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WO2018173090A1 - Procédé et dispositifs de production de membranes d'hydrogel remplies d'un liquide - Google Patents

Procédé et dispositifs de production de membranes d'hydrogel remplies d'un liquide Download PDF

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Publication number
WO2018173090A1
WO2018173090A1 PCT/IT2018/050050 IT2018050050W WO2018173090A1 WO 2018173090 A1 WO2018173090 A1 WO 2018173090A1 IT 2018050050 W IT2018050050 W IT 2018050050W WO 2018173090 A1 WO2018173090 A1 WO 2018173090A1
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Prior art keywords
solution
liquid
strainer
positive displacement
membrane
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PCT/IT2018/050050
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English (en)
Inventor
Andrea UGOLINI
Stefano CIMEI
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Ispherea Srl
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Ispherea Srl
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Priority to EP18718941.0A priority Critical patent/EP3599902A1/fr
Publication of WO2018173090A1 publication Critical patent/WO2018173090A1/fr
Anticipated expiration legal-status Critical
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    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
    • A23L27/00—Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
    • A23L27/70—Fixation, conservation, or encapsulation of flavouring agents
    • A23L27/72—Encapsulation
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23P—SHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
    • A23P10/00—Shaping or working of foodstuffs characterised by the products
    • A23P10/30—Encapsulation of particles, e.g. foodstuff additives
    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12G—WINE; PREPARATION THEREOF; ALCOHOLIC BEVERAGES; PREPARATION OF ALCOHOLIC BEVERAGES NOT PROVIDED FOR IN SUBCLASSES C12C OR C12H
    • C12G3/00—Preparation of other alcoholic beverages
    • C12G3/005—Solid or pasty alcoholic beverage-forming compositions

Definitions

  • the present invention concerns a process for the production of hydrogel membranes filled with a liquid, as well as the devices for implementing such process. More particularly, the invention relates to a procedure, and the relative instrumentation, which allows to obtain in rapid times, that is, the order of a few tens of seconds, spherical membranes of edible or not edible gels, which enclose internally liquids of any kind and composition, including acidic liquids or alcoholic liquids of any alcohol content, without altering the physical, chemical and organoleptic properties of said liquids.
  • spherification is a technique created in the frame of the york-garde cuisine known as "molecular cuisine", which allows to encapsulate substantially liquid foods, such as juices, syrups or smoothies, in spheres or pearls with a solid external structure and liquid core, concentrating the flavors in small globules that burst into the mouth similar to caviar.
  • the technique was brought to popularity around 2003 by the Catalan chef Ferran Adria, who proposed in his well-known restaurant El Bulli dishes based on a variety of pearls and spheroids obtained from the elaboration of edible products, with original combinations of flavors.
  • the technique is still used for the production of particularly eye-catching food preparations.
  • spherical structures is obtained with the help of a gelling agent, in particular, sodium alginate, and a second agent, generally a calcium salt such as calcium lactate or calcium chloride, which is able to exchange cations with the gelling agent.
  • a gelling agent in particular, sodium alginate
  • a second agent generally a calcium salt such as calcium lactate or calcium chloride, which is able to exchange cations with the gelling agent.
  • Sodium alginate is a polymer whose monomers consist of carbohydrates of various types, which share the
  • MB//A 17942 characteristic of having at least one carboxyl functional group bound to the monomeric ring.
  • the acid groups are salified with sodium, as shown in the followin structural formula.
  • Sodium alginate has a high solubility in water and tends to form more or less viscous aqueus solutions as the concentration of alginate changes.
  • Sodium alginate is therefore used in the food industry as a gelling agent, i.e. as an additive which increases the viscosity of the preparation. It is also used in the pharmaceutical industry as a gastroprotector, thanks to its ability to form a film on the stomach walls, which makes up for the lack of the natural protective film.
  • alginate An important feature of alginate is its great affinity for calcium, in its form of divalent cation.
  • the latter is chelated by carboxyl (and hydroxyl) groups of different alginate chains, as schematized in the following formula. For this reason when a salt containing calcium ions is added to a sodium alginate solution, the calcium ions are exchanged with sodium ions to give a structure that takes the following form:
  • Such structure becomes progressively more compact than the previous one, due to the chelating action of the carboxylate groups on the Ca 2+ ion, and there is a progressive stiffening of the structure.
  • the gelling agent has the characteristic of forming a gel when it comes into contact with the calcium ions, thus forming a more compact structure, which the authors themselves called "egg box” spatial arrangement, schematically represented below.
  • a given volume of sodium alginate solution dipped (e.g., poured drop-wise) in a solution containing calcium ions forms on its surface a gelatinous membrane of calcium alginate, more or less solid and elastic according to the concentration of sodium alginate and calcium ions in the two solutions. Therefore, when it is desired to enclose a (more or less viscous) liquid preparation in alginate spheres or beads, sodium alginate is mixed with the preparation to be spherified, and then the mixture thus obtained is put directly in contact with an aqueous solution of a calcium salt, for example, calcium chloride.
  • a calcium salt for example, calcium chloride.
  • spherification does not start until the time when sodium alginate or other similar gelling substance (such as carrageenans (or carrageenins), gellan gum, agar-agar, locust bean gum, tragacanth, gum arabic, pectin and other polysaccharides which may have similar behavior) do not come into contact with the ion-exchange agent, or is not cooled below a certain temperature, depending on the type of gelling agent. From that moment on, a gel membrane forms at the interface between the drop of mixture to be spherified and the external bath. If the formed sphere is not separated from the bath, it continues to thicken gradually towards the interior, leaving the remaining encapsulated liquid in the core, until the process is complete and the liquid core has disappeared.
  • gelling substance such as carrageenans (or carrageenins), gellan gum, agar-agar, locust bean gum, tragacanth, gum arabic, pectin and other polysaccharides which may have similar behavior
  • acidic drinks such as fruit juices or Coca-Cola also contain other chemical species, such as pectins or phosphates, which probably compete in the complexation of the calcium ions by alginate, thus making it impossible to obtain the membrane formation even with pH values higher than 1 .5.
  • alginate spheres Since the procedures for making alginate spheres involve mixing alginate in the liquid or in the beverage to be spherified and the permanence of alginate inside the formed sphere, it is inevitable that there is a reduction in sapidity of the initial product, more or less less noticeable depending on the type of product.
  • alginate spheres are not stable over time. Once the cation exchange has started, the calcium ions of the membrane spread towards the internal volume, which slowly leads to total gelation. The speed at which this occurs varies depending on the concentrations of the two solutions, on the temperature and the radius of the alginate sphere. This defect precludes the preventive preparation of the spheres and their storage for use in many preparations involving slow or delayed consumption.
  • a calcium salt (usually calcium lactate or calcium gluconate) is brought into solution directly into the liquid to be spherified, and subsequently this mixture is brought into contact with a sodium alginate solution.
  • the two reagents of the classical spherification process are topological ⁇ inverted, and the reaction between the alginate and the calcium ions takes place at the interface between the two liquids, but continues towards the outside of the formed sphere. Thanks to the presence of the calcium salt (which is tasteless) inside the sphere instead of alginate, the liquid contained within the sphere does not progressively change in flavor and consistency.
  • Times required for the express preparation are longer, as the spheres have to rest in the alginate bath for several minutes.
  • the preparation is more difficult to handle, given the difference in viscosity between the liquid to be spherifed, which remains fluid, and the alginate bath, which is viscous. Freezing the liquid may help, but in the case of high alcohol content this requires expensive tools and materials, such as liquid nitrogen or ultra-freezers.
  • the liquid product can be mixed with a thickener, but at the expense of flavor and organoleptic properties.
  • the spherified product contains moderate amounts of added calcium, and especially in the use of such products as a beverage risks for sensitive individuals cannot be excluded.
  • EP2537420A1 Biogades Food Tech. S.L.
  • Such method comprises a first step of forming the spheres by reverse spherification, i.e. the preparation of a solution of the alcoholic liquid, a thickening agent (for example, xanthan gum) and calcium gluconolactate (which must be left to rest preferably for 24 hours), the preparation of a second solution of water and sodium alginate, and the consequent formation of the spheres by introduction of portions of the first solution in the second solution.
  • a thickening agent for example, xanthan gum
  • calcium gluconolactate which must be left to rest preferably for 24 hours
  • the spheres are extracted from the bath and poured into a water bath to interrupt the gelling process, left to dry and then poured into a further "stabilizing solution” bath, consisting of a liquid with the same composition as the spherified liquid, but with a lower concentration of thickening agent.
  • a further "stabilizing solution” bath consisting of a liquid with the same composition as the spherified liquid, but with a lower concentration of thickening agent.
  • the apparatus described therefore, is able to process only the products that are notoriously processable manually with classical or reverse spherification, and does not allow to obtain, for example, spheres of products with a high alcohol content, or of particularly acid products, like many fruit juices.
  • This procedure was designed to allow the formation of the alginate sphere superficial membrane in its optimal conditions and to replace its internal volume with a liquid that would not have allowed formation of the alginate sphere.
  • sodium alginate and possibly ethanol may be added to the basic preparation, which will also be referred to below as "Solution A", both to vary the mechanical properties of the membrane which will be obtained at the end of the procedure, and to aromatize the membrane itself with particular flavors, as long as the relative proportions of water and alginate do not vary excessively.
  • the mechanical properties of the membrane may change in the presence of excipients in Solution A.
  • excipients in Solution A For example, the presence of mixtures of surfactant molecules such as soy lecithin, or fatty substances such as cocoa butter, olive oil or other edible fats make the membrane more elastic and delicate in its use, which in turn makes its consumption in gastronomy more pleasant.
  • This effect can also be obtained with the use of polysaccharides not interacting with calcium such as agar, xanthan gum, guar gum, etc..
  • aromatized membranes can be obtained by adding syrups or aromatic powders or alcoholic liquids to Solution A. In this way it is possible to create many combinations of flavors by combining different ingredients in the membrane, and then it is possible to decide which liquid to use for the internal filling. It should be noted that if it is desired to aromatize the membrane with an alcoholic beverage, the amount of alcoholic beverage to be added to Solution A will have to change according to the alcohol content of the same, in order to maintain the total alcohol content of Solution A at about 20% in volume. Therefore, in these cases the optimal amount to be mixed should be calculated according to what is described below.
  • the solution based on calcium salts in which the predetermined volume of the base preparation must be immersed, according to the procedure of the invention, in order to produce the calcium alginate membrane (which will also be referred to hereafter as "Solution B"), consists of an aqueous solution of calcium salts, preferably chloride or lactate.
  • Solution B will preferably have an alcoholic level similar to that of Solution A, so as to keep the ethanol concentrations in equilibrium during membrane formation.
  • the sphere After filling the sphere, in the fourth phase of the procedure the sphere is separated from the liquid exchanger device and immersed again, for a few seconds, in the calcium salt Solution B to seal the hole made by the device, and finally it is rinsed for a few seconds in water to remove calcium salt residues left on the membrane surface.
  • the proposed procedure allows to solve in a simple and cheap way the problem of realizing hydrogel membranes stable and suitable for any use, achievable in extremely short times, without any physico-chemical alteration of the content and with little manipulation, and therefore lends itself optimally to an express production, also for food products.
  • the proposed procedure can be carried out in the same manner by using another gelling agent instead of calcium alginate, which agent is capable of giving gelation by ion exchange, and also, with minimal variations, using agents gelling upon temperature variation, such as agar.
  • Solution A will have to contain a salt of the gelling agent with a counter-ion with which no gel is formed and Solution B will have to contain an ion with which the gel is formed, while in the second case Solution A will have to be at a temperature at which the substance employed does not gel and Solution B will have to be maintained at a temperature at which the gel is formed, and the operations of the third and fourth steps will have to be carried out at least at that temperature, as explained later on in the examples.
  • Figure 1a shows an orthogonal side elevation view of a strainer suitable for the execution of the second, third and fourth phases of a first embodiment of the present invention which employs a manual positive displacement liquid exchange device;
  • Figure 1 b shows an orthogonal side elevation view of a strainer suitable for the execution of the second, third and fourth phases of a second embodiment of the invention which employs a semiautomatic positive displacement liquid exchange device;
  • Figures 2a-2d schematically show the sequence of operations that are carried out in the second step of the process according to the invention, using for example the strainer of Figure 1 a, as well as the structure of the sphere thus obtained;
  • Figures 3a-3d and 4a-4d schematically show the sequences of operations that are carried out in the third and fourth steps of the process according to the invention, as well as the structure of the sphere thus obtained, using for example the strainer of Figure 1 a and the manual positive displacement liquid exchange device, a portion of which is shown schematically, the procedure which makes use of the strainer of Figure 1 b and of the automatic or semiautomatic positive displacement liquid exchange device being equivalent;
  • Figure 5 shows an overall perspective view of a manual positive displacement liquid exchange device for the implementation of the third phase of the first embodiment of the process according to the invention
  • Figures 6a-6d show the elevational views, front, rear, plan and side respectively, of the manual liquid volume exchange device of Figure 5;
  • Figures 7a-7d show the perspective views of four alternative needle types to be mounted in the center of the receiving chamber of the manual positive displacement liquid exchange device of Figure 5 or in a corresponding position in the semiautomatic positive displacement liquid exchange device of Figure 9 which follows;
  • Figure 8 schematically shows the connection of any one of the needles of Figures 7a-7d to the respective suction and liquid intake ducts of the positive displacement liquid exchange devices of Figure 5 and of the following Figure 9;
  • Figure 9 shows a perspective view of a positive displacement liquid exchange device for semiautomatic liquids for the execution of the third phase of a second embodiment of the process according to the present invention.
  • Figure 10 shows a partially exploded front perspective view of some of the components of the positive displacement liquid exchange device of Figure 9;
  • Figures 11a and 11 b show perspective views, respectively anterior and posterior, of the operating structure of the positive displacement liquid exchange device of Figure 9 without the two pumps;
  • Figures 12a and 12b show perspective views, respectively anterior and posterior, of the same operative structure of Figure 1 1 with the two positive displacement pumps in place;
  • Figures 13a and 13b show perspective views, respectively anterior and posterior, of the snap system for the exit of the needle in the positive displacement liquid exchange device of Figure 9;
  • Figure 14 shows a perspective view of the upper cover of the positive displacement liquid exchange device of Figure 9 and a side elevational view of the strainer of Figure 1 b in relation to the placement of the latter on the device during the third phase of the second embodiment of the process of the invention.
  • the present invention specifically provides a process for the preparation of closed hydrogel membranes containing a liquid, the process comprising the following operations:
  • the gelling takes place by cation exchange, and preferably said substance of the first aqueous solution is sodium alginate, while the second solution contains a calcium salt, preferably calcium chloride.
  • said strainer is substantially semi-spherical, semi-ovoidal (or semi-ellipsoidal), or in any case it has a concave bottom with a curved surface.
  • said first solution may contain one or more edible or non-edible substances having surfactant action, such as ethanol, soy lecithin, and/or one or more edible fats or oils, such as cocoa butter or oil olive.
  • ethanol soy lecithin
  • edible fats or oils such as cocoa butter or oil olive.
  • the first solution may contain one or more flavoring ingredients selected from aromatic powders or syrups, such as cocoa powder or mint syrup, and alcoholic beverages, such as for instance blue Curagao.
  • aromatic powders or syrups such as cocoa powder or mint syrup
  • alcoholic beverages such as for instance blue Curagao.
  • said first solution also contains a portion of ethanol not higher than 25% by volume
  • said second solution contains a portion of ethanol substantially equal to the ethanol portion present in said first aqueous solution.
  • the first solution contains, based on 1 00 ml, from 1 to 2 g of sodium alginate and from 18 to 25 ml of ethanol.
  • the first solution may also contain from 5 to 15 ml of syrup, or from 1 to 5 g of flavoring agent powder, or an amount by volume of alcoholic beverage such as to bring the final alcohol content of said first solution to no more than 25% by volume, the rest being made up of water.
  • the second solution contains, based on 400 ml, 2-4 g of calcium chloride and from 72 to 100 ml of ethanol.
  • positive displacement liquid exchange device any device or apparatus, whether manual or semi-automatic or completely automated, which allows to transfer a defined volume of liquid out of a delimited space, replacing it with another liquid which occupies substantially the same volume of the extracted liquid.
  • the two "emptying" and “filling” operations must be carried out consecutively and in rapid sequence.
  • the third phase (emptying and filling) of the invention process is carried out using a manual positive displacement liquid exchange device comprising:
  • a plunger fluid injection device connected in fluid communication to a second delivery path of said two-way hollow needle element
  • said plunger suction device is manually operated until the membrane of said spheroid is almost completely emptied, and then said plunger injection device is manually actuated until said membrane is filled again, completely, with said desired filling liquid.
  • the third phase of the process of the invention uses a strainer provided externally, at the bottom, with an annular magnetic element, and is carried out using a semiautomatic positive displacement liquid exchange device comprising:
  • annular housing for said strainer containing the spheroid formed in step 2 placed on a top surface of said container, at the center of which there is a hole from which said two-way hollow needle element may emerge, being preferably spring-actuated;
  • a fluid aspiration device constituted by a first positive displacement pump, preferably a peristaltic pump;
  • a fluid injection device consisting of a second positive displacement pump, preferably peristaltic;
  • a retractable support device for said two-way hollow needle element through which said needle element can translate vertically, preferably spring-actuated, between a first retracted position inside said container and a second extended position, in which it emerges from said hole, and in which, after positioning the strainer with said spheroid at said hole with the help of said annular magnetic element which is coupled with a corresponding magnetic element fixed to the upper surface of said container, the snap device is operated manually, effecting the two-way hollow needle element to emerge from said hole, then said first positive displacement pump is manually actuated until said membrane is almost completely emptied, and said second positive displacement pump is actuated until the membrane is completely filled again, with said liquid desired as stuffing. Said snap device is manually brought back into the initial phase by retracting the two-way needle out of the strainer and the obtained sphere.
  • the invention also relates to devices specifically designed for the positive displacement liquid exchange, both manual and semi-automatic, defined as above.
  • the devices mentioned are specifically suitable for use in the production of closed hydrogel membranes based on sodium alginate or any ion exchange or gelation hydrogels caused by temperature variation and containing a filling liquid of any kind not causing the destruction of the reticular structure of the membrane.
  • the concentration of ethanol in the prepared solution is 19 volumes. Although it is possible to form membranes even with a simple sodium alginate aqueous solution, the addition of ethanol gives them a softer and more elastic consistency. Presumably, the effect is due to the lower hydrophilicity of ethanol compared to water, in fact it has a short aliphatic tail capable of forming poor interactions with the alginate chains, but which contributes to "clutter" them by distancing them and making the plot more loose; moreover, through its hydroxyl group it is able to form three hydrogen interactions per molecule, compared to four molecules per molecule formed by water.
  • Solution B has an alcohol concentration of 20 volumes, similar to that of Solution A. This balance serves to maintain the percentage of ethanol in Solution A unchanged during membrane formation.
  • a few milliliters (on average 5) of Solution A are placed in a 35 mm diameter semispherical ladle or strainer (1 ), in order to avoid dispersion and to assist spherification.
  • the amount of Solution A fed into the strainer determines the size of the spheres.
  • the strainer (1 ) is pierced on the surface to allow the Solution B to filter in it and completely wrap the Solution A, as shown in Fig. 2b.
  • the immersion of the strainer (1 ) containing Solution A in Solution B causes the formation of the calcium alginate membrane, which almost instantly assumes a spherical shape, as shown in Figure 2c; this reaction takes on average 5/10 seconds to stabilize.
  • the sphere obtained, shown in Figure 2d, is therefore made up of a surface calcium alginate membrane and the internal sodium alginate solution remaining in original form since it has not yet come into contact with the calcium ions of the Solution B.
  • the created sphere undergoes rapid processing by an operator, which uses the positive displacement liquid exchanger (manual or automatic, Fig. 5 and Fig. 9 respectively) described below. This process is used to replace the Solution A of sodium alginate inside the sphere of Fig. 2d with any liquid to be introduced.
  • the process of processing the spheres obtained from phase two of the process must take place within 10 minutes after their creation, as they, prepared as such, are not stable and are gradually gelling.
  • step three can be performed by means of a manual, semi-automatic or automatic device.
  • Frame (2) its function is to provide support to the other parts of the instrument, in order to guarantee its mechanical stability during processing.
  • the frame (2) allows the insertion of two 50 ml syringes (3 and 4).
  • the same frame is equipped with extensions (5), always in stainless steel, for an ergonomic grip.
  • a syringe (3) is given the task of aspirating the alginate solution from the sphere, to the other syringe (4) has to inject the liquid chosen inside it.
  • the two syringes are designed to be connected to the respective suction (6) and injection (7) silicone tubes through the couplings (8) and the standard Luer threaded connections (9).
  • Receiving compartment (10) of the sphere is a hemispherical compartment (10) with a diameter of 35 mm in polypropylene or stainless steel, in which the sphere is introduced for processing. It has a central hole through which a needle passes (1 1 ).
  • the sphere is inserted inside the receiving compartment (10) by affixing the strainer (1 ) above it to be pierced by the needle (1 1 ).
  • the membrane is filled with the previously selected liquid and loaded into the syringe (4).
  • the filling liquid passes into the injection route (7) to the needle (1 1 ). It is preferred to inject a slightly larger volume than the aspirated one, to give a slight turgidity to the finished sphere.
  • the semiautomatic positive displacement exchanger is a device with which the spheres are processed in the third step of the process according to the invention in order to replace the internal solution of sodium alginate with a liquid of any type.
  • the receiving compartment (10) is no longer present: in its place a strainer (1 in Fig. 1 b) is used, separated from the device, which hooks onto the device through a magnet (12) placed at the base of the strain (1 a) itself, in correspondence with a housing (10a) located on the upper lid of the device, in the center of which there is a hole from which the needle (1 1 ) can emerge.
  • the syringes used in the previous embodiment are replaced by two peristaltic positive displacement pumps (3a and 4a), connected to two buttons (13 and 14 in Fig. 9) placed on the lid (15) of the machine, with which they can be activated manually suction and injection procedures.
  • a third embodiment of the fully automated positive displacement liquid exchange device in which the timing of the suction and injection phases is controlled by a programmable electronic controller, for example PC.
  • the suction pump (3a in Fig. 10) extracts the alginate from inside the membrane, pouring it out through a special tube (16) into a dedicated container.
  • the injection pump (4a) draws, from a dedicated external container through a special tube (17), the liquid to be inserted in the sphere just emptied.
  • the alginate extracted from the membrane is transferred through a tube connected to the side path (18 in Figures 1 1 a, 12a and 13b) of the two-way needle element (1 1 ), while the injection pump (4a) inserts the liquid selected through the vertical path (19 in Figures 1 1 a and 13) of the same two-way needle element (1 1 ).
  • the processing therefore consists of two phases:
  • the membrane is filled with the previously selected liquid and loaded into a suitable external container.
  • the filling liquid passes through the injection route (17) to the needle, through which it fills the sphere. Also in this case it is preferred to inject a slightly larger volume than the aspirated one, to give a slight turgidity to the finished sphere. Needles typology
  • the two-way needles (1 1 ) can be of different types, and are mounted so as to form a removable body from the rest of the positive displacement liquid exchanger, whether manual or semi-automatic. In this way they can be replaced according to the needs of product realization. The replacement takes place through the connections placed at the ends of the injection and suction path of the chosen needle.
  • the special suction and injection tubes can be inserted by pressure on the needle attachments, being of elastic material, and their elasticity allows a perfect seal during the operations necessary for processing the product.
  • holes (21 ) are made distributed crosswise around the needle (1 1 ), which constitute access to both the suction and the injection. Their cross arrangement is necessary to obtain a homogeneous aspiration from all sides of the spheroid.
  • the position of the holes (21 ) in relation to the bottom of the receiving compartment (10) is calibrated so that the suction, even if it has to take place from below to guarantee an optimal removal of the sodium alginate solution, leaves a small quantity in the near the needle entry hole to allow the membrane to close at the end of processing.
  • the holes (21 ) are made with an angle of incidence on the surface of the needle (1 1 ) of 45 ° upwards, so that in the injection phase they push the flow of the injected liquid upwards to assist the swelling of the membrane.
  • the longest part (24) of the double needle penetrates 10 mm into the receiving compartment (10). Its top is closed and rounded to prevent the upper part of the membrane from accidentally drilling during the suction phase. Near the top there are three holes (25) distributed uniformly along the semi-circumference of the needle, which constitute the access of the injection route. This arrangement of the holes (25) is necessary to obtain an injection which is as homogeneous as possible on all sides of the sphere.
  • the holes (25) are made with an angle of incidence on the surface of the needle of 45 ° degrees upwards, so that in the injection phase they push the flow of the liquid injected upwards to assist the membrane's swelling .
  • the catheter (26) of FEP is of large caliber (G14/G16) and within this the steel needle is replaced with a needle (27) of lower caliber (G20). The difference in diameters thus generates a gap between the inner wall of the catheter (26) and the outer one of the steel needle, which flows into the suction path.
  • the holes (28) are 3 mm away from the bottom of the receiving compartment (10), as the suction, even if it has to take place from below to guarantee an optimal removal of the sodium alginate solution, must nevertheless leave a small amount of sodium alginate near the entrance hole of the catheter needle into the sphere, to allow it to close at the end of processing.
  • the cross-shaped arrangement of the holes (28) is necessary in order to obtain a homogeneous suction on all sides.
  • the steel needle (27) instead crosses with the top (29) the sealing of the catheter, to inject into the environment of the emptied spheroid the chosen liquid. It is connected to the injection way, besides it is devoid of the usual oblique cut tip, in order to avoid that the upper part of the membrane is perforated during the emptying phase because of its possible reclining on the end of the needle.
  • the catheter needle described above presents an important problem: a strong resistance in suction and injection, there is therefore the need to use powerful thrusts and needles with a wider section (14G), which nevertheless leave a large hole in the membrane to such an extent that make it difficult to close. This is due to the simultaneous presence of two needles one inside the other, in which the wall of the internal one subtracts much of the section useful for the passage of liquids.
  • a system of needles has been realized which keeps the coaxiality composed of two needles with a smaller diameter (18G) than the previous ones (14G, 16G), arranged in series.
  • the plastic catheter is replaced by a steel needle (30a) 18G, which is able to pierce the membrane of the sphere due to its rigidity.
  • the steel needle (30a) is connected to a "T" fitting (31 ) typical of the two-way catheter needles.
  • the lateral pathway (18) (shown also in Figures 1 1 a, 12a and 13b) will be that of aspiration.
  • another needle (30b) 18G is hooked by means of a threaded connection, the end of which ends one millimeter before the needle (30a) previously mentioned begins.
  • the sucked liquid proceeds through the first steel needle and flows into the T-piece thanks to the millimeter of space left by the second needle, then flows into the suction pipe towards the pump (3a), from which the suction force comes from.
  • the injected liquid instead, runs through the tube coming from the injection pump (4a), arrives at the second needle (30b) and, once run across, it flows into the T-piece (31 ), covering that millimeter of space that brings it to the first needle (30a), and ending directly in the alginate membrane.
  • a disadvantage of the system with needles in series consists in the possibility of contamination of the base of alginate aspirated by the liquids injected in the previous processes. This base can not be reused.
  • the series system of needles (30a and 30b) penetrates and subsequently emerges from the membrane to perform the emptying and filling operations by means of a vertical snap system shown in particular in Figures 13a and 13b.
  • the snap system is regulated by a spring-loaded piston (32) and assisted by ball bearings (33), and is operated by the push-button (34) on the upper cover (15) of the illustrated device.
  • the formed sphere is removed from the positive displacement liquid exchanger by means of the strainer (1 ) and again immersed in Solution B to seal the needle entrance hole, which closes thanks to the small volume of alginate solution of sodium remained near the hole.
  • the spheres worked through the positive displacement liquid exchanger do not undergo modifications over time.
  • the internal volume no longer constituted by a solution of sodium alginate, can not be continued in gelation.
  • These spheres can be inserted in preparations that foresee a slow consumption, and it is allowed to be stored preferably in the short term (5 hours) and at temperatures close to the freezing threshold of the internal liquid.
  • the spheres prepared in step two are compatible with filling with moderately acidic liquids.
  • Freezing can be used to guarantee long-term storage. In the case of non-alcoholic substances this can take place in a normal freezer, whereas in the case of high-graded alcohol, temperatures up to -100 °C may be necessary. It should be noted that frozen membranes are very fragile and sensitive to thermal shock from thawing. Their fragility decreases as the alcohol content of the internal drink increases.
  • the alcoholic beverage has an alcohol content of less than 20 volumes: an amount of ethanol must be calculated to bring the final mixture to 20 volumes.
  • the addition of water is not necessary as it is already present in the flavoring drink.
  • the alcoholic beverage is already at a volume of 20 volumes, or next to it: this drink can be considered ready for mixing with sodium alginate, avoiding adding ethanol or water to it.
  • the alcoholic beverage has a gradation higher than 20 volumes: a quantity of water must be calculated to obtain a final solution of 20 volumes. It is not necessary to add ethanol, as it is already present in the flavoring drink.
  • the amounts of water and ethanol to be added to flavored membrane drinks can be calculated using the equations expressed below to obtain 100 ml of base solution.
  • G 0 alcohol percentage by volume of the flavoring drink
  • G f alcohol percentage in final volume of the mixture If Go ⁇ G f there can be used an amount of beverage equal to:
  • equations (1 ) and (2) do not take into account the fact that food ethanol is usually found at a concentration of 95% by volume.
  • the value of G f will be slightly inaccurate as G 0 decreases for each Go less than G f .
  • the correction factor would make the formula more complex in front of an insubstantial benefit. In case it is necessary to have avaialble ethanol at percentages by volume lower of 95% the discrepancy should be corrected.
  • Beverages with a gradation of less than 20% by volume Beverages with a gradation of less than 20% by volume:
  • soy lecithin 0.16 g are added in solution in 20 ml of ethanol, mixing until complete dissolution;
  • agar is a carbohydrate extracted from red algae (Gelidium, Gracilaria, Gelidiella, etc.) soluble in water at high temperatures (90-100 °C) which forms a hydrogel after cooling because it is not soluble cold.

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Abstract

Le procédé de l'invention permet d'obtenir rapidement, c'est-à-dire en une durée de l'ordre de quelques dizaines de secondes, des membranes d'alginate de calcium renfermant en leur sein des parties sphériques de liquides alimentaires de n'importe quel type et une composition, comprenant des liquides acides, ou des liquides alcooliques de n'importe quelle qualité ABV, sans altérer ses qualités physiques, chimiques et organoleptiques. L'invention concerne également un ensemble d'instruments et de dispositifs spécifiquement mis au point pour mettre en œuvre la méthode, soit dans un mode entièrement manuel, soit dans un mode automatique ou semi-automatique, tel qu'un dispositif d'échange de liquide à déplacement positif avec des pompes à déplacement positif (3a, 4a).
PCT/IT2018/050050 2017-03-24 2018-03-23 Procédé et dispositifs de production de membranes d'hydrogel remplies d'un liquide Ceased WO2018173090A1 (fr)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3849342A1 (fr) * 2018-09-12 2021-07-21 CDJ Partners, LLC Sphères comestibles contenant de l'alcool
IT202100006698A1 (it) * 2021-03-19 2022-09-19 Univ Degli Studi Di Sassari Metodo per realizzare una sfera edibile contenente una matrice liquida

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US4507327A (en) * 1983-05-23 1985-03-26 Q.P. Corporation Process for preparing edible products in the form of capsules
US20130045319A1 (en) * 2010-05-04 2013-02-21 Oriol Castro Projected, S.L. Method for the encapsulation of a food product and food product
US20150118365A1 (en) * 2013-10-31 2015-04-30 Steven J. Hollenkamp Alcohol containing beads and method for making same
US20160257916A1 (en) * 2013-10-31 2016-09-08 Steven J. Hollenkamp Method for mass producing alcohol-containing spherical beads

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US4507327A (en) * 1983-05-23 1985-03-26 Q.P. Corporation Process for preparing edible products in the form of capsules
US20130045319A1 (en) * 2010-05-04 2013-02-21 Oriol Castro Projected, S.L. Method for the encapsulation of a food product and food product
US20150118365A1 (en) * 2013-10-31 2015-04-30 Steven J. Hollenkamp Alcohol containing beads and method for making same
US20160257916A1 (en) * 2013-10-31 2016-09-08 Steven J. Hollenkamp Method for mass producing alcohol-containing spherical beads

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UNKNOWN: "Tomato Water Spheres Injected with Basil Oil", 2 February 2015 (2015-02-02), XP002777309, Retrieved from the Internet <URL:http://www.molecularrecipes.com/spherification-1/tomato-water-spheres-basil-oil/> [retrieved on 20180115] *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3849342A1 (fr) * 2018-09-12 2021-07-21 CDJ Partners, LLC Sphères comestibles contenant de l'alcool
IT202100006698A1 (it) * 2021-03-19 2022-09-19 Univ Degli Studi Di Sassari Metodo per realizzare una sfera edibile contenente una matrice liquida
WO2022195428A1 (fr) * 2021-03-19 2022-09-22 Università Degli Studi Di Sassari Procédé de production d'une sphère comestible contenant une matrice liquide

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