Classifications

• • A—HUMAN NECESSITIES
  • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
  • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
  • A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
  • A23L3/40—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by drying or kilning; Subsequent reconstitution
  • A23L3/44—Freeze-drying
• • A—HUMAN NECESSITIES
  • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
  • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
  • A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
  • A23L3/36—Freezing; Subsequent thawing; Cooling
  • A23L3/37—Freezing; Subsequent thawing; Cooling with addition of or treatment with chemicals
  • A23L3/375—Freezing; Subsequent thawing; Cooling with addition of or treatment with chemicals with direct contact between the food and the chemical, e.g. liquid nitrogen, at cryogenic temperature
• • A—HUMAN NECESSITIES
  • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
  • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
  • A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
  • A23L3/40—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by drying or kilning; Subsequent reconstitution
  • A23L3/42—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by drying or kilning; Subsequent reconstitution with addition of chemicals before or during drying
• • A—HUMAN NECESSITIES
  • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
  • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
  • A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
  • A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
  • A23L33/105—Plant extracts, their artificial duplicates or their derivatives
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K8/00—Cosmetics or similar toiletry preparations
  • A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
  • A61K8/0241—Containing particulates characterized by their shape and/or structure
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K8/00—Cosmetics or similar toiletry preparations
  • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
  • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
  • A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
  • A61K8/35—Ketones, e.g. benzophenone
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K8/00—Cosmetics or similar toiletry preparations
  • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
  • A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
  • A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
  • A61K8/9728—Fungi, e.g. yeasts
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K8/00—Cosmetics or similar toiletry preparations
  • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
  • A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
  • A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
  • A61K8/9783—Angiosperms [Magnoliophyta]
  • A61K8/9794—Liliopsida [monocotyledons]
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K8/00—Cosmetics or similar toiletry preparations
  • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
  • A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
  • A61K8/99—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from microorganisms other than algae or fungi, e.g. protozoa or bacteria
• • A—HUMAN NECESSITIES
  • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
  • A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
  • A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs

Definitions

• the invention relates to the field of products in the form of dry powders obtained by lyophilization. More particularly, the invention relates to a lyophilization process comprising a prior step of cryogenics under pressure of a matrix containing dissolved gas. It also relates to the powder obtained by this process as well as its uses in food processing, cosmetics, pharmacy and in human and animal health.
• Lyophilization is a process of dehydration by sublimation of water under conditions of temperature and pressure allowing the water contained in solid form in the products to be transformed directly into water vapor for elimination. The process therefore involves treating products which have been previously frozen, so that the water contained is solid. This freezing generally takes place around 0 ° C. A lower temperature may be necessary depending on the composition of the product (presence of sugar or salt in food preparations for example). Lyophilization is carried out at temperatures considered to be low (below -20 ° C), making it possible to limit the degradation of the organoleptic properties of the products and of the active ingredients they contain. However, the first step, freezing or deep-freezing, causes alterations that it would be desirable to reduce.
• Patent KR20190005308A proposes a modification of the lyophilization process to reduce the final water content contained in the products, while patent CN109156511A proposes to carry out the vacuum deep freezing step so as to improve the quality and stability in the products. the time of freeze-dried jackfruit.
• Document KR2019 / 0071382 describes a process for producing a freeze-dried food having improved health functional properties by increasing the content of active ingredients, such as vitamins in fruits or vegetables, using cryogenic cooling and freezing.
• the process is characterized by the steps of: bringing a dried product containing fruits or vegetables into contact with a liquefied gas cooled to -190 to -80 ° C for 0.5 to 30 minutes to cool the product cryogenically; supplying the dried material which has been cooled to a vacuum dryer and vacuum drying at room temperature; immerse vacuum-dried material in nutrient solution; And lyophilize the dried food immersed in the nutrient solution at a temperature of -50 to -20 ° C to prepare a lyophilized food.
• Document US2019 / 133150 describes a process for producing a powder containing proteins. This method comprises the steps of: providing a raw material containing a protein; freezing the raw material containing proteins between -196 ° C and -80 ° C; and grinding the protein-containing raw material to obtain the protein-containing powder, wherein an average particle size of the protein-containing powder is smaller than a cell size of the protein-containing raw material.
• application WO2008 / 043909 discloses a method implementing two successive steps consisting in dissolving gas in a more or less viscous liquid matrix by bringing into contact of said matrix with an atmosphere of which the partial gas pressure is greater than 2 bars and then in cryogenization, under the same pressure conditions as during the first step, the matrix containing the gas dissolved dropwise in a cryogenic fluid at l liquid state.
• the advantage of this process lies mainly in the properties provided to the final product, both during storage and during re-use.
• the properties provided let us cite for example the development of protection against oxidation during storage on the one hand and the formation of foam during reheating on the other hand.
• document WO2019 / 234341 describes a process for obtaining a product in the form of granules, particles or frozen balls, from a liquid, semi-liquid or pasty matrix, comprising the steps of gasifying the matrix by dissolving a gas, dispensing the matrix in the form of drops and cryogenizing the matrix drops by immersion in a cryogenic fluid.
• Patent application US2017 / 049126 illustrates the general principles of these processes in which the beads or granules are formed by flow from a shower, then drop into a cryogenic fluid before being extracted therefrom by a sieve or a filter.
• the cryogenic fluid can be set in motion by gravity flow or using a pump, for example.
• Lyophilization is a long and expensive process that consumes a lot of energy.
• none of the cryogenic solutions proposed to date have made it possible to significantly improve the properties of the lyophilized products.
• most of the solutions proposed are based on a vacuum applied during the freezing phase and no technique has envisaged the application of an excess pressure during this step.
• the inventors have developed a new process for preparing dehydrated products in which a gas is dissolved in the matrix before deep freezing by pressurizing and the deep freezing step prior to lyophilization is also carried out under pressure.
• the invention relates to a process for preparing a dehydrated product consisting of:
• a) have a product in the form of a liquid, semi-liquid or pasty matrix; b) dissolving a gas in said matrix by passing through a zone dense in gas molecules, such a density being obtained (i) either by virtue of the gas flow generated by the evaporation of a cryogenic fluid, (ii) either by a rise in pressure, (iii) or by a combination of the two;
• step b) cryogenizing said gas-rich matrix obtained in step b) at a pressure making it possible to maintain said dissolved gas in order to obtain frozen granules, particles or beads;
• the invention also relates to a powder obtained according to the process of the invention which has very advantageous properties, as well as the uses of such a powder in sectors such as the food industry, cosmetics, pharmaceuticals and human health and animal.
• the invention also relates to equipment for implementing said method comprising a cryogenic chamber in which a pressure greater than or equal to atmospheric pressure is maintained and a lyophilizer.
• the invention aims to remedy the existing problems by proposing a process and associated equipment for making it possible to obtain a product in dehydrated form; this process consists first of all in dissolving a gas in a liquid, semi-liquid or pasty matrix by passage through a gas flow and / or under pressure, then in deep freezing this matrix via a deep freezing process under pressure in contact with 'a cryogenic fluid, so as to maintain the gas in large quantity in the matrix.
• the frozen matrix is then lyophilized.
• the pressurized cryogenics step allows substantial improvements in both drying and the properties of the products produced.
• Cryogenics is an almost instantaneous process, making it possible to continuously produce and at high rates (several hundred kg per hour on standard equipment) balls of initially fluid product.
• the time saving is considerable compared to freezing in a cold room, even if they operate at very low temperatures (-40 ° C to -80 ° C in general).
• Cryogenic beads are extracted from equipment producing them at temperatures generally between -80 ° C and -120 ° C, which makes it possible to start freeze-drying directly, with products whose temperature is around -60 ° C, without a prior cooling step.
• the lyophilization time itself is very greatly reduced (up to a factor of at least 2).
• the duration of the process as a whole is significantly reduced.
• the use of the process according to the invention makes it possible to obtain products in the form of high quality powder, without the “edge / core effect” usually obtained when the lyophilization is carried out on plates.
• product which induces a drying gradient and damaged matrices on the exteriors of the plates (usually called "cake").
• cake the spherical shape of the frozen matrix and the presence of gas allow homogeneous dehydration without alteration; the product is therefore of better quality.
• the lyophilized powders obtained from cryogenized products containing dissolved gas are much more porous than those obtained from conventionally frozen products.
• the quality of the dehydrated products is therefore higher than that of the freeze-dried products obtained by a conventional process because the conditions used in this process are on the whole softer, less aggressive and less destructuring for the matrix.
• cryogenized beads containing dissolved gas make it possible to obtain, whatever the pressure applied and after freeze-drying, a fine powder, which can be handled simply because it can be measured and not sticky.
• the resulting powder does not pick up moisture easily when left in ambient conditions.
• the freeze-drying of frozen products in a conventional manner only makes it possible to obtain agglomerates of product, which must generally be reprocessed (by grinding for example) to facilitate, or even allow, their use.
• the powders are very fine, of very low bulk density and do not require grinding before use. They can, if necessary, be compacted for ease of use.
• the dehydrated powders according to the invention dissolve quickly and leave no deposit.
• the method according to the invention and the equipment used also make it possible to improve the preservation of the integrity of the starting matrix, in particular in terms of its physicochemical properties.
• the organoleptic properties are significantly improved compared to the lyophilized products obtained by the methods of the prior art.
• the gas is an inert gas and, more particularly, is not oxygen, oxidation reactions are avoided.
• the inert gases once dissolved in the matrix, protect the integrity of the structures and preserve the properties of the matrices, in particular the organoleptic properties of the food matrices and the living properties of the cellular matrices.
• a first object of the invention relates to a process for preparing a dehydrated product consisting of:
• a) have a product in the form of a liquid, semi-liquid or pasty matrix; b) dissolving a gas in said matrix by passing through a zone dense in gas molecules, such a density being obtained (i) either by virtue of the gas flow generated by the evaporation of a cryogenic fluid, (ii) or by a increase in pressure, (iii) or by a combination of these two means;
• step b) cryogenizing said gas-rich matrix obtained in step b) at a pressure making it possible to maintain said dissolved gas in order to obtain frozen granules, particles or beads;
• the pressure making it possible to maintain said gas dissolved in the matrix during the cryogenic stage is generally a pressure greater than or equal to atmospheric pressure.
• the dissolved gas can be an inert gas such as nitrogen, argon, helium ... or another gas such as oxygen, or C02 for example used in sparkling drinks or protoxide of nitrogen used for its foaming power. It is also possible to use a mixture of gases depending on the desired properties. The use of inert gas is preferred when it is desired to avoid oxidation of the matrix, and therefore to preserve the properties of the starting matrix.
• zone dense in gas molecules or “zone dense in molecules” within the meaning of the invention, is meant a zone in which the number of molecules per unit of volume is higher than that which would be observed at atmospheric pressure. As this volume is not closed and can in particular constitute a subunit of a larger volume, the high number of molecules found there does not necessarily translate into a visible increase in the pressure of the assembly. It is also possible to consider it as a local but non-measurable pressure, this pressure being formed by the combination of the possible pressure applied to the assembly and the effect induced by the density of molecules generated.
• the quantity of gas dissolved in the matrix depends on the control of said flow and it is typically equivalent, when no pressure is applied, to that which would be obtained by applying relative pressures of between 0.001 bars and 2 bars.
• a particularly preferred cryogenic fluid in this case is liquid nitrogen.
• this pressure is greater than atmospheric pressure, and may in particular be greater than 0.5 bar, 1 bar, 2 bars, 5 bars, 10 bars, 50 bars, 100 bars, 200 bars, or even 250 bars or more. In a particular embodiment, it is between 2 and 100 bars.
• the zone dense in molecules is obtained at least in part thanks to a gas flow generated by the evaporation of a cryogenic fluid. It can be obtained by combining the evaporation of a cryogenic fluid with an increase in pressure; this condition corresponds to the combination of the two means for dissolving the gas in the matrix mentioned in (iii) of step b) of the process.
• under pressure within the meaning of the invention, is meant conditions which allow the dissolution of a gas in a matrix and / or the maintenance of the gas dissolved in said matrix during deep freezing.
• the pressurization can be obtained either by increasing the pressure, or by bringing the matrix into contact with a cryogenic fluid, the evaporation of this gas creating a density of gas molecules equivalent to pressurizing so that the gas molecules dissolve in the matrix.
• the increase in pressure can also be obtained by a movement of gas creating a local pressure.
• putting “under pressure” corresponds to the application of relative pressures, that is to say that atmospheric pressure is considered as a pressure of 0 bar. All the pressures expressed in this document are relative pressures and the process is not carried out under partial vacuum.
• step b) takes place at a relative pressure sufficient to allow gas to dissolve in the matrix and an equivalent pressure is maintained in step c) to keep the dissolved gas inside the matrix during cryonics.
• the lyophilization step d) can be carried out either immediately following the cryogenics step c), or subsequently after storage of said frozen granules, particles or beads.
• the process conditions can be adapted as a function of the product to be dehydrated, in particular the pressure during the cryogenics step, and the lyophilization parameters. Those skilled in the art will know how to make such adaptations.
• the product to be dehydrated can be any type of liquid, semi-liquid or pasty matrix. It is preferably a natural matrix, for example a vegetable juice, a vegetable must, a fruit or vegetable juice, or a plant root.
• the product to be dehydrated in the form of a liquid, semi-liquid or pasty matrix comprises spirulina, turmeric, truffle or ginger.
• the matrix contains only spirulina, turmeric, truffle or ginger.
• the gas used will preferably be an inert gas such as liquid nitrogen.
• a second subject of the invention relates to a dehydrated powder capable of being obtained by a process as defined above.
• the powder according to the invention is obtained by the process described above.
• the fact of combining a deep freezing under pressure of a matrix in which a gas has been dissolved beforehand and a lyophilization gives new properties to the dehydrated powder thus obtained.
• the powder according to the invention is defined by the presence of particles of spherical shape.
• Spherically shaped particles represent a significant fraction of these particles.
• the spherical particles represent at least 25% of the powder, or even 30%, 40%, 50%, 60%, 75% or more. This characteristic differentiates this powder from the powders of the prior art.
• Another advantageous property is the fineness of the powder which is linked to a particle size of less than 30 microns without grinding the powder. In a particularly preferred embodiment, the particle size is less than 20 microns. In a very particular embodiment, it is less than 10 microns. These sizes are typically determined by optical microscopy.
• the powders according to the invention can therefore be characterized by the presence of particles of spherical shape whose size is less than 30 microns.
• This powder also has other properties which differentiate it from products freeze-dried by a conventional deep-freezing-freeze-drying process. Indeed, it is less dense and dissolves more easily. The rate of solubilization is remarkably increased compared to an equivalent product obtained by a conventional deep-freezing-lyophilization process, in particular at room temperature. The powder also has a color different from that of a powder obtained by a conventional process; it is overall clearer. All these characteristics testify to a more respectful preparation of the raw material, smoother and less destructuring conditions. These properties are shown in the experimental part.
• the process according to the invention makes it possible to prepare products with significantly increased organoleptic properties compared to equivalent products obtained by a conventional deep-freezing-lyophilization process.
• the product has a low density characterizing it, it can be compacted to facilitate its use (introduction into soft capsules for nutritional or pharmaceutical applications, compaction to reduce the volume of packaging for food products. ).
• the invention also relates to a powder in compacted form so as to reduce the volume of the product.
• the powder comprises spirulina, turmeric, truffle or ginger. In a preferred embodiment, it contains only spirulina, turmeric, truffle or ginger.
• a third object of the invention relates to the use of a powder as defined above in the food industry, in cosmetics, as well as in pharmacy and in human or animal health.
• a powder according to the invention can be used in the food industry to flavor food preparations or as colorants. It is particularly advantageous in particular because of its preserved organoleptic properties and its high solubility.
• the powder can be used in pharmacies, especially in compacted form.
• the powder is fine and homogeneous, which is a guarantee of quality and processability. It preserves the properties of raw materials for optimum efficiency. In addition, it dissolves easily in a drink for a drinkable formulation or after ingestion for a formulation in the form of a tablet to swallow.
• ingredients or active principles in particular of natural origin, thanks to the fact that the properties of the raw materials are little or not altered by the dehydration process.
• the high solubilization capacity is favorable to good bioavailability of the active ingredients.
• spirulina which is used in particular to combat fatigue and stress and to strengthen immunity.
• a fourth object of the invention relates to equipment for implementing the method as defined above and comprising:
• a matrix passage area located between the means for dispensing the matrix and the receptacle; a means for generating a dense zone of gas molecules in the passage zone, said means being either (i) a gas flow generated by the evaporation of a cryogenic fluid, or (ii) a pressurizing means, (iii) or a combination of these two means;
• freeze-dryer for transforming the frozen granules, particles or beads in the form of dehydrated powders.
• the dense zone of molecules or zone of passage of the matrix is located above the receptacle containing a cryogenic fluid.
• FIG. 9 illustrates an embodiment of the implementation of the present method in which the zone dense in gas molecules is generated by the combination of a flow of a gas and a pressurization of an enclosure.
• Figure 1 Represents the lyophilization kinetics observed for the 3 preparation conditions. Round: Reference; Triangle: Cryo BP; Square: Cryo MP.
• Figure 2 Microscopic observations made on the three coffee powders according to the preparation conditions; A: freeze-dried coffee particles obtained under cryo BP condition; B: freeze-dried coffee particles obtained under Cryo MP condition; C: freeze-dried coffee particles obtained under conventional conditions (reference freezer -20 ° C).
• Figure 3 Correlation between powder density and rehydration time of coffee powders.
• Figure 5 Chromatograms obtained following analysis by an electronic nose of the three powders obtained after lyophilization (Reference conditions, Cryo BP and Cryo MP).
• Figure 7 Correlation between densities and luminances of 3 freeze-dried coffee powders.
• Figure 8 Thermal characterization of coffee powders by modulated DSC.
• Figure 9 Schematic diagram of the process implemented showing the effects of pressure and gas dissolution / release in the product, a. preparation of the product at atmospheric pressure; b. dissolution of gas in the product, the partial pressure Pp of the dissolved gas being the sum of the pressure of the enclosure Pel and the local pressure linked to a flow of gas Pfl; vs. cryogenics of the product containing the dissolved gas, operating at a pressure Pc greater than or equal to the partial pressure Pp of the gas contained in the product, the pressure Pc itself possibly resulting from the combination of an enclosure pressure Pe2 and local pressure associated with a flow of gas Pf2; d. possible storage of the product in the form of solid beads at atmospheric pressure and at a temperature below the melting point of the product; e.
• the arrows represent the gas which is applied to the surface of the product in step b., Which remains in equilibrium in step c. and which escapes in step e.
• Figure 10 variation in the amount of phycocyanin-C during storage of lyophilized spirulina powder.
• the method according to the invention consists in dissolving a gas in large quantity in a matrix, in cryogenizing said matrix in the form of granules or beads and then in lyophilizing said matrix.
• the gas dissolution and cryogenics steps can be carried out in two distinct ways:
• the step of gasification of the matrix consists in dissolving in large quantity the gas generated by the evaporation of a cryogenic fluid in a matrix so that the product is at least saturated with said gas, the dissolution being carried out by increasing the number of gas molecules in an area of high gas density, known as a “high molecular density area”, located above the surface of the cryogenic fluid and on the path of the matrix drops before their immersion in the fluid, said zone of high molecular density being created by carrying out the gasification and cryonics of the gasified matrix within a closed chamber provided with a vent arranged to allow evacuation of the gas generated by the evaporation of the cryogenic fluid by convection natural and maintain the interior of the enclosure at a pressure greater than or equal to atmospheric pressure;
• the matrices rich in gas and in the form of frozen granules, particles or beads are then subjected to lyophilization according to conventional conditions. On leaving the freeze-dryer, dehydrated beads a few millimeters in diameter are obtained. These are very easily transformed into powder, a simple friction causing the crumbling of the very porous structure of the beads obtained.
• the matrix was prepared from a preparation of 3 L of filtered coffee, separated into 3 batches of IL each and then subjected to cooling as described above.
• the matrix was prepared from a turmeric juice obtained by entraining and crushing the roots of said plant between two endless screws enclosed in an eight-shaped tube. For 1 kg of roots, approximately 750 g of juice are obtained. This was then subjected to the process which is the subject of the invention without further intermediate treatment. c / Spirulina
• spirulina paste fresh seaweed collected, drained and pressed
• 800 g of water containing 2 g / L of salt The preparation was then subjected to the process which is the subject of the invention without further intermediate treatment.
• the process according to the invention makes it possible to prepare dehydrated products in a shorter time than the deep-freezing-lyophilization processes of the state of the art.
• cryogenized beads containing dissolved gas make it possible to obtain, whatever the pressure applied, a fine powder, which can be handled simply because it can be measured and not sticky.
• the resulting powder also does not pick up moisture easily when left at room conditions.
• the Reference freeze-drying only makes it possible to obtain agglomerates of product, which must generally be reprocessed (by grinding, for example) to facilitate or even allow their use.
• cryogenized products containing dissolved gas are much less dense than those obtained from conventionally frozen products.
• Table 1 above shows the density measurements carried out on the coffee powders obtained under the three different conditions.
• the frozen balls are non-porous (the incorporated gas is dissolved and allows the product to retain its "full", non-porous structure), a release of nitrogen takes place during lyophilization which allows the formation. small, very porous particles. The more the quantity of dissolved gas increases, the greater the porosity. The process under pressure thus produces a powder of very low bulk density (see Table 1), which does not require grinding (the dehydrated beads are reduced to powder by simple crumbling or crushing).
• the powder can still be easily compacted if necessary (eg pharmaceutical applications).
• Turmeric is used as a food ingredient in many preparations and recipes. Its solubility is an important problem for its addition in aqueous preparations.
• the process according to the invention makes it possible to obtain a turmeric powder which is very easily dispersible in food.
• An experiment for dissolving a powdered commercial turmeric and turmeric prepared by the “cryo MP” process was carried out. Stirring for one minute was carried out for the 2 products in distilled water at 22 ° C. At the end of the stirring, visually, the product “Cryo under pressure” is very well dispersed or even very widely solubilized. The industrial product is only very slightly solubilized.
• the olfactory profile of each coffee was determined by double ultra-fast gas phase chromatography (Héraclès II electronic nose, AlphaMos). For this, 0.01 g of each sample were taken in a 20 ml vial and placed at 40 ° C. for 1 hour to allow the release of the aromas which are then analyzed automatically. Each analysis is repeated 3 times.
• PCA Principal Component Analysis
• This global analysis leads to obtaining a discrimination index between the samples of 62, which is significant.
• This discrimination index can be explained more than 75% by the difference in area between the peaks (represented by the main component 1, denoted CPI).
• Table 3 Euclidean distance between samples Euclidean distances are important between pressurized cryogenic coffees and the frozen Reference. The products are very significantly different. Cryogenics under pressure produces coffees with aromatic profiles different from conventional deep freezing. The higher the pressure, the greater the distance. Overall, the increase in pressure increases the olfactory intensity of coffees.
• the “benchmark” coffee was detected as being significantly different from the other 2 coffees by 93% of the tasters. This coffee was detected at 76% as “less aromatic” than the other 2.
• the two Cryo BP and Cryo MP coffees were detected different by 61% of the tasters. This difference is therefore less sensitive than the difference between cryogenic coffees and the Reference. Among the tasters who judged the 2 cryogenized coffees to be different, 64% preferred the Cryo MP coffee because of a “more marked aromatic development”.
• the color of the coffee powders was analyzed according to the three preparation conditions described above.
• the colorimetric analyzes were carried out using a DataColor Konica-Minolta colorimeter according to the measurement procedure standardized in the L, a, b reference system.
• Table 4 Colorimetric analyzes of coffee powders according to the L, a, b standard.
• the measurements show that the “luminance L” (also called “clarity”) increases with the quantity of dissolved gas and therefore when the density of the powder decreases.
• the coffee cryogenized under 5 bars of pressure and then lyophilized has a distinctly lighter shade (higher luminance) than the other samples.
• coffees prepared under pressure are clearer, more aromatic, and dissolve better than coffee prepared according to the Reference process. These properties are due to the process and, as shown by the results obtained with turmeric, are generally applicable to all types of products.
• the thermal characterization measurements of the 3 coffee powders were carried out by modulated DSC (Differential Scanning Colorimetry).
• Powdered spirulina samples treated according to the three protocols described in point 1.2, were stored over time, at room temperature, and measurements of the quantity of phycocyanin C were carried out by spectrophotometry, after rehydration of the samples and lysis of the samples. cells by sonication at regular intervals. The results are shown in Figure 10.
• the process according to the invention therefore makes it possible to conserve and preserve active agents in dry and stable form over time, in a much more efficient manner than what can be obtained by conventional freezing then lyophilization.

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• 2019
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