of purified purified propolis.

The mixing of the two products generated a rise in temperature to about 70 ° C which caused the mixture to soften. The softened mixture was extruded through a 4 mm die and the resulting filaments were fractionated by rotary knives placed at the die exit, to form granules.

The granules were then cooled and milled in an oscillating knife mill. Finally, sieving was carried out at a size of between 500 and 1000 micrometers.

Preparation of the tablets: Tablets having a diameter of 20 mm, a thickness of 5 mm and a weight of 2 grams, containing: propolis granules (prepared above) 97, were prepared by direct compression on a rotary tablet. 50% Carboxy-methylcellulose 2.00% Magnesium stearate 0.50% EXAMPLE 4: PRODUCTION OF PROPOLIS INFUSION Preparation of the propolis granules: The propolis granules were prepared as in Example 3 except that size selection by sieving was carried out at a size between 500 and 1500 micrometers.

Preparation of infusion: The propolis granules obtained were incorporated in a mixture of cut plants having a particle size of between 500 and 1800 micrometers, in the proportions. The mixture obtained was packaged in 2-gram unit doses in sachets 35 for infusion. following: Thyme leaves: 60% Badiane fruit: 25% Cinnamon bark: 5% Propolis pellets (prepared above): 10%

Claims (5)

CLAIMS1 / propolis-based solid propolis particle, characterized in that it contains a carrier comprising water-soluble dietary fiber. 2 / particle according to claim 1, characterized in that the dietary fibers consist of a fully water-soluble polymer selected from the group consisting of inulin, oligo-fructose (also called fructo-oligosaccharides (FOS)), acacia gum, used alone or as a mixture. 3 / particle according to claim 1, characterized in that the dietary fiber is inulin. 4 / Particle according to one of the preceding claims, characterized in that the support consists exclusively of soluble dietary fiber. 5 / particle according to one of claims 1 to 3, characterized in that the carrier further contains maltodextrin. 6. Particle according to one of the preceding claims, characterized in that the propolis is purified propolis. 7 / Particle according to one of the preceding claims, characterized in that it is in the form of granules. 8 / particle according to any one of the preceding claims, characterized in that it contains between 5 and 30%, preferably between 10 and 15% by weight of propolis, the complement to 100% by weight being composed of the support. 9 / Particle according to claim 8, characterized in that the carrier contains between and 15% by weight of maltodextrin. 10 / Use of a particle according to any one of the preceding claims, for the production of a pharmaceutical composition, a food supplement, a food preparation, a beverage, a cosmetic product. 11 / Use of a particle according to any one of the preceding claims, for the production of a syrup, a mono-oral dose, a spray, a ampoule, a tablet, of a sucking tablet, of an orodispersible dry mono-dose, of a capsule, of a capsule, of a preparation to be diluted, of an infusion preparation. 12 / A process for producing solid propolis-based hydrodispersible particles, characterized in that, in the absence of hydrophilic solvent: propolis is mixed with the support comprising dietary fibers until a softened mixture is obtained, extruded the mixture softened through a die, the filaments resulting from the extrusion are broken up to obtain particles. 13 / A method of manufacture according to the preceding claim, characterized in that the propolis and the dietary fiber are supplied in powder form or ground.