WO2012154018A1 - Activated, micronized zeolite, method for activating and micronizing same and use thereof as a carrier in pharmaceutical preparations and dietary supplements - Google Patents

Abstract

The invention relates to an activated, micronized natural zeolite, to the use thereof as a carrier for herb and fruit extracts, vitamins, organic and synthetic molecules and animal derivatives, and to the use thereof in pharmaceutical preparations and dietary supplements. Specifically, the invention relates to an activated, micronized natural zeolite, which has: a particle size of 1 to 15 micrometres, a surface area of 20 to 30 m²/g and thermal activation at a temperature of 250 ºC to 400 ºC for 2 to 4 hours. In addition, the loading of the herb and fruit extracts, vitamins, organic and synthetic molecules and animal derivatives, which are encapsulated in the pores of the activated, micronized zeolite and/or in the surface thereof, is carried out by a tribochemical reaction process under dry conditions in a high-intensity turbo mixer and/or a tribochemical reaction process under wet conditions in a multiple colloid mill. The carrier of the present invention can be used for the production of pharmaceutical preparations and dietary supplements in the form of tablets, hard capsules, soft capsules, suspensions, etc.

Description

 ZEOLITE ACTIVATED AND MICRONIZED, PROCESS FOR YOUR

 ACTIVATION AND MICRONIZATION AND ITS USE AS A CREDITOR IN PHARMACEUTICAL PREPARATIONS AND FOOD SUPPLEMENTS

FIELD OF THE INVENTION

 The invention relates to a natural activated and micronized zeolite and its use as a carrier of herbal, fruit extracts, vitamins, organic and synthetic molecules and animal derivatives. Particularly, the activated and micronized natural zeolite has a particle size of 1 to 15 microns and a surface area of 20 to 30 m2 / g.

BACKGROUND OF THE INVENTION

 In June 2001, U.S. Pat. No. 6,241, 975 describes a method of preparing an extract of powdered pine salt comprising:

 a) .- Mix 20 g of the pine leaf extract and refined salt with 200 g of purified water.

 b) .- Load the extract of the pine leaf and refined plant salt into the porous powder carrier, by adding 200 g of precipitated silica (carrier) of a particle size of 400 microns and keep it with stirring until saturation.

 c) .- After adding 200 g of carnauba wax, continue mixing and heat it to a temperature of 85 to 95 ° C. Thus, 398 g of powder were obtained from coated pine salts.

However, natural zeolite is not mentioned at any time activated and micronized as carrier of herbal, fruit, vitamins, organic and synthetic molecules and animal derivatives etc. nor is a particle size of 1 to 15 microns mentioned, nor a surface area of 20 to 30 m2 / g; nor is a tribochemical reaction process treated in a high intensity dry turbo mixer treated and a tribochemical reaction process treated in a wet condition in a multiple colloid mill.

 In December 2002, world patent number WO02100420 describes the use of a chemically activated natural zeolite (clinoptilolite) with zinc and loaded with erythromycin for the treatment of acne comprising:

 a) .- Grind the zeolite to a size smaller than 150 microns.

 b) .- Chemical activation of zeolite to a sodium form, by adding a 1M solution of NaCl to a solid / liquid radius of 35mg / ml. c) .- Chemical activation of zeolite to a form of zinc, by adding a 0.5M solution of ZnS047H20.

 d) .- Wet micronization of the zeolite activated with zinc, (2g of powder; in 15 ml of deionized water; 15 minutes of grinding).

 e) .- The erythromycin charge was carried out by evaporation of a solution of erythromycin in ethanol, in which the micronized carrier had previously been dispersed and loaded with zinc.

However, this patent exclusively describes the use of chemically activated zeolites with zinc and loaded with erythromycin for the preparation of pharmaceutical compositions for topical application. At no time is the activated and micronized natural zeolite mentioned as carrier of herbal extracts, fruit, vitamins, organic and synthetic molecules and animal derivatives etc .; nor is a particle size of 1 to 15 microns mentioned, nor a surface area of 20 to 30 m2 / g; nor is a tribochemical reaction process treated in a high intensity dry turbo mixer treated and a tribochemical reaction process treated in a wet condition in a multiple colloid mill.

 In April 2009, U.S. Patent No. 20090098208 describes synthetic zeolites from the group of faujasites of type X or ALSX, which are used in pharmaceutical compositions as carriers for pharmacologically active molecules such as: diclofenac, ketorolac, ibopruphene, naproxen, ketoprofen and comprising:

 a) .- An activation treatment comprising heating the synthetic zeolite X or ALSX at a temperature of 200 to 600 ° C.

 b) .- A warm-up time of 3 to 4 hours

 c) .- The loading of the synthetic zeolites X or ALSX with the pharmacologically active molecules is effected by impregnating the zeolites with solutions of these molecules in one or more solvents and the subsequent evaporation of the solvent (s). The impregnation is effected by dispersion under stirring at a temperature of 25 to 30 ° C for a time of 36 to 48 hours.

 d) .- Synthetic zeolites X or ALSX impregnated with pharmacologically active molecules are subsequently separated by solvent filtration or solvent mixtures. Once separated, the synthetic zeolites X or ALSX impregnated with the pharmacologically active molecules are dried under vacuum in a rotary evaporator.

However, this patent exclusively describes the use of zeolites Synthetic X or ALSX as carriers for pharmacologically active molecules such as: diclofenac, ketorolac, iboprufen, naproxen, ketoprofen, etc. At no time is the activated and micronized natural zeolite mentioned as a carrier of herbal extracts, fruit, vitamins, organic and synthetic molecules and animal derivatives, etc .; nor is a particle size of 1 to 15 microns mentioned, nor a surface area of 20 to 30 m2 / g; nor is a tribochemical reaction process treated in a high intensity dry turbo mixer treated and a tribochemical reaction process treated in a wet condition in a multiple colloid mill.

BRIEF DESCRIPTION OF THE INVENTION

 The invention relates to an activated and micronized natural zeolite and its use as a carrier of herbal, fruit extracts, vitamins, organic and synthetic molecules and animal derivatives and its application in pharmaceutical preparations and food supplements comprising: a) .- Micronization of the natural zeolite,

 b) .- Thermal activation of the micronized natural zeolite,

 c) .- The loading of herbal, fruit, vitamins, organic and synthetic molecules and derivatives of animals encapsulated within the pores of the activated micronized zeolite and / or on its surface by:

1) .- Tribochemical reaction process, treated in dry condition in a turbo mixer of high intensity, between the mixture of activated and micronized zeolite and the herbal extract, fruit, vitamin, organic and synthetic molecule and animal derivative selected from: Standardized herbal extracts of: Echinacea, Ginkgo biloba, Astragalus, Nettle, Green tea, etc .; Excerpts Standardized fruit trees of: Cranberry, grape seed, red raspberry, plum, cherry, strawberry, lycopene, etc .; Vitamins: A, B1, B2, B6, B8, B12, C, D3, E, etc .; Organic molecules: Amino acids, etc. Synthetic molecules: PEAK ATP® (5 'adenosine triphosphate) Animal derivatives: Royal jelly, propolis, bovine colostrum, whey protein, etc.

 2) .- Tribochemical reaction process, treated in a wet condition in a multiple colloid mill, between the aqueous suspension of the activated and micronized zeolite and the herbal, fruity, vitamin, organic and synthetic molecule extract and animal derivative selected from: Extracts standardized herbs of: Echinacea, Ginkgo biloba, Astragalus, Nettle, Green tea, etc .; Standardized fruit extracts of: Blackberry, grape seed, red raspberry, plum, cherry, strawberry, lycopene, etc .; Vitamins: A, B1, B2, B6, B8, B12, C, D3, E, etc .; Organic molecules: Amino acids, etc. Synthetic molecules: PEAK ATP® (5 'adenosine triphosphate); Animal derivatives: Royal jelly, propolis, bovine colostrum, whey protein, etc.

DETAILED DESCRIPTION OF THE INVENTION

The invention relates to an activated and micronized natural zeolite and its use as a carrier of herbal, fruit, vitamin, organic and synthetic extracts and derived from animals selected from: Standardized herbal extracts of: Echinacea, Ginkgo biloba, Astragalus, Nettle, Te green, etc .; Standardized fruit extracts of: Blackberry, grape seed, red raspberry, plum, cherry, strawberry, lycopene, etc .; Vitamins: A, B1, B2, B6, B8, B12, C, D3, E, etc .; Organic molecules: Amino acids, etc. Synthetic molecules: PEAK ATP® (5 'adenosine triphosphate) Animal derivatives: Royal jelly, propolis, bovine colostrum, whey protein, etc. and his Application in pharmaceutical preparations and food supplements comprising:

 a) .- Micronization of the natural zeolite, the natural zeolite is micronized in a micronizer mill, whose rotors are propelled at high revolutions and countercurrent, conditions that are desirable for a fine grinding of the material. Subsequently, the micronized material is classified by means of a turbo classifier until a particle size of 1 to 15 microns and a surface area of 20 to 30 m2 / g is obtained.

 For the realization of the invention, a natural zeolite of the clinoptilolite / heulandite type was used with the following composition:

 Component% by weight

 Si02 65.50 to 70.50%

 AI203 1 1.50 to 13.50%

 CaO 2.50 to 3.50%

 K20 3.20 to 4.50%

 Fe203 1 .00 to 2.50%

 MgO 0.50 to 1.50%

 Na20 0.20 to 1 .50%

 ΤΊ20 0.10 to 0.30%

 Drying losses @ 100 ° C 2.50 to 3.50%

 Losses from calcination @ 1000 ° C 7.50 to 9.0% b) .- Thermal activation of the micronized natural zeolite, thermal activation of the micronized natural zeolite is carried out by heat treating the zeolite at a temperature of 250 ° C for 2 hours .

c) .- The load of herbal extracts, fruit, vitamins, molecules organic and synthetic and animal derivatives, encapsulated within the pores of the activated and micronized zeolite and / or on its surface by:

 c.1) .- Tribochemical reaction process, treated in dry condition in a turbo mixer of high intensity, between the mixture of activated and micronized zeolite and the herbal, fruity extract, vitamins, organic and synthetic molecules and animal derivatives selected at a speed from 875 to 1750 rpm for 15 minutes.

 c.2) .- Tribochemical reaction process, treated in a wet condition in a multiple colloid mill, between the suspension of the activated and micronized zeolite and the herbal, fruit extract, vitamin, organic and synthetic molecule and animal derivative selected at a rate from 1750 to 3500 rpm for 15 minutes.

Preparation of Compounds according to the Invention:

 The best way to carry out the invention is to mix the components in the following way:

 a.1) .- In a turbo mixer the activated and micronized and thermally treated zeolite is added, then the herbal, fruit extract, vitamin, organic and synthetic molecule and selected animal derivative are added. a.2) .- Subsequently the tribochemical reaction is carried out by means of the turbo mixing of the components at a speed of 1750 rpm for 15 minutes.

a.3) .- The final product obtained through the tribochemical process shows a homogeneous powder of a "zeolite" with herbal extracts, fruit, vitamins, organic and synthetic molecules and animal derivatives, encapsulated within the pores of the activated zeolite and micronized and / or in its surface

 b.1) .- In a multiple colloid mill the suspension of the activated and micronized and thermally treated zeolite is added, then the herbal, fruity extract, vitamin, organic and synthetic molecule and selected animal derivative are added.

 b.2) .- Subsequently the tribochemical reaction is carried out by means of the turbo mixing of the components at a speed of 3500 rpm for 15 minutes.

 b.3) .- The final product obtained through the tribochemical process shows a homogeneous suspension of a "zeolite" with herbal extracts, fruit, vitamins, organic and synthetic molecules and animal derivatives, encapsulated within the pores of the activated zeolite and micronized and / or on its surface.

 The main advantage of the process of the invention is that a pharmaceutical preparation and / or nutritional supplement can be obtained with the encapsulated assets and / or on the surface of the zeolite quickly and effectively.

 The conditions in the turbo mixer and in the multiple colloid mill, provide good contact between herbal, fruit extracts, vitamins, organic and synthetic molecules and animal derivatives and the interchangeable cations in the hydration zone that begin the chemical reaction of the mineral, forming a zeolite with assets encapsulated within the pores of the activated and micronized zeolite and / or on its surface.

The high intensity mechanical energy released by the turbo mixer and the multiple colloid mill activates layers of hydrated molecules of water around the exchangeable cation, promoting good Conditions for the chemical reaction between activated and micronized zeolite and herbal, fruit, vitamin, organic and synthetic molecules and animal derivatives.

 EXAMPLE

 The following preparation was performed according to the processes described above, using the composition indicated in Table A.

 TABLE A

 Compound Formulation: ZAM + Cranberry Extract Ingredients Witness * Invention

ZAM (activated and micronized zeolite) 400.00 g 400.00 g

 Blackberry Extract 160.00 g 160.00 g

 * Normal mixing in homogenizer

The properties of the compound were evaluated as follows:

 To check the encapsulation within the pores of the activated and micronized zeolite and / or on its surface of the fruit extract, gravimetric determination tests were performed.

 The results are shown in Table B.

TABLE B

 % of encapsulated and / or surface extract

Test Witness * Invention% of Encapsulated Extract 27.25 97.35

* Normal mixing in homogenizer To determine the changes in the surface area, surface area tests (BET Method) were performed before and after the tribochemical reaction, which shows the decrease in the surface accessible to nitrogen gas. The above shows us that the cranberry extract has remained inside the pores and on the surface of the zeolite. The results are shown in Table C.

TABLE C

 Surface area of compound (BET method) Test Witness * Invention

 Surface area (m2 / g) (BEFORE) 22.5 22.5

 Surface area (m2 / g) (AFTER) 19.7 7.2

^* Normal mixing in homogenizer The present invention is not limited by the particular characteristics that have been specified or by the details of the example chosen to illustrate it. Many modifications can be made to the particular characteristics and to the example, which has been described to illustrate the components that constitute it, thereby without departing from the scope of the invention.

Having sufficiently described my invention, I consider as a novelty and therefore claim of my exclusive property, the content of the following:

Claims

 1.- An activated and micronized natural zeolite as a carrier of herbal, fruit, vitamin, organic and synthetic molecules and animal derivatives, characterized in that it comprises:  Component% by weight  Si02 65.50 to 70.50%  AI203 1 1.50 to 13.50%  CaO 2.50 to 3.50%  K20 3.20 to 4.50%  Fe203 1.00 to 2.50%  MgO 0.50 to 1.50%  Na20 0.20 to 1.50%  ΤΊ20 0.10 to 0.30% 2. An activated and micronized natural zeolite according to claim 1, characterized in that it comprises:  a) .- a particle size of 1 to 15 microns,  b) .- a surface area of 20 to 30 m2 / g,  3. - An activated and micronized natural zeolite according to claim 1, characterized in that the activated and micronized natural zeolite is selected from the group of clinoptilolite-heulandite.  4. - A process for the preparation of an activated and micronized natural zeolite for use as a carrier according to claim 1, characterized in that it comprises: a) .- micronization of the natural zeolite, the natural zeolite is micronized in a micronizer mill, whose rotors are propelled at high revolutions and countercurrent, conditions that are desirable for a very fine grinding of the material, subsequently, the micronized material is classified by a turbo classifier until obtaining a particle size of 1 to 15 microns and a surface area of 20 to 30 m2 / g;  b) .- thermal activation of the micronized natural zeolite, the thermal activation of the micronized natural zeolite is performed by heat treating the zeolite at a temperature of 250 ° C for 2 hours;  c) .- load the herbal, fruit, vitamins, organic and synthetic molecules and animal derivatives extracts, encapsulated within the pores of the activated and micronized zeolite and / or on its surface.  5. The process for the preparation of an activated and micronized natural zeolite according to claim 4, characterized in that the step (c) for loading the extracts comprises:  c.1) .- a tribochemical reaction process, treated in a dry condition in a high intensity turbo mixer, between the mixture of activated and micronized zeolite and hecbal extract, fcutal, vitamins, organic and synthetic molecules and selected animal decivated at a speed of 875 at 1750 rpm for 15 minutes;  c.2) .- a tribochemical reaction process, treated in a wet condition in a multiple colloid mill, between the suspension of activated and micronized zeolite and the herbal, fruity, vitamin, organic and synthetic molecule extract and animal derivative selected to a speed from 1750 to 3500 rpm for 15 minutes. 6. - The use of an activated and micronized natural zeolite according to claims 1 to 3, as a carrier of active ingredients for the preparation of pharmaceutical preparations and food supplements. 7. The use of an activated and micronized natural zeolite according to claims 1 to 3, as a carrier for use in the preparation of pharmaceutical preparations and food supplements in the form of tablets, hard capsules, soft capsules, suspensions, etc.  8. An activated and micronized natural zeolite, prepared in accordance with the process claimed in claims 4 and 5, for use as a carrier of active ingredients for the preparation of pharmaceutical preparations and food supplements.  9. An activated and micronized natural zeolite, prepared in accordance with the process claimed in claims 4 and 5, for use as a carrier for use in the preparation of pharmaceutical preparations and food supplements in the form of tablets, hard capsules, soft capsules, suspensions, etc.