EP0783251A2 - Encapsulation d'aromes - Google Patents

Encapsulation d'aromes

Info

Publication number
EP0783251A2
EP0783251A2 EP95935021A EP95935021A EP0783251A2 EP 0783251 A2 EP0783251 A2 EP 0783251A2 EP 95935021 A EP95935021 A EP 95935021A EP 95935021 A EP95935021 A EP 95935021A EP 0783251 A2 EP0783251 A2 EP 0783251A2
Authority
EP
European Patent Office
Prior art keywords
coffee
matrix
volatile
aroma compound
melt
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP95935021A
Other languages
German (de)
English (en)
Other versions
EP0783251A4 (fr
Inventor
Charles V. Fulger
Lewis M. Popplewell
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
McCormick and Co Inc
Original Assignee
McCormick and Co Inc
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by McCormick and Co Inc filed Critical McCormick and Co Inc
Publication of EP0783251A2 publication Critical patent/EP0783251A2/fr
Publication of EP0783251A4 publication Critical patent/EP0783251A4/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23F—COFFEE; TEA; THEIR SUBSTITUTES; MANUFACTURE, PREPARATION, OR INFUSION THEREOF
    • A23F5/00—Coffee; Coffee substitutes; Preparations thereof
    • A23F5/46—Coffee flavour; Coffee oil; Flavouring of coffee or coffee extract
    • A23F5/48—Isolation or recuperation of coffee flavour or coffee oil
    • A23F5/486—Isolation or recuperation of coffee flavour or coffee oil by distillation from beans, ground or not, e.g. stripping; Recovering volatile gases, e.g. roaster or grinder gases
    • 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
    • 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

Definitions

  • the present invention relates to techniques to encapsulate materials which can undergo compositional changes in process and/or storage. Such encapsulation improves material shelf-life and usefulness in the preparation of products such as foods.
  • the present invention also relates to a method for encapsulating coffee aroma compounds, such as those contained in natural or synthetic coffee grinder gas, in a glassy matrix of a food polymer as well as compositions in which such coffee aroma compounds are so encapsulated.
  • Flavors are complex substances made up of multiple chemical components, some comparatively stable, some extremely volatile, others unstable to oxidation and reactive interactions and the like.
  • Many flavorants contain top notes (i.e., dimethyl sulfide, acetaldehyde) , which are quite volatile, vaporizing at or below room temperature. These top notes are often what give foods their fresh flavors.
  • the traces of the isopropyl alcohol remaining in the product after quenching can be detrimental. This technique limits the materials which can be encapsulated to those which are immiscible in the matrix.
  • An additional disadvantage of the product resulting from this process is that although reasonably dense, the product may contain microporosity when low boiling point components are present in the flavor. The microporosity increases the surface area, and thus, may increase the evaporation of volatiles and the potential for degradation of the product by interaction with atmospheric oxygen. Furthermore, the effect of the microporosity is enhanced as the product is sold in a finely divided state, which increases the surface area of the particles and thus the possibility that degradation of the flavor will occur if the product is stored over a period of time.
  • This patent suggests utilizing as the encapsulant a mixture of two materials, one having a high molecular weight and the other having a low molecular weight; as a result, the mixture may be successfully extruded.
  • the minor component melts and the major component dissolves into the minor component.
  • the volatile flavorant becomes dispersed or solubilized within the molten mass which upon cooling produces a single phase matrix.
  • the '534 technique needs to utilize as the encapsulant a mixture of materials, one having a melting point sufficiently low such that the remainder will melt into it thereby becoming extrudable under reasonable process conditions.
  • U.S. Patent 5,009,900 ('900) is directed to a procedure very similar to that of '534 only using a more complex mixture of materials to form the encapsulant material.
  • the '900 patent requires a water-soluble, chemically-modified starch, maltodextrin, corn syrup solids and mono- or disaccharides. The flavorant is mixed into the mixture and the result is extruded. It would not be possible with either of the techniques of '534 or '900 to encapsulate pure low boiling point materials such as acetaldehyde in a dense matrix at commercially significant loads since the resulting product would foam due to the vaporization of acetaldehyde as it exits the extruder.
  • a long-standing problem in the instant coffee art is the preparation of instant coffees having the same aroma as freshly roasted and ground coffee itself.
  • a similar problem of aroma dissipation also exists in holding ground roast coffee for a time before consumption.
  • Many methods have been utilized in attempting to approach this desired end result. For example, aroma materials have been stripped from roast and ground coffee and added back to instant coffee after complete processing; and coffee oil collected from extracted roast/ground coffee beans has been used to absorb the aroma volatiles and added back to final instant coffee product as an aroma-enhancing material.
  • Aroma frost is a low temperature condensate of volatiles which escape during coffee processing, for example, during roasting, grinding, steam distillation, extracting where it is employed, and dry distillation and the like. These volatile constituents are often obtained by low temperature condensation of escaping gaseous material, for example at liquid nitrogen temperatures, by passing the escaping gas through a liquid nitrogen trap to yield a condensate which is referred to herein as an aroma frost.
  • the aroma frost may be grinder gas frost, roaster gas frost, a dry distillation frost, a steam distillation frost, and the like.
  • aroma frost must then be incorporated in a relatively stable manner into the coffee product whose roast and ground coffee aroma is desired to be increased.
  • this coffee product is an instant coffee because instant coffees are notably deficient in characteristic roast and ground coffee aroma.
  • the aroma frost itself must be incorporated into a stable carrier in order to have any significant amount of retained aroma value.
  • the most common carrier is coffee oil.
  • Grinder gas that is the gas which is released from roasted whole coffee beans when their internal cell structure is disrupted, such as during grinding of the beans and which also continues to be evolved from the disrupted and/or fractured beans for a short period thereafter, has long been recognized in the art as a highly desirable natural coffee aroma.
  • a great deal of effort has been directed toward the development of a method for recovering and fixing a high percentage of grinder gas aromas on a substrate for subsequent addition to coffee products, particularly soluble coffee powder.
  • U.S. Patent no. 3,021,218 discloses a method whereby a coffee aroma condensate is vaporized to admit the more volatile coffee aromas into void spaces of a container filled with soluble coffee.
  • U.S. Patent no. 2,306,061 describes the addition of condensed grinder gas to chilled soluble coffee powder. These two methods are similar in that grinder gas aromas are contacted directly with coffee particles in order to improve the aromatics of the coffee product. However, both methods fail to provide the convenience, stability, and high level of grinder gas fixation, desired in the coffee field.
  • 3,979,528 describes contacting a glyceride and condensed grinder gas in a pressure vessel at a temperature of 70° to 75°F, and a pressure above 100 psig to enable aromatic transfer from the liquid carbon dioxide phase to the liquid glyceride phase, and then venting the vessel.
  • This procedure involves repeated venting of said pressure vessel from a high pressure ranging from 75 to 120 psig, to a low pressure of 0 psig.
  • U.S. Patent no. 4,007,291 discloses contacting a glyceride with condensed grinder gas in a pressure vessel at a temperature of 70° to 85°F, and a pressure in excess of 700 psig, then slowly venting the pressure vessel, preferably isothermally.
  • U.S. Patent no. 4,119,736 discloses the removal of a water phase from a pressure vessel containing condensed grinder gas at a high pressure and temperature, contacting the demoisturized grinder gas with a glyceride, and slowly venting the pressure vessel. The separation of aromas from the removed water phase, such as by vacuum distillation, and to reclaim or recycle vented aromatics, is also described.
  • European patent application 205,204 describes a complex process for the preparation of a liquid coffee aroma, which comprises first condensing the coffee grinder gas, then subjecting it to a high pressure, and finally, through a number of further operations, converting it into a liquid coffee aroma substantially free from C0 2 .
  • This coffee aroma can be used for aromatizing a substrate, such as ground coffee or a coffee powder.
  • European patent application 201,968 describes the treatment of ground coffee with a carrier gas to remove aroma components from ground coffee. The aroma components can then be removed from the carrier gas by condensation.
  • European patent application 144,758 discloses a process in which ground coffee is heated to a temperature between 30° and 95 ⁇ C, and the released aroma components are contacted with instant coffee.
  • European patent application 28,043 describes aromatizing coffee, by cooling coffee grinder gases with dry ice, optionally together with the coffee.
  • European patent application 41,370 also describes the condensation of coffee aroma components on coffee at cryogenic temperatures.
  • British patent publication 2,063,640 also teaches the condensation of aroma components on ground coffee.
  • U.S. Patent no. 3,823,241 describes a method wherein an absorbent carrier is cooled to at least - 40 ⁇ F. (preferably - 150°F.) and then placed in communication with roast and ground coffee under pressure conditions which transfer the coffee aroma to the absorbent carrier.
  • Another example is aroma frost equilibration with an aroma substrate which is typically a liquid glyceride such as coffee oil.
  • U.S. Patent no. 3,783,163 discloses a method for aromatizing edible oils by adding the oil to a cryogenic fluid to form a slurry, adding an aroma frost to the slurry, preferably with mixing, and then allowing the mixture to equilibrate to evaporate the cryogenic fluid, leaving behind a residue of aroma-enhanced oil.
  • U.S. Patent no. 4,335,149 and European patent application 10,804 disclose methods of condensing grinder gas on a food substrate such as ground coffee at cryogenic temperatures.
  • U.S. Patent no. 4,520,033 describes a method for preparing capsules which contain a foamed core containing an aqueous essence such as coffee distillates.
  • the core may be foamed with coffee grinder gas.
  • U.S. Patent no. 3,821,447 discloses a method of stabilizing coffee aromas by condensing grinder gas with an edible glyceride such as an oil and then removing excess water. The resulting blend may then be mixed with an aqueous coffee extract or dry soluble coffee.
  • U.S. Patent no. 3,991,223 teaches a method for treating steam coffee aromas by means of liquid glyceride extraction to yield glyceride and aqueous phases with smooth, buttery flavors.
  • U.S. Patent no. 4,044,167 teaches a method of aromatizing soluble coffee products in which grinder gas is added to a liquid glyceride which is then frozen and then blended with the soluble coffee.
  • U.S. Patent no. 4,556,575 discloses a method for aromatizing soluble coffee by contacting the water phase, normally drained from equilibrated grinder gas and discarded, with a glyceride to recover coffee aromatics in the glyceride which may then be refluxed with liquid carbon dioxide before combining with a soluble coffee powder.
  • U.S. Patent no. 5,079,026 describes a process for preparing an expanded gasified coffee glass in which a melt of coffee solids and coffee oil is injected with a gas such as nitrogen or carbon dioxide, extruded through an orifice, allowed to expand, and then quickly cooled.
  • a gas such as nitrogen or carbon dioxide
  • U.S. Patent no. 5, 035,908 discloses a method for preparing a coffee glass by evaporating a coffee extract to form a viscoleastic fluid and rapidly cooling the fluid.
  • the hot viscoelastic fluid may be gasified to lower the density of the glass, in which case the gasified fluid is allowed to expand prior to cooling.
  • European patent application 353,806 teaches a method in which the content of the aroma components in coffee grinder gas is increased, such as by increasing the pressure or removing a portion of the C0 2 , before contacting with coffee.
  • Synthetic coffee aroma such as those described in U.S. Patent nos. 1,696,419 3,852,481, 3,873,746, 3,655,397, and 4,378,380 have also been employed to enhance overall coffee flavor and aroma by mixing together compounds known to exist in coffee.
  • a second embodiment involves forming a melt containing an encapsulate dissolved in a solvent and an encapsulating matrix which is optionally subjected to an elevated pressure, followed by venting to remove at least some of the solvent while largely retaining the encapsulate in the product.
  • the dense amorphous, essentially non- crystalline solid encapsulant may be described in many cases but not exclusively by those knowledgeable in the art as a 'glass' as characterized by a glass transition temperature.
  • the present invention provides a process in which the encapsulate contains a volatile coffee aroma compound, such as one or more components of natural or synthetic coffee grinder gas.
  • the encapsulate is a volatile gas such as those emitted when baking dough products, like bread, or roasting foods, like nuts, or peanuts, or meats.
  • Figure l is an illustration of the present process where the flavor component to be encapsulated is introduced into the extruder where a matrix material has been melted.
  • the drawing shows both atmospheric and pressurized discharge points. These were used in examples to produce comparative samples;
  • Figure 2 is an illustration of another embodiment wherein the matrix is first melted in an extruder and the flavor and melted matrix material are mixed in a static mixture and then recovered.
  • the drawing shows both atmospheric and pressurized discharge points. These were used in examples to produce comparative samples;
  • Figure 3 is an illustration of the present process where the flavor component is diluted in a volatile solvent and said solvent is removed via venting;
  • FIG 4 is a generalized overview of process sequence steps which can be utilized in the present process.
  • melting equipment herein referred to as M melter M
  • the components of the matrix are introduced into a melter where they are liquefied.
  • the melting may be accomplished in a batch containment.
  • the melter also can be simply a device transporting the matrix through a heating zone wherein sufficient heat is introduced to convert the matrix to liquid form, i.e., melted.
  • the process can utilize a conventional single or twin screw extruder having mixing zones, homogenizing zones, melting zones, venting zones and the like as is conventionally known in the art.
  • the matrix materials may be composed of a variety of melting compositions so that the resulting dense matrix will not become sticky and agglomerate at lower temperatures yet will melt/dissolve at under normal application conditions and temperatures as described in the prior art. Any meltable matrix ingredient can be utilized.
  • the solvents which can function as the plasticizer include any liquid material in which the matrix is soluble. Typical solvents include water, water-ethanol, glycerin, propylene glycol and the like. An optional process step, venting, can be added where some or all of the solvent can be removed. Following, the encapsulate is then mixed into the matrix. Essentially any encapsulate, insoluble, slightly soluble or miscible in the matrix may be employed in this particular embodiment. In cases where the encapsulate exists as a solution in a volatile solvent (e.g. water, alcohol) , the melt may be vented to substantially eliminate the encapsulate solvent.
  • a volatile solvent e.g. water, alcohol
  • Cooling of the melt can be accomplished at ambient conditions, with cooled gas, by direct contact with metal belts or rolls, or by quenching in a suitable solvent, as in the prior art, or most preferably as introduced by the invention, under pressure so as to prevent "puffing" or expansion of the matrix material into a non-dense, porous form.
  • this embodiment can be performed using a wide variety of apparatus to form the melt and to extrude it through a die into the pressurized zone.
  • the simplest technique is to form a melt using the procedures described in U.S. Patents 4,610,890 and 4,707,367. These techniques utilize a batch reactor to form the melt.
  • the matrix material with suitable solvent is introduced into the tank and melted. Once the melt has been established, then the material to be encapsulated is added. It is possible to vary this procedure where the material to be encapsulated also functions as a solvent for the solid matrix material.
  • the encapsulate and solid matrix are added together without the use of any separate solvent and the melt established.
  • the tank or vessel in which this is accomplished can either be opened to the atmosphere or closed. It is particularly preferred that the vessel be a pressure vessel and closed during the process so as to reduce the losses of any volatile components in the material to be encapsulated. If the volatile components comprise a significant portion of the encapsulant, then pressure should be established in the vessel so as to reduce the vaporization of the low boiling components in the vessel and thereby increase their yield.
  • the vessel can then be pressurized further, if necessary, and the pressure in the vessel used to force the melt through the die into a solidification zone.
  • Prior art as described above used an ambient pressure solidification step.
  • the present invention introduces the use of a pressurized solidification zone having a pressure sufficient to preclude the vaporization of the significant portion of the volatile components in the melt during solidification.
  • the pressure in the solidification zone is chosen to be sufficient so as to prevent puffing or microporosity.
  • the melt can be delivered by either the pressure of the containment or by a pump to the die.
  • Other techniques for forming a melt containing the matrix and encapsulant can also be used. Essentially any of the techniques described in the prior art for forming a mixture of matrix and encapsulant can be used.
  • the use of extrusion is preferred.
  • the heat necessary to form the melt can be provided by the mechanical working of the screw alone or in cooperation with external sources of heat. Heated extruders for use in the food industry are well known and can be used for this purpose so that heat from both the external sources, such as the steam jacket around the extruder, as well as from the mechanical working of the extruder can be used.
  • the plasticizer/matrix melt may have its pressure reduced so as to vaporize a portion of the plasticizer. This reducing of pressure or venting to vaporize a portion of plasticizer may occur either before or after the encapsulate is introduced into the matrix into the melt when the encapsulate is of low volatility. If it is a highly volatile encapsulate then, the venting should occur prior to introduction of the high volatile component. After the highly volatile component is added, the melt is then extruded through a die and pressure cooled. Venting is particularly advantageous for use with encapsulates which are dissolved in a solvent which also function as plasticizers for the melts.
  • the resulting solid product may have undesirable properties, such as tackiness, softness at low temperatures and a tendency to agglomerate.
  • One technique for avoiding these problems is to simply use a total quantity of plasticizer and encapsulate which results in the desired properties. This procedure would restrict the loading of encapsulate which can be used.
  • venting the plasticizer it is possible to incorporate higher quantities of encapsulate into the matrix without adversely affecting the properties of the final product. When venting is used, it is necessary to repressurize the melt after the venting so as to eliminate from the melt any bubbles which might have been caused by venting of the solvent. In an extruder, this is easily accomplished using appropriate screw configurations.
  • introduction of the melt into a melt pump after venting can accomplish the same purpose.
  • the degree of repressurization depends upon the degree of pressure necessary to remove the voids which were formed in the matrix by the venting and be sufficient to allow extrusion through the die into the pressurized zone where cooling or solidification of the melt occurs.
  • plasticizer tends to produce a softer and tackier product than reduced quantities of plasticizer in general.
  • the finished product may be overcoated with a material to reduce tackiness.
  • the encapsulate may migrate to the surface and possibly to evaporate from the product. In such instances, it is possible to overcoat -27-
  • the product with a hard coating which prevents or reduces such migration and evaporation.
  • Figure 1 illustrates one method by which the process can be accomplished.
  • the matrix material is introduced into a continuous melter where it is melted. If necessary, the solvents described above will also be used to assist in the melting process.
  • the injected encapsulate is mixed into the matrix.
  • the matrix is then extruded and cooled to form the encapsulated product.
  • the extrusion may be directly from the melting equipment under pressure or, as shown in Figure 1, a melt pump 06 may be employed to feed the extrusion die.
  • alternative methods are illustrated for cooling the encapsulated material. Discharge of the molten matrix/encapsulate mixture to atmospheric pressure illustrates the state of the art technique.
  • the mixture of matrix and encapsulate is introduced into a pressure vessel, 08, where it is formed through a nozzle 09 into a continuous/batch pressure confinement.
  • the pressure is provided by any gas, if necessary, food grade and/or inert, such as nitrogen, helium, or the like in pressure holding vessel 13.
  • Pressure cooling is utilized wherein either the encapsulate contains a substantial quantity of volatile components, that is, components having boiling points substantially below the temperature of the melt.
  • the product After cooling under pressure, the product generally needs size reduction by grinding or the like to provide a free flowing material which is readily mixed with other components.
  • the nozzle utilized to extrude can be any type of nozzle and the size of the strands to be extruded is not critical. Typically, a "spaghetti" type nozzle will be employed so as to minimize the amount of particle size reduction which must be accomplished mechanically.
  • the molds are normally closed and the material injected under pressure and cooled before the mold is opened.
  • a further alternative is to introduce the melt under pressure into a body of liquid having a sufficient liquid head so as to establish a pressure at the point of melt introduction sufficient to preclude substantial volatilization of the volatile component.
  • any liquid can be used for this purpose, however, food grade liquids are preferred.
  • overriding gas pressure can be used over the body of liquid to assist in establishing the pressure at the point of melt introduction into the liquid body.
  • the pressure is chosen to be sufficiently high so as to prevent foaming of the matrix if the matrix expands due to the vapor pressure of the plasticizer, solvent, or encapsulate.
  • the amount of pressure necessary can be readily determined by simple experimentation.
  • the pressure should be greater than the vapor pressure exerted by the volatile components at the molten product exit temperature.
  • Many materials e.g., the essential oils like orange oil, lemon oil and the like do not necessarily require pressure cooling since they tend to contain only small quantities of highly volatile materials. However, when these materials are enhanced with low boiling point top notes such as acetaldehyde, pressure cooling may offer advantages in reducing the microporosity of the finished product. The use of pressure cooling or atmospheric cooling with these materials is a matter of choice.
  • the encapsulate is not introduced into the melter directly but rather is introduced either immediately prior to or into a static mixer into which the melted matrix ingredients are also introduced.
  • the static mixer is illustrated as item 07, Figure 2.
  • the remainder of the system is similar to that illustrated in Figure 1.
  • the encapsulate in vessel 12 will be fed to a pressurized container, 04, and then pumped to the static mixer.
  • the use of a pressurized container is dependent on the volatility of the encapsulate.
  • the plasticizer solvent can be vented from the system before the matrix and flavor components are admixed.
  • melt pump, 06 can be omitted if the molten matrix is introduced directly from the continuous processor into the static mixer.
  • the encapsulates which are employed are typically those which have high solubility in the molten matrix, or disperse easily at the desired concentration level.
  • this system also finds particular use when highly volatile components are to be encapsulated.
  • the use of pump 05 and melt pump 06 facilitate the injection of low boiling point components into the molten matrix.
  • the remainder of the process after the static mixer is the same as for the previous embodiment. Examples of products which can be encapsulated by this technique include fragrances, colors, flavors, pharmaceuticals and the like.
  • FIG. 3 Another embodiment of the invention illustrated in Figure 3 is involved when encapsulating materials that are diluted in large amounts of volatile solvents that plasticize the matrix.
  • the process would consist of an initial melting zone, a flavor mixing zone, a venting zone from which the solvent(s) are allowed to escape, followed by a re-pressurization zone and subsequent forming and cooling. Cooling could take place at either ambient or pressurized conditions, depending on matrix composition, process parameters, and encapsulate.
  • the equipment which can be used for this process can be essentially the same as that described above.
  • the solvents in which the materials to be encapsulated are dissolved are also solvents for the matrix materials.
  • the use of a separate solvent in the formation of the melt is optional.
  • the use of a separate solvent may be useful to eliminate losses of the desired components during the phase in which the solid matrix is being converted into a melt.
  • the melt may be formed either in a batch process using a tank or large vat as discussed previously or through the use of extruder technology also as discussed previously.
  • the melt is then vented at atmospheric pressure or under vacuum depending on the desired level of solvent removal, vapor pressure of the solvent itself, vapor pressure of the encapsulate, and molten matrix characteristics.
  • the temperature is determined primarily by the conditions under which the venting of the melt is to occur and by the inherent vapor pressure of the solvent or solvents to be removed. If venting is accomplished to atmospheric pressure, higher temperatures are required than if vacuum conditions are used to vent.
  • the matrix is repressurized so as to remove any voids which are formed during the venting and then formed through a die.
  • the amount of solvent to be removed differs depending upon the matrix, the final properties desired in the solidified product, and loading. For hard, dense products more solvent must be removed than if the final product is to be soft. The product at this point may be either cooled under ambient pressure or under elevated pressure as described previously.
  • additional encapsulates may be introduced if desired. If these additional encapsulates are volatile, then it is preferred that the melt be extruded into a pressurized zone having sufficient pressure so as to preclude vaporization of significant quantities of the volatile components during solidification.
  • This technique has the advantage of allowing one to effectively concentrate vanilla solutions which have generally been difficult to concentrate because of the sensitivity of vanilla to degradation. It is believed that the matrix serves to stabilize the vanilla during the process.
  • Matrix materials are fed continuously to Melter 1 where they are melted prior to flavor injection.
  • the matrix/flavor mixture is discharged to the feed port of Melter 2.
  • Volatile solvents are vented out of the feed port of Melter 2, while the flavor containing melt is conveyed forward and discharged.
  • the material is fed to a melt pump which conveys the matrix/flavor mixture to forming and cooling operations.
  • the melt pump is optional. Not shown in this illustration is the linkage of this process with pressure cooling which would be desirable in some cases.
  • Flavorants which can be encapsulated in this technique include: Flavor Volatile Solvents Wt % oriq. flavor weight matrix
  • the invention provides for a further enhancement of the above technique by a secondary injection of volatile encapsulates after venting of the solvent from the primary encapsulate and re-pressurization. This, especially when combined with the previously described pressure cooling, allows the encapsulation of a massive variety of encapsulate compositions.
  • a further variation on the above processes just described involves venting the melting equipment to remove the solvent which has been added to serve as the plasticizer before injection of the flavor component.
  • the solvent utilized is water
  • it would be arranged to have a first mixing zone where the matrix and water are intimately mixed, a second where heat and/or pressure are applied by any means to cause the matrix materials to melt/fluidize and then a pressure reduction section from which the water is allowed to vaporize and thus be removed. Re-pressurization of the matrix would follow, with subsequent flavor injection, mixing, forming, and finally cooling.
  • Figure 4 represents a generalized flow sheet for the foregoing embodiments.
  • the process involves converting the matrix materials into a melt, and mixing in the encapsulate and then cooling to produce a dense, amorphous product.
  • the encapsulate is not soluble in the matrix or is only slightly soluble, the result is an encapsulated product while if the encapsulate is soluble in the matrix material there results essentially a solid solution.
  • a plasticizer solvent is introduced with the matrix to assist in melting. This plasticizer solvent may be vented if desired or may be retained in the mixture.
  • the mixing of the encapsulate and matrix can occur either in a continuous process such as in a tubular reactor containing a helix screw to provide positive movement of the matrix from one end to the other or in a separate static mixture which is in fluid communication with the continuous melter which converts the matrix into a melt.
  • the materials which can be encapsulated will depend upon the matrix material chosen. By selecting the appropriate matrix, it is possible to encapsulate virtually any material with this particular technique. This includes insoluble, and slightly soluble encapsulates and also encapsulates which are soluble when the encapsulate does not detrimentally affect the plasticity and melting point of the matrix. Many matrix materials can be used in this embodiment.
  • the classes of matrix materials include not only those listed in the above citations, but also materials such as mono- and disaccharides, oligomeric carbohydrates such as dextrins, and polymeric carbohydrates such as starches; soluble proteins and especially partially hydrolyzed proteins such as gelatin; other biopolymers; for example, hydrocolloids, gums, natural and modified celluloses; lipids, derivatives and/or any suitable mixtures of the above.
  • Lactalbumins Guar gum Glutein/glutenin Pectins Soy protein Tragacanth Myosin Gum Arabic Actinomyosin Carageenans
  • the finished product can be coated with an anticaking agent should that be necessary.
  • caking is generally not a problem when the matrix materials have a sufficiently high softening point, typically above about 40 ⁇ C.
  • any encapsulate which remains on the surface of the finished product can be removed by utilization of suitable solvent in which the encapsulate is soluble but the matrix is either insoluble or only slightly soluble. While essentially any solvent having such characteristics can be utilized, food grade solvents having those characteristics are preferred.
  • the encapsulate is a lipophilic flavorant such as lemon oil, orange oil and the like, isopropanol has proven a successful solvent. Such washing may not be necessary where cooling has been accomplished by quenching in a quench medium selected to both cool and remove any surface flavorant from the product.
  • the present process allows for the successful encapsulation not only of high boiling point materials but also those having boiling points below about 100°C and most beneficially below 40 ⁇ C in molten amorphous matrices.
  • materials having boiling points below these limits have not been successfully encapsulated in concentrated form but only when diluted with other flavorants.
  • acetaldehyde may be somewhat successfully encapsulated when it has been introduced as a component in oil-based flavorants like lemon oil and orange oil.
  • the present process provides for encapsulating pure acetaldehyde at high loadings above about l gram of acetaldehyde per 100 grams of matrix. Similar concentrations are possible with other low boiling point materials.
  • the use of pressure cooling allows for the formation of a dense amorphous matrix, which may be known in the art as a glass; this material being substantially free of porosity, both gross porosity and microporosity.
  • This substantial freedom from porosity will extend the shelf life of the product by reducing the amount of surface area exposed to the atmosphere.
  • the present process offers the advantage of increased loadings of materials in the matrix and a longer shelf life.
  • the absence of porosity also ensures a dense material that will penetrate through the surface tension of liquids, expediting dissolution, and reducing the opportunity for lumping.
  • the present process allows for the successful dense matrix encapsulation of materials diluted in volatile solvents.
  • encapsulates diluted in volatile solvent systems could not be successfully encapsulated at commercially significant loads due to the plasticizing effect of the solvent on the matrix.
  • This is overcome by the removal of the solvent after encapsulate injection via atmospheric or vacuum venting. Since the solvent removal takes place from the molten process stream, the resulting product is dense, thus the porosity formation caused by other solvent removal techniques such as spray or freeze drying is avoided.
  • secondary encapsulates may be injected into the process stream after removal of the primary encapsulate solvent. This is especially applicable to highly volatile secondary encapsulates, particularly when combined with the pressure cooling embodiment of the present process.
  • the present process can successfully encapsulate a much wider range of materials in dense, amorphous matrices than was previously possible.
  • the present process when compared with spray drying and other state of the art processes, offers greater efficiency in encapsulating materials containing volatile components or those diluted in volatile solvents, often at a processing cost advantage. Furthermore, because essentially any material can be encapsulated by proper selection of processing conditions and matrix materials, a wide variety of products can be produced all having essentially about the same density and flow characteristics, an advantage in blending. Furthermore, products which have been encapsulated or otherwise incorporated into matrix materials can be blended together to produce unique flavor combinations with reduced concern for settling or stratification upon standing since the relative densities and particle sizes of the materials can be chosen to be approximately the same. Thus the present process will offer a full range of encapsulants all having approximately the same density and flow characteristics making handling, metering, measuring and the like much easier for the processor.
  • the term "encapsulated product" includes not only those products truly encapsulated, where the encapsulate is insoluble in the matrix but also those products wherein the encapsulate is soluble in the matrix.
  • the encapsulates in the present process do not need to be subjected to elevated temperatures in the presence of oxygen. This is a significant improvement over spray drying where the use of antioxidants is essential to be able to encapsulate products sensitive to oxidation. Such materials include but are not limited to citrus oils, highly unsaturated lipids, oxidation sensitive colorants and the like. The present process allows the encapsulation of such products reducing the need for the use of antioxidants.
  • the present invention provides a method for preparing compositions which contain one or more volatile aroma compounds, such as a coffee aroma compound or a volatile gas emitted during the baking of a dough product or the roasting of a food like nuts, peanuts, or meats, and which retain these compounds for a prolonged period of time.
  • the present method involves the formation of a composition in which the volatile aroma compound is encapsulated in a meltable food matrix, especially a food polymer. This embodiment may be carried out as follows:
  • the volatile aroma compound is a coffee aroma compound.
  • coffee aroma compound means any volatile compound which confers the aroma of freshly ground coffee.
  • the coffee aroma compound may be a single compound or may be contained in a mixture such as synthetic or natural coffee grinder gas or an aroma obtained by collecting the vapors removed from coffee extract during dying. Examples of compounds which confer the aroma of freshly ground coffee include:
  • any component of natural coffee grinder gas which confers the aroma of freshly ground coffee may be used.
  • Such compounds include: ethyl mercaptan, ethyl acetate, methyl ethyl ketone, thiophene, pyridene, octane, l-hexanol, and furfural. As noted above, these compounds may be used singly or in combination.
  • the coffee aroma compound be natural grinder gas.
  • Grinder gas may be obtained by enclosing or hooding coffee grinding equipment, such as commercial grinders.
  • the gases liberated from the ground coffee may be removed by a pump or rotary blower; additionally, when desired, a stream of inert, preferably moisture free, gas may be used to sweep gas from the coffee and to have the grinding operation take place in a substantially inert atmosphere.
  • a stream of inert, preferably moisture free, gas may be used to sweep gas from the coffee and to have the grinding operation take place in a substantially inert atmosphere.
  • U.S. Pat. No. 2,156,212 describes a method of collecting gases evolved during roasting, but which can be equally applied to the collection of gases evolved during the grinding or cellular disruption of whole freshly roasted coffee beans. If pumping is employed, it may be desirable to cool the gas ahead of the pump so that the heat added by pumping will not deteriorate the aromatics contained in the gas.
  • the chemical composition of the evolved gas is largely carbon dioxide together with water vapor and the characteristic aromatic constituents of roasted coffee.
  • the amount of moisture in the gas may be lowered by the use of dry roasting conditions and low-moisture quenches or quenching mediums.
  • the evolved gas is preferably passed through a first condenser where it is cooled to between 35° and 50 ⁇ F and where substantial quantities of water are removed.
  • the relatively low-moisture gas is then fed to a second condenser, such as a jacketed, vertically-mounted, scraped-wall heat exchanger, which is cooled by means of a liquid gas refrigerant.
  • the second condenser is cooled by means of liquid nitrogen and the gas flow into the exchanger is maintained within the range of about 1 to 5 cubic feet per minute per square foot of heat exchanger surface.
  • the nitrogen gas that evolves from the cooling system is useful as an inert gas stream which might be used elsewhere in the soluble coffee process, such as sweeping grinder gas from the grinder or inert gas packaging of a soluble coffee product.
  • the aroma bearing gas is condensed into the form of a frost as it comes into contact with the heat transfer wall of the condenser.
  • Typical grinder gas frost is collected at a liquid nitrogen jacket temperature of -195 ⁇ F to -220°F, contains approximately 87% carbon dioxide, approximately 10% water, and approximately 3% coffee aromas.
  • the frost, as it is removed from the condenser wall and collected, is thus very dilute in the coffee aromas.
  • the frost may be held for a short period at low, such as liquid nitrogen, temperatures without deteriorating; however, it is preferred to immediately utilize the frost in accordance with the present invention.
  • the coffee grinder gas frost may be used directly as the coffee aroma compound, it is preferred that the coffee grinder gas frost be further process to increase the concentration of the compounds which confer the aroma of freshly ground coffee.
  • the coffee grinder gas frost may be equilibrated at a pressure in excess of 750 psig to form three phases (a water phase, a liquid carbon dioxide phase, and a gaseous carbon dioxide phase) , and the water drained, after which the liquid carbon dioxide is introduced into a vessel at a temperature less than -80°F, and this vessel is vented at 0 ⁇ F and then warmed to a temperature between 0°F and 30°F to obtain a highly concentrated liquid coffee aroma.
  • This method is disclosed in U.S. Patent no. 4,574,089, which is incorporated herein by reference.
  • a similar method for preparing a concentrated liquid coffee aroma is described in U.S. Patent No. 4,551,345, which is also incorporated herein by reference.
  • U.S. Patent no. 4,008,340 which is also incorporated herein by reference, describes a method for concentrating and stabilizing coffee grinder gas aroma, by combining coffee grinder gas frost with ascorbic acid or a salt thereof, warming to obtain a fluid, contacting the fluid with a liquid fluorinated hydrocarbon, separating the fluid condensate from the liquid fluorinated hydrocarbon, contacting the fluid condensate with a mixed solvent, and separating the condensed residue as an aqueous phase.
  • the matrix material can be any of those described above.
  • the matrix material is mannan oligomer obtained from spent coffee grounds.
  • a suitable method for producing such mannan oligomers is described in U.S. Patent no. 4,508,745, which is incorporated herein by reference.
  • Other preferred matrix materials are galacto-mannans, such as those obtained by multi- step coffee extraction by the application of heat/steam etc.
  • a plasticizer to the matrix to form the melt.
  • the water contained in the frost may serve the role as plasticizer.
  • the liquid may also serve to plasticize the matrix.
  • a plasticizer such as water, glycerol, etc. may be added.
  • the pressure under which the melt of matrix material and coffee aroma compound need be cooled will depend on the volatility of the coffee aroma compound but in general will be at least 500 psig, preferably at least 750 psig.
  • the pressurized cooling of the melt is conveniently carried out in a closed chamber or vessel. Thus, the process may be carried out by extruding the melt directly into a closed chamber or vessel.
  • the pressure in the cooling chamber or vessel may be created by an overriding pressure of an inert gas, such as nitrogen, air, etc.
  • the cooling chamber is pressurized with a gaseous coffee aroma compound, especially coffee grinder gas.
  • a key feature of the present method is that it affords dense, glassy matrices directly, without the need for an additional drying step, and the coffee aroma compound is stably encapsulated in the glassy matrix. That is, the present compositions will retain the coffee aroma compound for prolonged periods of time. Typically, the present compositions will contain the coffee aroma compound in an amount of from 0.01 to 10 wt.%, preferably 0.1 to 5 wt.%, based on the total weight of the glassy matrix. Although it is preferred to encapsulate natural coffee grinder gas which has been treated to concentrate the aroma, it is also possible to formulate compositions which are a blend of two different glassy matrices, which each may contain a different coffee aroma compound and/or matrix material.
  • the present compositions which contain a coffee aroma compound may be added to any composition for which it is desired to enhance or create a coffee aroma.
  • the present compositions may be added to any conventional instant coffee powder or ground roast coffee.
  • instant coffee is meant to include not only those materials consisting of 100% coffee but also to substitute or extend coffees which may contain roasted grain, chicory, etc.
  • the present compositions may also be added to instant cake mixes, instant pudding mixes, candies, or any other coffee flavored foodstuff which is stored in a dry state and is rehydrated when either prepared or eaten.
  • the volatile aroma compound is a gas emitted during the baking of a dough product, like bread, or the roasting of a food, like nuts, peanuts, or meats.
  • the gas emitted during the baking of dough products may be collected in a similar manner as described for collecting grinder gas. Specifically, air or an inert gas such as nitrogen may be blown through the oven and then passed through a series of cold traps to collect a bread baking gas frost, which can optionally be dewatered before incorporation in the matrix melt. Similarly, air or an inert gas such as nitrogen may be passed through the oven in which peanuts (either shelled or in- the-shell) are being roasted, and a peanut roasting gas frost collected.
  • the aroma released during the grinding of roasted peanuts may also be collected and used as the encapsulant.
  • the aroma released when roasting true nuts, such as almonds and cashews, may be collected and used in a similar fashion.
  • Other types of aromas such as the volatile gas emitted during the roasting of meats such as poultry, beef, pork, lamb, etc. may also be collected and used as the volatile aroma compound.
  • Sample 2 Atmospheric pressure cylindrical collection vessel in ice bath.
  • Sample 3 Cooled in cold 99% isopropanol (initial temperature -18°C) at atmospheric pressure, approximately 130 g sample collected in 2000 g IP.
  • Sample 4 Pressure cooled; approximately 20 minutes under
  • samples 1-3 were white and puffed with a porous internal structure. Sample 4 appeared dense, hard and relatively clear.
  • Example 2 A carbohydrate based matrix composed of:
  • the matrix and diacetyl mixture was then delivered under pressure to one of the nozzle discharges for forming and subsequent collection.
  • the flow system was arranged so that forming and solidification could take place under either atmospheric or pressurized conditions.
  • the product temperature was approximately 132°C. Four samples were taken.
  • Sample 2 Atmospheric pressure cylindrical collection vessel in ice bath
  • Sample 3 Cooled in cold 99% isopropanol (initial temperature -18 ⁇ C) at atmospheric pressure, approximately 125 g sample collected in 2000 g IP (final IP temperature was -8 ⁇ C) .
  • Sample 4 Pressure cooled; approximately 20 minutes under
  • samples 1-3 were pale yellow, relative opaque, and puffed with a porous internal structure.
  • Sample 4 appeared dark yellow, dense, hard and relatively translucent.
  • a carbohydrate based matrix composed of: 56% Amerfond (Domino Sugar, 95% Sucrose, 5% Invert sugar) 42% Lodex Maltodextrin (American Maize, 10 DE) 2% Distilled monoglyceride (Kodak, Myverol 18-07) Flavor:
  • vanilla extract (3 1/3 fold, 11.9% solids, 39.8% alcohol) was fed at a rate of approximately 114 grams/minute into continuous processor 1 ( Figure 3) .
  • the mixture was melted in processor 1.
  • Processor 1 was maintained at 143°C.
  • Processor 1 screws were operating at 70 RPM.
  • the vanilla extract was injected into processor l through a port at a flow rate of approximately 22 grams/minute.
  • the molten mixture was discharged directly into processor 2 (143°C jacket temperature, 120 RPM) . Water and ethanol vapor were allowed to escape from the open feedport of processor 2.
  • the molten mixture was discharged into the melt pump which discharged through the nozzle onto trays for cooling and solidification.
  • the product temperature exiting processor 1 was 102°C.
  • the product temperature at the discharge of the melt pump prior to nozzle forming was approximately 115"C.
  • the temperature out of processor 1 was 98 ⁇ C and the product temperature out of processor 2 was 127°C. After cooling, the product was hard and dense, having the flavor characteristics of vanilla extract.
  • Example 5 A carbohydrate based matrix composed of:
  • Example 3 Conditions were as described in Example 3 except the feed rate for the beef flavor was 29 grams/minute and no melt pump was used.
  • the temperature out of processor 1 was 112°C and the product temperature out of processor 2 was 129°C.
  • the jacket temperature was maintained at 160°C.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Polymers & Plastics (AREA)
  • Health & Medical Sciences (AREA)
  • Nutrition Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Fats And Perfumes (AREA)
  • Seasonings (AREA)
  • General Preparation And Processing Of Foods (AREA)
  • Tea And Coffee (AREA)

Abstract

Cette invention se rapporte à un procédé qui permet d'incorporer un constituant volatil dans une matrice et qui consiste à cet effet: (a) à former un bain de fusion contenant ce constituant volatil (12) et cette matrice (10); (b) à solidifier ce bain de fusion sous une pression suffisante pour empêcher toute volatilisation du constituant volatil (8). Dans un mode de réalisation préféré, le constituant volatil est un composé aromatique volatil, tel que les composés contenus dans les gaz des moulins à café ou tels que ceux qui sont produits lorsqu'on cuit une pâte au four ou lorsqu'on fait griller un aliment.
EP95935021A 1994-09-29 1995-09-28 Encapsulation d'aromes Withdrawn EP0783251A4 (fr)

Applications Claiming Priority (3)

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US31490994A 1994-09-29 1994-09-29
US314909 1994-09-29
PCT/US1995/011967 WO1996009773A1 (fr) 1994-09-29 1995-09-28 Encapsulation d'aromes

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EP0783251A4 EP0783251A4 (fr) 1997-11-12

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US5750178A (en) * 1996-06-18 1998-05-12 Nestec S.A. Method of making coffee particles containing aroma
AU744156B2 (en) * 1996-10-28 2002-02-14 General Mills Inc. Embedding and encapsulation of controlled release particles
EP1342548B1 (fr) 1996-10-28 2015-12-23 General Mills, Inc. Inclusion et encapsulation de particules à libération contrôlée et produit encapsulé
US6723358B1 (en) 1998-03-23 2004-04-20 General Mills, Inc. Encapsulation of components into edible products
ES2237949T3 (es) * 1998-11-04 2005-08-01 Firmenich Sa Sistema de liberacion solida para ingredientes aromaticos.
US6500463B1 (en) 1999-10-01 2002-12-31 General Mills, Inc. Encapsulation of sensitive components into a matrix to obtain discrete shelf-stable particles
US6251478B1 (en) * 1999-12-22 2001-06-26 Balchem Corporation Sensitive substance encapsulation
US6436453B1 (en) 2000-06-16 2002-08-20 General Mills, Inc. Production of oil encapsulated minerals and vitamins in a glassy matrix
US6468568B1 (en) 2000-06-16 2002-10-22 General Mills, Inc. Oligosaccharide encapsulated mineral and vitamin ingredients
US6572905B2 (en) * 2000-12-21 2003-06-03 Kraft Foods Holdings, Inc. Preparation aroma system for dehydrated food product compositions
US8334007B2 (en) * 2003-03-19 2012-12-18 Firmenich Sa Continuous process for the incorporation of a flavor or fragrance ingredient or composition into a carbohydrate matrix
ES2399093T3 (es) * 2004-05-24 2013-03-25 Nestec S.A. Aislado de arabinogalactano procedente de café verde tostado para aplicaciones alimentarias y de administración, y procedimiento para su producción
EP1632135A1 (fr) * 2004-08-18 2006-03-08 Nestec S.A. Matrices inertes et vitreuses pour la stabilisation des aromes du cafe soluble
US7803413B2 (en) 2005-10-31 2010-09-28 General Mills Ip Holdings Ii, Llc. Encapsulation of readily oxidizable components
AU2007313849B2 (en) 2006-10-31 2010-06-10 Wm. Wrigley Jr. Company Flavor releasing cores and their use in chewing gum

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EP0354810A2 (fr) * 1988-08-12 1990-02-14 Kraft General Foods, Inc. Café vitrifié et produits
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EP0783251A4 (fr) 1997-11-12
JPH10506784A (ja) 1998-07-07
WO1996009773A1 (fr) 1996-04-04
AU3719795A (en) 1996-04-19
MX9702317A (es) 1997-07-31
CA2200849A1 (fr) 1996-04-04

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